Final Report Functional Coatings for 3D Printed Parts_JONATHANAMBROSE
1. UNIVERSITY OF CENTRAL LANCASHIRE
SCHOOL OF COMPUTING, ENGINEERING AND PHYSICAL
SCIENCES
COMPUTER AIDED ENGINEERING BEng (Hons)
FINAL PROJECT REPORT
Project – MP3997
A STUDY ON
HB9 - Functional Coatings for 3D Printed Parts
TUTOR
Dr Hadley Brooks
REPORT BY
Jonathan Ambrose
ACADEMIC YEAR
2014/2015
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I. Declaration
I would like to declare that all of the work within this dissertation is my
own. Also, all references, quotations and support information are fully
identified and acknowledged in the reference list.
StudentName:
StudentUCLAN ID:
Signed:
Date:
3. 3
II. Acknowledgements
I would like to thank Charlotte Pickthall for being supportive and
understanding during my period at university.
A special thank you to my mother for her supportive nature and
encouragement to make me the person I am today.
With the addition consideration of all family, friends and tutors who have
provided understanding and support through thick and thin.
‘It is during our darkest moments that we must focus to see the light’
Aristotle Onassis
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III. Abstract
Physical testing results have shown that applying a metal coating to a
3D printed part improves the material properties whilst retaining the low
mass of the polymer.
Further tests and research are to be conducted to improve the two
methods of the process; Conductive Coating Solution and
Electrodeposition.
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IV. Equation and VariableList
Faraday’sLaw of Electrolysis (Electroplating DepositionRate)
I = Electric Current, t = Time, Q = Electric Charge
W = Weightof the depositedmaterial (g)
μ = Weightof one mole of the anode (Metal)
n = Number of electrons transferred by the ion into the solution
F = Faraday’s Constant = 96485 Coulombs
Considerelectric charge = Q = I * t
Then Faraday’s law may be expressed by the following formula:
Faraday’s Law = W = I*t*μ /(n*F)
Vickers Hardness (HV) Conversion(Top)and HV Formula (Bottom)
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V. Table List
Table 1 – 12 Orders of Magnitude
Table 2 - Polymer Solvent Reactivity Table
Table 3 - Conductive Coating Phase Risks
Table 4 - Electricity Human Damaging Table
Table 5 - ElectrodepositionPhase Risks
Table 6 – WeeklySchedule of Work
Table 7 – Risk Management
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VI. Applicable / Useful Patents, Standards and Safety
Legislations
The following are useful and applicable patents that allow for a better understanding
of the conductive coating and electrodeposition phases:
US 7235165 B2 – Safe Electroplating Solution
US 3715289 A – Brightener Composition for Acid Copper Electroplating
Baths
US 3542655 – Electrodeposition of Copper
CN 1152098 C – Graphite Conductive Coating Material
US 5476580 A – Process for Preparing a Non-conductive Substrate for
Electroplating
US 3249559 A – Conductive Coating.
The following are useful and applicable standards that allow for quality assurance of
material composition, preventing the influence of contaminants during the conductive
coating and electrodeposition phases:
BS EN 509-1:1987 – Acetone Purity Standard
BS EN 13604 – Copper Bar Purity Standard
BS EN 12166 – Copper Wire Purity Standard
ASTM B281 – 88 (2013) – Standard Practise of Preparing Copper
Electroplating Coatings
BS OHSAS 18001 – Occupational Health and Safety Management.
8. 8
Applicable / Useful Patents,Standards and Safety Legislations
(Continued)
Before commencing work on the project, the following laws and regulations were
read and understood.
Health and Safety at Work Act (HASAWA) 1974
Control of Substances Hazardous to Health (COSHH) 2002
Personal Protective Equipment at Work Regulation 1992
Chemicals (Hazard Information and Packaging for Supply) Regulations
(CHIP) 2002
Electrical Equipment (Safety) Regulations 1994
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Contents
I. Declaration
II. Acknowledgements
III. Abstract
IV. Equation and VariableList
V. Table List
VI. Applicable, Useful Patents and Standards and Safety
Legislations
1 Summary………………………………………………….……………..14
2 Introduction………………………………………………………….….15
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1 Summary
This report presents the development of functional coatings for 3D printed parts.
This was initially composed due to the need for simple and effective coating
techniques upon 3D printed parts. This is only viable for polymer printed parts;
therefore two elements were devised for successfully producing plated coatings
upon polymer parts:
Creating a uniform Conductive Coating
Electroplating Homogenously
The techniques developed were compared for value simplicity and quality of
coating, whilst considering cost, material properties and safety.
The stages of development shall include multiple techniques to which they are
applied with; the superior methods shall include evidence and data with
controlled experimental methods.
This report finds that combining conductive coating and electroplating techniques
upon the 3D printed part.
This successfully enhances the electrical conductivity, Young’s Modulus,
compressive and tensile strength and hardness from the incorporation of the
metal coating; with the additional benefit of having an increased resistance to
corrosion.
For more information on the plan and specification see appendices 8.3 project
plan and specification.
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2 Introduction
This project will be the sole work of Jonathan Ambrose under the supervision of
Dr Hadley Brooks. This report has been written to satisfy the learning outcomes
stated in module MP3997. This module is a requirement for awarding an honours
degree at the university of central Lancashire.
A head researcher of manufacturing stated” the additive manufacturing industry
has grown exponentially from a value of $200M in 2009; to 2014 with $1B worth
of systems” Gibson, I (2011). This developing manufacturing technique is
improving how products are manufactured; locally and internationally.
There is a continued need to improve this process, to expand the capabilities of
the technique whilst reducing price and increasing quality.
Additive manufacturing technology is still in its early embryonic stages and has
great potential for future development.
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3 LiteratureReview
3.1 Additive Manufacturing (3D Printing)
Additive manufacturing (AM) is the creation of a 3D object from a CAD model to a
solid model via an AM technique. Experts have stated that it is important to
understand that AM was not developed in isolation from other technologies. For
instance it would not be possible for AM to exist were it not for innovation in areas
like 3D graphics and Computer Aided Design software, this view was supported
by Gibson, I (2011).
This report shall investigate the Fused Deposition Modelling (FDM) technique.
FDM uses a .STL file (a CAD file which has been converted into a path to follow)
which manipulates the extruder nozzle on the FDM.
The extruder follows via Cartesian coordinates whilst extruding material;
essentially developing and building a 3D Model as supported by Dr Chua, C
(2014)
Other AM techniques offer a variety of qualities in regards to cost, material
properties, speed of print, variety of materials used, tolerance of print, less waste
etc. This flexibility AM offers has near limitless capabilities to which it has been
realised that the biggest spur for AM was not the limitless customisation, but the
economics of production.
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3.2 Conductive Coatings
A researcher stated that conductive coating is an applied material which is
electrically conductive, embedded upon a component which may or may not be
previously conductive. Davis, J (2004). The following are crucial parameters
which need to be considered and adopted when developing a conductive coating
solution and method:
Adhesion
o Quality of adhesion between conductive solution and component
which is to be coated
Conductivity
o The resistance of the post-electroplated part is at least 95% of the
anode
Hardness
o Hardness of post-coated part is hard enough to resist damage
during electrodeposition is aimed at achieving 75% of the anode
Safety of Chemicals
o The chemicals used during this phase need to have MSDS for each
to make the user aware of the risks involves with specified PPE for
each. The safest methods shall be of priority.
Research has been conducted to develop a conductive solution based on systematic
experimentation. Data from these trials has been developed and improved.
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3.3 Electroplating
Electroplating (or otherwise known as electrolysis) is the method of applying an
electrically conductive material (known as the anode) upon a conductive part
(known as the cathode).
This method uses a power supply, Anode, Cathode and a plating solution; with
multiple parameters depending on application. However in practise this works as
follows:
The Plating Solution is placed in a non-conductive container (Usually
Glass)
The power supply is set-up connecting the anode to positive (coating
material) and the cathode to negative (component being plated)
The Anode and Cathode are placed within the solution (Not Touching)
The power supply is turned on to the relevant voltage / current
Apply coating material sulphate to solution to speed up coating (e.g. if
using copper as the Anode, add copper sulphate to the solution to speed
up the coating process) Also use Faraday’s Law to calculate the
deposition rates
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3.4 SEM (ScanningElectronMicroscope)
3.4.1 Introduction
“A SEM uses a focused beam of high-energy electrons to generate the
topography of the component or sample of solid specimens” stated by Egerton,
R. F. (2005). The signals which develop the information are from electron-sample
interactions which reveal information about the specimen including topography,
material composition, crystalline structure and orientation of materials which
make up the sample. In the majority of applications the data collected is from a
selected area on the surface of the part which generates a 2D / 3D image
displaying the spatial variations on a tribological scale. The SEM is used due to
the order of magnitude required to gain reliable results for this particular
application. See below for the 12 orders of magnitude.
Table 1- 12 Orders of Magnitude
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The applicable surface area range which the SEM can develop is approximately
1cm to 5 microns squared. This can be imaged in conventional SEM techniques.
Magnification can range from 20X to 30,000X, with spatial resolution of 50 to
100nm. A SEM scientist described the capability of the SEM as “capable of
generating graphical feedback showing the topography on a 3D generated graph
also showing the average peaks and troughs between designated areas”. Clarke,
A. R. (2002).
3.4.2 SEM essential equipment
The SEM needs the following essential components to be able to produce highly
accurate results and sustain component quality:
Electron source
Electron lenses
Sampling stage
Signal detectors (Electron Sample Interactions)
Output Devices to Display Data (i.e. Monitor)
Infrastructure Requirements:
o Power Supply
o Vacuum System
o Cooling System
o Vibration-Free Floor
o Room free of magnetic and electronic interference (fields)
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SEM has the following benefits; it has the ability to produce data extremely fast,
with the sample preparation time being less than 5 minutes. The data available is
in digital formatting making it highly portable. As an investigating tool the SEM is
of great importance in all fields that require specification of solid materials from
topography to composition.
An extremely useful aspect of the SEM, is its ability to also produce composition
tests to accurately produce sample material composition reading with supporting
graphs. The SEM (Inspection Machine 1) used to conduct the experiments is
shown below.
Inspection Machine 1 - SEM (Found in JB Firth Building)
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3.4.3 SEM Limitations
However, the SEM does have limitations which are the following:
Samples must be Solid
Maximum Horizontal Dimensions are around 10cm
Maximum Vertical Dimensions are around 40mm
Samples must be stable in a vacuum at 10-5 to 10-6 torr
Samples may depreciate at low pressures (Low vacuum and
Environmental SEM variations exist)
SEMs cannot detect very light elements (H, He and Li) and unable to
detect elements with atomic numbers less than 11
Electrically Conductive coatings must be applied to electrically insulating
samples for study in conventional SEMs (However Gold Powder Coating is
Available for Non-Electrically conductive samples)
For more information on the usage of the SEM and the Official UCLAN Training
manual see appendices 8.7 SEM Training Manual.
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3.5 Grain Growth effecting CoatQuality
During electroplating, the grain growth on the Cathode is directly proportionate to
the voltage applied during electrolysis; which in-turn reflects the quality of the
applied coat.
A Grain Growth researcher considered that the energy of the grain nucleus’
formation, depends on the cathode of potential voltage. A. Milchev (2002).
The following parameters need to be adjusted to accommodate for the copper
plating process on the graphite:
Maintaining Optimum PH Level
Electroplating Solution Temperature
o An electroplating researcher stated “It should be noted that
increasing the bath temperature has two contradictory effects; (i) an
increase in critical size of nucleus due to a decrease in
thermodynamic driving force of the crystallization. This leads to
lower nucleus densities, (ii) an increase in kinetic the driving force
that can lead to a higher nucleation rate” J.W.P. Schmelzer (2003):.
Electroplating Solution / Copper Sulphate Density
Voltage through Anode to Cathode
It was found that increasing the voltage beyond the limit affects growth
consistency and quality. This is due to during the electroplating phase the
voltage breaks the anode down and attaches that to the cathode. This
replaces electrons; during this process the anode is heated and therefore
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expands creating bigger grain growth. The use of Faraday’s law and an
SEM should be used to gather information of the optimum voltage for
electroplating. For this specific grade of copper used. The optimum voltage
for this experiment was found to be 1.5V / 20mm2.
Below shows how voltage during electrodeposition affects grain growth
Figure 2 –Low voltage electroplating (Left), High Voltage Electroplating (Right)
From the observation it can be seen that increased grain growth affects the
aesthetics of the part however it has not yet been tested whether this affects the
material properties. Further research should be conducted whether it could be used
at an advantage to improve a specific area of material properties.
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3.6 VickersHardness TestingMachine (VHTM)
3.6.1 Introduction
The Vickers Hardness Testing Machine (VHTM) is a material property testing tool
that measures the material property of hardness. This test uses a square based
pyramid diamond indenter with an angle of 136 degrees between the opposite
faces at the vertex. The Indenter presses into the sample using a user defined
force (F), the total test time is 20 seconds long; once the force is removed, the
legnths of the vertex’s are measured (d). The hardness number is given by the
following formula. See HV rating and conversion rating formula below.
Equation 1 - Vickers Hardness Conversion to Mega Pascal
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Diamond Indenter
3.6.2 VHTM Essential Equipment
The VHTM requires essential components to be able to produce highly accurate
results and sustain component quality. The following are the essential
components of the VHTM:
Diamond Indenter
Calibration Blocks and Setters
Sampling Base
Output Gauge.
Due to the basic set-up and operation of the
VHTM and no electronic source, it becomes
simple to measure the HV rating.
VHTM Calibrating Gauge Set
The VH testing machine used to conduct material tests on the samples
developed is showns on the next page.
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Hardness Testing Machine 1 – Vickers Hardness Testing Machine
For the methodology of using the VHTM see appendices 8.8 VHTM training
Manual.
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3.6.3 VHTM Limitations
Due to the simplicity of the VHTM, measurements of the indenting vertex are
inspected by the user, which introduces human error during measurement. With
the addition of calibration introducing any further error.
The indenting of the sample during the release of the load, can spring back due
to elasticity of the component which introduces further inaccuracies.
The wear and tear of the indenting tool can also affect inaccurate results,
however being diamond tipped this can be of low possibility.
Overall the limitations which appear are the inaccuracies of preparation and
usage by the user. However careful preparation and measurements are to be
carefully to ensure the highest of accuracy.
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3.7 ProjectManagement
Project Management is key in creating an efficient and effective usage of a
project resources, deliverables and quality of products. This ensures the project
runs smoothly to which milestones are met at designated time frames.
3.7.1 Introduction
This section of the report, introduces the project management methods
implemented. The following will describe and evaluate the methods used.
‘Even if you are on the right track, you will get ran over if you just sit there’ (Covey
1996) The quote by Steven Covey tells us that no matter if you are on the right
direction, a plan needs to be made and progress needs to keep going. One of the
largest risks in this module is the possibility of failing, with this being of core
priority this has to be passed.
Progress has to be made to ensure success; this is why project management is
crucial for this instance. The following sections shall delve into more detail in time
and resource management of the project.
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3.7.2 Time Management
The managing of time is one of / if not the most crucial resource within any
project of any size. Without proper managment of the project over an available
time scale, the work done will be hard to track and maintain a momentum to
complete the course at university.
This is to be prepared and managed effectively at the start of the project to create
milestones and effectively utilize of one’s time; an effective tool for managing time
is by creating a Gantt chart.
Henry Ford who is the founder of Ford Motor Company once said ‘ Nothing is
particularly hard if you divide it into smaller jobs’; from the success of Henry Ford
this shows that any task can be completed by dividing into smaller chunks to
complete, which is therefore why the development of the Gantt chart began.
See appendix 8.4 for this projects developed Gantt chart.
Due to the amount of work to be completed during the time at the university
course a weekly project plan was developed to organize and schedule the time
resource. This can be seen in table 6 to the right.
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Table 6 – Weekly Schedule of Work
The above table shows the initial weekly schedule plan which was used as a
guide to maintain work progress between modules, to which it shows at least 20
hours allocated for the project work each week.
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3.7.3 Risk Management
Throughout any project, a degree is risk exists which could affect the overall
progress and relinquish resources. This is why at the start of a project, the risks
need to be identified early to minimize the impact on the project and develop
necessary actions to take when one does occur.
Table 7 shows the risks present from the start of this project and processes made
to reduce each risk. A traffic light system has been used to identify the level of
each risk; with green being low, indicating the impact will be low on the project;
red being the highest of risks therefore having the greatest impact on the project.
Table 7 - Risk Management
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The majority of the risks are universally the same at a project of this level. The
processes to reduce each slightly differ; however notice how losing motivation can
be of low risk to which it has been identified that the project student is a kinaesthetic
learner from the VAK test taken; this therefore creates a customized solution.
3.7.4 Resource Management
An expert in project management stated “the management of resources at their full
potential whilst extracting the knowledge and creating progress is key with any
resource” Pugh, S. (1991). The following are resources used with benefits and
limitations to both:
Time
o The benefit is that time is free and becomes better utilized to which the
more is spent.
o The limitation is that the resource may be low and repetition and
boredom can occur if used on a regular basis; reducing the utilization
of the resource.
Computer Software
o The benefit is that it allows quicker processing of information.
o The limitation is that it requires skills which may not have been learned
therefore time would have to be used to learn.
Online Information
o The benefit is that it allows a broader knowledge to be gained, it
requires heavily on the resource time but can gain a lot of knowledge
from similar projects already made.
o The limitations is that it may not be a valid source of information
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Chemicals / Materials
o The benefit allows direct hands-on experimentation validating results
investigated.
o The limitations are it requires money and possible lead-time if ordered
in.
Computer Software
o The benefit is that it allows creation and sorting of tasks, such as gantt
chart, Microsoft word and excel, supporting interfaces with machines
etc.
o Costs money for software and time to train to learn.
3.7.5 Experimentation Management of Project
Throughout the preliminary stage of the project, current methodology of the
project was of low existence which depended on experiments and trial and error
to be heavily focused on. This created a burden on the developed Gantt chart
and its processes, however maintaining a weekly schedule and creating an
effective process of gained knowledge allowed progression to be exponential.
This developed a learning curve of knowledge allowing me to strategic set tasks
from the results gained, to increase the chance of creating concrete results to
develop a methodology.
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3.7.6 Evaluation
During the management of the project a good way to keep track of the progress
was to create a Gantt chart and define set times within the week to work. The
main problem which occurred was that all the tasks could not be defined. This
was due to lack of knowledge during preliminary stages, preventing progress to
be met.
This resulted in repetition of the testing phases to produce adequate knowledge
and effectively produce a learning curve to understand the process.
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4 Electroplating Method
4.1 Conductive Coating
4.1.1 Materials / Resource Requirements
The conductive coatings stage, consisted of multiple techniques that require use
of various equipment and materials. The following list shall consist of all
equipment used for all the methods:
Paint Brushes / Variable Brushes (Preferably Short Bristles)
Rotary Buffer / Polisher (Minimum 2000 RPM)
Polisher Pads (for Rotary Buffer)
Buffer Pads / Cloth
Glass Container (Preferably >250ml)
Atomizer / Spray Bottle (Not made from ABS, Acrylic, CPVC, PC, PVC and
PVDF)
Graphite (Powder) At least 90% Carbon*
Acetone Solution BS EN 509-1:1987*
Grey Primer AutoTek*
ABS (Solid State)
Copper Powder
*Note Materials to British Standard are Ideal but not necessary, to which poor
quality material will still perform the experiment well i.e. instead of copper rod
a 2 pence coin as the anode will still perform electroplating but poorly.
37. 37
An alternative to Acetone is Grey primer; from the experiments has shown
significant improvements in material wear resistance and cathode coverage.
Results have shown that the Grey Primer has additional solvents are including
which have shown to improve the quality of the coating.
Check table below for applicable materials which will work B – D with possible
results from A. Different solvents. If safety and speed of plating is priority,
Acetone is recommended; if quality and increased mechanical properties are
priority the use of primer is recommended. Both are to be used carefully with
safe preparation and control.
Table 2 - Polymer Solvent Reactivity Table - Prairie, E. (2009)2
.
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Key:
A = No Attack, possible slight absorption. No effect on mechanical properties.
B = Slight attack by absorption. Some swelling and a small reduction in
mechanical properties.
C = Moderate attack of appreciable absorption. Material will have limited life.
D = Material will decompose or dissolve in a short time.
‘* ‘ = No Data Available.
4.1.2 Health and Safety
Health and safety was considered for all multiple methods that require a certain
degree of preparation to avoid possible risks. The chemicals / materials used are
relatively safe to which skin contact with any of them listed; will not cause harm.
However due to being pure chemicals it is recommended to wear protective
goggles and gloves whilst handling the materials.
Also be aware of the low vapour pressure properties of Acetone and grey primer;
which is highly flammable in its liquid and vapour state. This can cause light-
headedness during inhalation; it is recommended to wear a procedure mask
during usage; however from the MSDS in Appendix 8.1 there is no evidence to
suggest carcinogenic properties exist in Acetone due to the organic nature of the
chemical.
To see the Material Safety Data Sheet of any of the chemicals listed above see
Appendix 8.1.
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The equipment used for creating the conductive coating is relatively safe with no
lethal consequence under normal use; however the only piece of equipment
which may cause harm is the rotary buffer; which is powered electronically
therefore posing the risk of electrical faults and moving parts (spinning rotary).
Under normal / safe operation of the equipment listed and correct PPE equipped,
the operation shall pose minimal risk.
Table 3 - Conductive Coating Phase Risks
4.1.3 Method and Constraints
Creating a conductive coating on an ABS part can be split into two phases;
initially embedding graphite into the ABS; secondly, aligning the graphite to
become conductive. The following 4 phases of applying the conductive coating
are as follows:
1. Firstly creation of the conductive solution; uses 1 part graphite powder to
10 parts solvent. This mixture is flexible to change as long as the solution
becomes dark. This is due to the solution evaporating during normal
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atmospheric use. (Note: Too much solvent will cause details within the
model to smoothen)
2. The solution is then applied to the component via brushing. Once the part
is fully covered leave for 5 minutes at room temperature for the solution to
evaporate in a well ventilated; area due to risk of light headiness. During
evaporation the component appears cold, this is due to the low vapour
pressure of the solution. It is recommended to wait until the component
returns to room temperature to avoid damaging the component.
WARNING: Beware of application of ACETONE near sparking tools due to
FLAMABILITY. To ensure safety; when applying, leave to dry before
setting sample upon the electroplating phase.
3. Once the part is dried, the buffing stage begins. It is recommended to use
a rotary buffer (RB) at 2000 RPM, however if that is unavailable use of a
cloth or tissue, is recommended. Rub in small circular motions until the
component appears Grey Metallic.
4. The first layer should now be complete; repeat this step 2 more times to
develop 3 layers. Once all 3 layers are complete, record the resistance
using the multimeter. Usage of the RB method should record a resistance
of around 50Ω-100Ω or using the cloth / tissue the resistance should be
around 150Ω-400Ω.
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The resistance on the surface of the component is directly proportional to the
quality of the buffer to which the lower the resistance of the buff the better the
quality of coat.
The lower the resistance the quicker and smoother the electroplating will be so
ensure that the component is fully buffered on each layer and comprises of a
shiny grey texture.
Due to lack of resources at this current time, it is found that the quality of the
conductive coating is directly correlated to the quality of the electroplating
procedure. A superior theoretical alternative will be to buffer the post-conductive
coated part with a fine sand blast. This provides benefits of being able to reach
complex areas (which are unable to be buffered due to location), and provides a
smooth alignment of the graphite grain.
Observations and Risks
During creation of the conductive coating it has been found that during
impregnation of the graphite / solvent solution the surface of the component will
remain soft to which buffering / contact during this stage is to be avoided until the
solution has evaporated. To test the surface softness, lightly press the multimeter
probe against the component, if an indent appears, leave the component longer
to cure. DO NOT apply component near a heat source i.e. radiator due to this
may cause the graphite to separate from the polymer sample.
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Scratchable Rating:
A: Unscratable, Very hard to remove coat
B: Hard, Scratable but takes effort to remove
C: Intermediate, Takes abit of pressure to remove
D: Soft, Little pressure needed to remove
E: Easily Scratched off, No or Little pressure needed.
Conductive Coating Phase
Resistance in Ohms
(10mm^2 and 20mm^2) Scratch able Rating
1L-2RPM 550 E
1L-10RPM 280 D
3L-2RPM 50 C
3L-10RPM 30 C
1L-2RPM-ABS 800 E
1L-10RPM-ABS 750 E
3L-2RPM-ABS 500 D
3L-10RPM-ABS 450 C
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Key:
1L : 1 Layer of Graphite / Acetone Solution
3L : 3 Layers of Graphite / Acetone Solution
2RPM : Buffered at rotary speed of 2000 RPM
10RPM : Buffered at rotary speed of 10000 RPM
ABS : 2% ABS 98% Graphite / Acetone Solution
BRPM : Lowest Resistance out of 2000 / 10000 RPM
2HR : Data Recorded after 2 hours Electroplating @ 1V
4HR : Data Recorded after 4 hours Electroplating @ 1V
OS : Electroplating using Original Solution
NS : Electroplating using New Solution
Acetone / Graphene Solution Experiment
Spray + Burn 1 Layer 3 Layers Spray 1 Layer 3 Layers
+ Gr = None 800 300 + Gr = None 1200 800
+ Gr = 10% 700 150 + Gr = 10% 1100 750
+ Gr = 30% 550 60 + Gr = 30% 1000 700
Key:
+ Gr = Added Graphite
ALL UNITS ARE IN OHMS
Burn = Burnished
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A problem occurred during the preliminary stages of the project of that the
atomizer became clogged due to the graphite / acetone solution. An emulsifier
could be incorporated within the solution to reduce the pressure vapour within the
solution therefore allowing the solution to flow through the nozzle, reducing the
clogging. The atomizer is to be avoided due to this case.
It is found from the preliminary experimenting with the initial samples that
increasing the number of applied layers and buffering rotary speed, significantly
improves the coating quality. This reduces the overall electrical resistance
(OHM). However adding ABS into the conductive solution reduces this
improvement of the coat, it was initially theorised that this will increase the
bonding to which it may have done, but results have shown it decreases the
overall electrical resistance (OHM).
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4.2 Electrodeposition
4.2.1 Materials / Resource Requirements
During the electroplating stage, multiple techniques require use of a range of
equipment and materials, the list following shall consist of all equipment used for
all methods:
Power Supply / DC Unit
Glass Container (Preferably >250ml)
Power Supply Clips / Crocodile Clips
Oxalic Acid
Trisodium Phosphate
Ammonium Sulphate
Water (Preferably Distilled)
Copper Sulphate
Nickel / Copper Anode
Copper Rods / Bar BS EN 13604*
Copper Wire BS EN 12166*
Hydra* Copper Brightener
*Note materials / brands and British Standards are Ideal but not necessary.
Poor quality material will still perform the experiment sufficiently i.e. instead of
copper rod a 2 pence coin as the anode will still perform electroplating but
poorly.
It is found that alternative electrolysis solutions exist that may improve the quality
of the coat; however from existing patents and research this solution has been
46. 46
found to suffice to the needs of the project. The current solution is safe to apply
(Contains No Corrosive Chemicals) and is applicable to current resources. See
VI Applicable / Useful Patents, Standards and Safety Legislations for alternative
electroplating solutions.
4.2.2 Health and Safety
Health and safety are considered for all methods that require a certain degree of
preparation to avoid possible risks; the chemicals / materials used are relatively
safe to which skin contact with any of them listed will not cause harm. However
due to being pure chemicals it is recommended to wear protective goggles and
gloves whilst handling the materials.
Due to a majority of the chemicals listed, being used as baking products (Except
Copper Sulphate) it is relatively safe. However it is recommended to wear
protective goggles and gloves whilst handling the materials; however due to the
increased risk with ingestion or inhalation of copper sulphate it is strongly
recommended to wear protective goggles, procedure mask and gloves whilst
handling this chemical.
To see the Material Safety Data Sheet of any of the chemicals listed above see
Appendix 8.1.
The equipment used during electroplating are non-lethal, however the piece of
equipment that offers risk is the DC Unit. It is recommended to be aware of the
outgoing current which may cause electrocution.
See electric damaging scale to the right, to see how much current is harmful.
47. 47
Table 4 - Electricity Human Damaging Table - Oli Glaser. (Sep' 2011).1
Table 5 - Electrodeposition Phase Risks
48. 48
4.2.3 Method and Constraints
Electroplating the polymer conductive component uses methods which are
capable to be manufactured on an experimental, commercial and industrial level.
However the electroplating solution involving the following Ideal* mixture of
chemicals:
32g Oxalic Acid
10g Trisodium Phosphate
4g Ammonium Sulphate
950mL Distilled Water
5g Copper Sulphate
(1g Copper Brightener)
The above mixture excluding brackets is under a patent No US 7235165 B2 by
Richard Lacey. This allows experimental and scientific exploration uses, but
prevents commercial and industrial use; without patent consent. Patent No US
3715289 A by Stauffer Chemical Co uses a Brightener composition for acid
copper electroplating baths. In this instance this patent isn’t used but can be used
as a guide to improve the quality of the methods listed further in this report.
However the mixture of the chemicals mentioned above (including the bracket) is
currently not patented (Correct at April 2015); therefore it can be applied
privately, commercially and industrially without any legal consequences.
The solution used is relatively safe, however it is recommended to wear
appropriate PPE.
49. 49
The following are 8 phases of the electroplating stage:
1. The cathode (+) is the component that is to be coated and the anode is the
substance of the coat. The anode for this case shall be copper bar or
ideally copper wire. (Recommendation: Copper wire shall fully surround
the Cathode with a recommended length of 3 times the circumference of
inside the container)
2. The cathode is to be connected to the negative electric flow (-) via the DC
unit and anode to the positive. (Do not turn on the power supply till all
equipment is secure and set-up).
3. Using the crocodile clips to connect each substance, do NOT let the clips
become submerged in the solution as this will attract the copper ions
during electroplating and influence the components coat to be uneven.
4. During total submersion of the part at 1v for 2 hours. Rotate the
component to improve the uniformity of the coating. Repeat this stage by
incrementally increasing voltage by 1v (Maximum of 5v).
(Recommendation: Between each stage ensure that the solution is stirred
due to the instability of the copper sulphate within the electroplating
solution.)
5. If all phases mentioned previously have been followed and care has been
taken on each step the copper coating shall be bright, however complex
50. 50
parts may endure decolourisation upon the part; if this occurs repeat the
final submersion stage (5v for 30mins) as many times till satisfactory coat
has been performed.
6. If a copper coat is not satisfactory after phase number 5, check the
resistance of the Anode. Exposure of the anodes integrity can fall due to
material being converted into copper sulphate within the solution; or re-
buffer component and repeat. If problem persists there may be a fault with
the purity of chemicals, composition of solution or power supply failure.
7. During electroplating oxides and discolouration can occur, this is just a bi-
process of the electrodeposition phase. To overcome this copper
brightening agent should be used in-conjunction with the electroplating
solution; this dissolves the oxides and promotes uniformity within the
applied layers. If discolouration hasn’t occurred continue to step 8.
8. To improve the aesthetics of the coat quality, electroplate for 15 minutes
@1.5v, this produces fine copper grain growth and creating an overall
better post-electroplate look. Repeat if necessary.
9. Submerge in a solution of 10 parts water, 1 part brightener powder for 15
minutes to achieve a brightened component. See post-electroplated Yoda
below.
52. 52
4.2.4 Observations and Risks
Observations and experiments have been made with the appropriate coding’s
and results below.
Electroplating Sample Phase
Resistance in Ohms (10mm^2 and 20mm^2) Scratchable Rating
1L-BRPM-OS-2HR 80 C
1L-BRPM-OS-4HR 30 C
3L-BRPM-OS-2HR 10 C
3L-BRPM-OS-4HR 2 B
1L-BRPM-NS-2HR 60 C
1L-BRPM-NS-4HR 25 C
3L-BRPM-NS-2HR 10 C
3L-BRPM-NS-4HR >1 B
Key:
1L : 1 Layer of Graphite / Acetone Solution
3L : 3 Layers of Graphite / Acetone Solution
2RPM : Buffered at rotary speed of 2000 RPM
10RPM : Buffered at rotary speed of 10000 RPM
ABS : 2% ABS 98% Graphite / Acetone Solution
BRPM : Lowest Resistance out of 2000 / 10000 RPM
2HR : Data Recorded after 2 hours Electroplating @ 1V
4HR : Data Recorded after 4 hours Electroplating @ 1V
OS : Electroplating using Original Solution
NS : Electroplating using New Solution
53. 53
Scratchable Rating:
A: Unscratable, Very hard to remove coat
B: Hard, Scratable but takes effort to remove
C: Intermediate, Takes abit of pressure to remove
D: Soft, Little pressure needed to remove
E: Easily Scratched off, No or Little pressure needed.
From the electroplating sample phase results. Evidence has found that the increase
in applied layers and submersion time during electrodeposition is directly
proportionate to the electrical resistance and scratch able rating. However it is shown
that using the grey primer delivers a better post-electroplated sample.
From the results above, the general trend of the solvents performance can be shown
on a graph below.
54. 54
The trend is caused by the additional graphite content and mixture of solvents
which attribute for the application of this process. It is recommended that with
further research, the content of graphite in conjunction with a mixture of
adhesives, can improve the quality of the coatings. (See Appendices 8.3 Material
Data Safety Sheet MSDS – AUTOTEK GREY PRIMER MSDS)
The observational risks that can occur electroplating during the phase is that
exposure to high amounts of voltage can cause a degrading of a coat quality
During the submersion of the component in the electroplating solution, ensure
that the part is cleansed after submersion. This prevents a crystalline texture can
be caused due to solution drying and oxidizing on the surface. See Crystallized
Part below.
Post-Electroplated Crystalized Component
55. 55
5 MechanicalProperty Testing
5.1 HardnessTest
5.1.1 Results
The current experimental samples have been conducted upon the Vickers
Hardness Testing Machine. Below shows a table of the Hardness Vickers Rating
with the conversions into Pascal shown.
56. 56
Evidence shows that the conductive coatings solution added on the ABS sample
provides no additional hardness, however the application of copper for 4 hours of
sample 3L-10RPM-CP has shown a total hardness of 40% (215MPa) that of the
Anode; 3L-10RPM-CP-NP has been exposed for a total of 8 hours (4 for Copper
and 4 for Nickel) has shown a total hardness of 90% (540MPa) of the hardest
anode.
57. 57
5.2 Conductivity Test
5.2.1 SEM Images
The image to the right shows that
the acetone / graphite solution at a
magnification of 800x, with a scale
on the bottom right at 50 microns.
Notice how there are large contours
and the brightness of the sample
piece.
This is a basic indication of the
electrical conductivity between
samples (as long as the brightness /
contrast aren’t adjusted on the SEM
interface).
The image to the right shows that the
grey primer / graphite solution at a
magnification of 800x with a scale of
50 microns. Notice that this image
appears brighter and has less large
contours; this reflects electric conductivity as the SEM uses electrons bouncing of
a sample to develop an image. This shows that this image should have a lower
electrical resistance. From the results shown previously, this theory appears to be
correct.
Figure 3 - Acetone / Graphite Solution@800x
Magnificationon SEM
Figure 4 - GreyPrimer/ Graphite Solution
@800x Magnificationon SEM
58. 58
6 Conclusion and Recommendations
6.1 FurtherResearch Recommendations
6.1.1 Experimental / Commercial / Industrial Applications
The methods and material compositions used in both the conductive coating and
electroplating phases; are bound to no legal limitations for experimental,
commercial and industrial applications.
6.1.2 Conductive Coating Recommendations
The following are further application recommendations, which would have been
progressed to. However due to time and resource as the main constraint, this
feature has been developed to provide an insight to the planned further research.
Further advancements on the current processes, can be improved with the use of
a fine sand-blasting for the buffer phase. The parameters which will need further
research are the sand size and force per cm2. This has shown theoretical benefits
of reaching complex locations on the component, an increased homogenous of
the electro-resistance coat and more control over producing a low electrical
resistance. With the possible capability of developing an even lower resistance
rating than initially developed.
59. 59
The following are the benefits of sand blasting and the theoretical material
property advancements:
Homogenous Post-buffer coating
o Creating a more even electroplating coating
More Control over the Post-buffer Coating
o Due to constant force of blasted particles at the same
distance allows various conductivity ratings for various sizes
and materials.
Possibility of very low electroplating resistance than from methods
used initially
o Less Voltage needed to electroplate
o Less Time to coat
An additional recommended method that could be developed, will be vacuum
bagging of the component to compress the graphite grains. Theoretically
mimicking the burnishing phase, the following are the possible benefits:
Homogenous Post-Buffer Coating
Lower Removal of Material
Possible lower resistance achieved
60. 60
A materials / chemicals recommendation will to continue further study into a
higher applicable solution. From current studies it has shown that adding graphite
with the AutoTek grey primer has shown significant improvements than just
adding graphite to 95% pure acetone. Therefore below is the chemical list of
added materials with the majority being a mixture of butane, propane and
acetone. This provides the possibility that the mixture of solvents improves the
application. Below shows the current composition table of the AutoTek Primer
from Appendices 8.9 Material Data Safety Sheets.
During the bonding of the graphite particles, a certain percentage of added
graphite increases the connectivity until bonding is of excess; this can be
described as the percolation threshold. This is recommended to be further
researched to gain a broader knowledge on the optimum amounts of added
graphite.
61. 61
6.1.3 Electroplating Recommendations
Further Advancements on the current process enables multiple layers of coatings
to develop multiple material characteristics. The following are ambiguous
methods applicable from multiple layers:
Multiple coats including thermal protection, electrical conductivity,
increased impact / hardness / tensile properties etc.
A battery expert stated that “In collaboration of a zinc and copper coat
submerged in an electrolyte can essentially produce a battery which can
be used for applications that may be submerged in sodium, potassium,
calcium, bicarbonate, magnesium, chloride, hydrogen phosphate and
hydrogen carbonate” A.M. Rashidi. (2010).
A circulation pump within the electrodeposition tank can be developed to
aid the sulphates bond to the cathode evenly.
There appears to be room for improvement for the electroplating solution. From
the perspective of current resources and safety, practically the current solution is
acceptable for this application.
62. 62
6.2 Evolution of ExperimentalSample Results
From the preliminary experimental samples, the lack of expertise in theoretical
and practical applications created poor results. However with increased research
in specific elements of the process, the results can be shown to be progressed
visually with SEM statistics as evidence.
6.2.1 Initial Experimentation Sample Results
Initial methods of the application have shown to be significantly improved. Below
are the preliminary results from the lack of expertise, the methods have still
shown dramatic improvements to which all the methods where re-defined and
improved.
The graph above shows the application of the initial solution (Acetone and
Graphite) and the building up of layers to which are measured at 10mm2 and
20mm2.
1 Layer 2 Layer 3 Layer
10mm 4200 3500 1200
20mm 10000 7000 2000
4200
3500
1200
-2000
0
2000
4000
6000
8000
10000
12000
14000
16000
18000
20000
RESISTANCERATINGINOHMS
APPLIED LAYERS OF CONDUCTIVE SOLUTION
Conductive Resistance of Coating
Application
63. 63
The graph above shows the application of burnishing each layer between the
applications of layers for the Initial Solution.
The graph above provides evidence for the amount of hours exposed in the
electroplating phase decreases the resistance of the coating in OHMS.
The graphs provided the foundation to develop methods from to utilize the best
method for the application to get the desired material properties; this data was at
the preliminary testing stage.
1 Layer 2 Layer 3 Layer
20mm Burnished 5500 2100 1500
10mm Burnished 3200 1800 800
5500
2100
1500
3200
1800
800
0
1000
2000
3000
4000
5000
6000
RESISTANCERATINGINOHMS
APPLIED LAYERS OF CONDUCTIVE SOLUTION
Results after Burnishing Each Layer
400.0
160.0
3.4
0.0
50.0
100.0
150.0
200.0
250.0
300.0
350.0
400.0
450.0
1 2 3
RESISTANCERATINGINOHMS
HOURS EXPOSED IN ELECTROLYSIS
Resistance of Coating in Ohms
64. 64
The sample pieces created during experimentation, improved through trial and
error, each method was incrementally improved. This has reached the highest
quality due to the time constraints to which future recommendations has been
logged in 6.1 Further Research Recommendations.
Below shows a time view representation of
how visually the sample processes had
evolved which each step defined to the right.
1. Shows the initial sample to which the
copper powder used within the conductive
solution, a problem occurred with the quality
of the copper powder.
2. Once the conductive coating had
been of an acceptable quality, it was set-up
to electroplate to which the voltage was too
high and caused the coat to bubble.
3. The first sample showing the
successful low quality coat of copper.
4. A thicker coat was achieved, to which
3 layers of conductive coating and 8v
electrodeposition @30mins was used.
5. An increase in voltage made the
plating quality decrease which was the
cornerstone for low voltage.
65. 65
6. After many samples of tweaking the processes, the defining time and voltage
was achieved at 1volts for 2hrs. The copper coat can be clearly seen and
distinctive.
6.2.2 Implementing Experimentation Knowledge to Final Design
Once the methods where re-worked and defined to its current levels, work on the
Yoda model begun. This was particularly complex due to the variety of the
surfaces which became a model to test the boundaries and quality of the
methods.
YODA – 3D Printed Part RAW
The image to the left shows the PLA Yoda
model in the preliminary phase or Pre-
Conductive Coating Phase.
YODA – 3D Printed Post-Conductive Coating
Phase
To the right shows the post-conductive coating
completion applied on the part, to which the
successful coating solution (Grey Primer Mixed
with 10% Graphite + 10% Acetone) has been
applied onto the part, left to vapour off the
solvent and embed the graphite.
66. 66
The part was then burnished between each layer; this was repeated 3 times putting
a total of 3 layers applied. See 4.1 – Conductive Coatings for more details.
YODA – 3D Printed Post-
Electroplating Phase
The post-electroplating phase is
the effect of a total submersion and
electro-deposition of 6 hours using
the electroplating method in
section 4.2 electrodeposition.
YODA – POST-ELECTROPLATING-BRIGHTENER-SUBMERSION PHASE
The image (right) shows
the component which
has been brightened and
buffered repeatedly until
a higher level of quality
was achieved. However,
oxidisation within the
atmosphere created the
component to become
darker, tarnishing the
quality of the component over time.
67. 67
To the left shows the OHM ratings of the
YODA at particular phases of the
procedure, the area of measurement was
from the top of the head to the bottom of
the component being a length of 100mm.
The results above, provide evidence that the electroplating on a complex component
has been successfully in coverage. From tests, it is safe to assume that the
component gains the material property advantages recorded from the sample
pieces.
68. 68
6.3 External Constraints
Many constraints exist that can affect the timing and quality of a project; some can
be so critically damaging to even stop the project from developing. The two main
sectors of external constraints that exist are commercial and industrial; these shall
be discussed with actions to take to prevent them from occurring.
6.3.1 Industrial Constraints
Constraints exist industrially for this project via, any problem that can affect the
timing and quality of the project from developing; this could be from new technology
or new advancements in coating polymers; therefore making this method less
applicable.
6.3.1.1 Manufacturing
Manufacturing this project industrially can cause mass exploitation of the benefits
that this technology offers. It is theoretically possible to mass manufacture metal
coated polymer parts, also offering the possibility of customized mass manufactured
3D Printed Metal Coated parts; which are cost effective. The only major constraint is
the time it takes to print, cover in conductive coating and apply electrodeposition.
6.3.2 Commercial Constraints
Commercial constraints are constraints that occur, which affects the selling of the
methodological process applied to the polymer parts. To the right identifies
commercial constraints that could occur.
69. 69
6.3.2.1 Customer Needs
During the start of the project, customer needs where considered from the improved
material properties these methods offers. For instance the added hardness achieved
with the assumed thermal insulating capability could achieve the propeller blade
rotary testing for a plane; this requires thermal testing’s whilst retaining essential low
weight.
6.3.2.2 Selling Price
The selling price of the method will entirely depend on the complexity of the
component coating to which it will be hard to define a costing system for the part.
6.3.2.3 Quality Regulation
Due to the technology being new, regulation of the quality of the method will have to
be defined on the materials used. A possible definition of the regulation of quality
could be the comparison of the Anode to the final coat, the thickness achieved
and/or material properties gained.
6.3.2.4 Patenting
A patent gives the inventor / institute the exclusive rights to whatever they have
invented. This means that they are the only people / body who are able to
manufacture or sell the rights to manufacture the idea. This could be a constraint
because it would mean that all of the researched which has been conducted wouldn’t
be able to be used d be a waste of time if a patent already exists for coating of a 3D
printed part, which isn’t the case from the delivery of this report.(April 2015)
70. 70
6.4 Conclusion
6.4.1 Conclusive Introduction
Two main phases within the methodology of creating an electroplated 3D printed
model have been found. They are the conductive coating phase and the
electroplating phase; only applicable to 3D printed polymers.
6.4.2 Conductive Coating Conclusion
During the conductive coating phase, from the experimental results it has shown
that building up the coating layers whilst buffering in-between. Using grey-primer
as the solvent and increasing the acetone level, avoiding too high of a purity
gives a good quality pre-electroplating component.
6.4.3 Electrodeposition Conclusion
During the electroplating phase, from the experimental results it has shown that
using a low voltage induces small grain growth of the anode upon the cathode.
Adding Brightener to the electroplating solution has shown improvements in the
post-electrodeposition quality.
71. 71
6.4.4 Post-Treatment Conclusion
For the Post-Electroplating after treatment, soaking in brightener has shown
significant aesthetical improvements to which increases the hardness; as shown
in evidence on the scratch able test.
6.4.5 Hardness Conclusion
The hardness of the sample pieces are directly correlated to the hardness of the
anode and the submersion time during electrodeposition. From results shown in
5.1.1 nickel has been coated upon a copper sample which has shown significant
hardness improvements.
6.4.6 Final Conclusion
During this project it is found that the conductive coating method is universal to a
range of polymers so being applicable to most 3D printed polymers. The
electroplating phase has been found to be applicable to nickel and copper to
which different metals will require changes in voltage. This method is applicable
to a wide range of polymers and metals. The coatings of the samples have found
to achieve a 90% hardness value of that of the anode showing significant
engineering applications for 3D printed parts.
The following possible applicable usages of the coatings are as follows:
Thermal Insulation / Conductivity
Improved Hardness / Impact Resistance
Lightweight
Improved Strength
72. 72
Electrically Conductive
Improved Toughness
Chemical / Atmospheric Resistance
Experience has shown to be a tremendous benefactor to completing this
project, however the documentation of the experiences needs to be logged to
ensure other uses can continue from the author’s progression from the
recommended further research. Attached is the project diary and all other
support information to support future research.
73. 73
6.4.7 Project Costing
Below shows the Project Costings with assumed rates of pay for engineers, with
equipment and material costings including and time on processes.
74. 74
7 References
1Oli Glaser. (Sep' 2011). How much voltage is “dangerous”?. Available:
http://electronics.stackexchange.com/questions/19103/how-much-voltage-is-
dangerous. Last accessed 01/2015
2Prairie, E. (2009). Chemical Resistance. Available:
http://www.plasticsintl.com/plastics_chemical_resistence_chart.html. Last
accessed 01/2015
3Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis.
Kluwer Adacemic/Plenum Pulbishers, 689 p.
4Reimer, L. (1998) Scanning electron microscopy : physics of image formation
and microanalysis. Springer, 527 p.
5Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction
to TEM, SEM, and AEM. Springer, 202.
6Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press
(electronic resource)
7Schlesinger, M. (2010). Analysis of Electroplated Files using SEM techniques.
In: Snyder, D and Paunovic,M Modern Electroplating. Milan: Wiley. p637-642.
8J. E. Palmer, C. V. Thompson, and H. I. Smith(1987), J. Appl. Phys. 62, pg2492
9L. H. Chou (1991), Appl. Phys. Lett. 58, 2631 ~1991!.
75. 75
10A. Milchev (2002): Electrocrystallization, Fundamentals of Nucleation and
Growth, Kluwer Academic Publishers, 2002, 11.
11J.W.P. Schmelzer (2003): Mater. Phys. Mech., 2003, 6, 21.
12A.M. Rashidi. (2010). Effect of Electroplating Parameters on Microstructure of
Nanocrystalline Nickel Coatings. Electroplating. 1 (1), p1-5.
13Knowlton, K. (2006). The 2006 California Heat Wave. Impacts on
hospitalizations and emergency department visits. (1)(5), p1
14Davis, J (2004). Copper and Copper Alloys. 3rd ed. London: Pearson. p136.
15Gibson, I (2011). Additive Manufacturing Technologies. 2nd ed. London:
Pearson. p19-23
16Chua, C (2014). 3D Printing and Additive Manufacturing. 4th ed. London: World
Scientific Publishing. p34-56.
17 Pugh, S. (1991). Total Design . Cornwall: Addison-Wesley.
18 Covey, S. (1996). Total Design Methodology. London: Pearson..
76. 76
8 Appendices
8.1 Personal Learning
The start of the project involved the coating of 3D printed parts to which the
author had limited knowledge, therefore the beginning of the project involved a
major amount of researching to understand the processes and methods of
conductive coatings and electroplating. However from being a kinaesthetic
learner the author found this to be repetitive.
Therefore the author began studying whilst conducting research from the
knowledge gained from the journals with trial and error from experiments with
journals of electroplating as support. This enabled the author to visualize and
build upon the knowledge learnt by hand-on experiments to which progress
spurred the author to continue progress.
As the project neared the end and the addition of a new born baby, bringing the
project to the end became crucial, to which additional hours and training upon
the VHTM was conducted to finalize the improved material properties.
Successfully enough the improved material improvements and the aesthetically
improved Yoda became the icing on the cake to which the author feels major
progress has been made.
77. 77
8.2 ProjectDiary
Project Meetings Scheduled with Hadley
07/11/2014
The brief meeting about the project involved the possible processes involved in the
project and the following tasks to complete:
Streamline Specification and Plan to reflect meeting
Enquire access to the Tribology Lab
Develop sample pieces
Develop knowledge of application of coatings research
Develop knowledge of improved material properties
From now on research shall be made to develop a better understanding of the
processes.
The following processes shall be researched to gain sound knowledge and be able
to practically produce samples are:
Create Conductive Coatings which are applicable to ABS (3D printed part
material)
Electroplate parameters (Material, Solution, Voltage)
Chemistry knowledge of Acetone, Graphite, ABS and any relevant material
which shall also be used.
Safety Knowledge of the above Materials and Chemicals
18/11/2014
From the previous research made and development of the spec and plan has
progressed my report to develop a sample with a conductive surface.
During today’s meeting, we tried to apply a solution of acetone and graphite. This
infused the graphite to the surface therefore creating a conductive surface, we wiped
down the part with force to connect the graphite together.
This experiment worked surprisingly successfully as it seemed that the graphite was
embedded into the component it gave a highly conductive surface with minimal
removal during wiping down; we shall leave the ABS component to cure and check
the properties afterwards
78. 78
For the next meeting we shall have a brief meeting, with myself being scheduled to
provide ABS sample parts and apply a graphite and copper sample with one being a
mixture then the results will be initially checked via multimeter.
25/11/2014
During today’s meeting, we examined the conductivity of the sample piece to which
was highly conductive; therefore we approached using a solution with dissolved ABS
within the Acetone / Graphite. This gave a soft top coating which gave a low reading
on the multimeter.
Therefore burnishing graphite was looked at to which it improves the conductivity
coat due to burnishing arranged the graphite bonds.
02/12/2014
This weekly meeting involved experimenting with the 3 methods of sampling
applying from 1, 2 and 3 layers of each method therefore a total of 9 samples is
made. The methods are Graphite mixed with Acetone, Copper mixed with Acetone
and Graphite / Copper mixed with Acetone; these were applied to give results of
resistance per sample. I then took some equipment home and begun experiments of
electrolysis there.
06/01/2015
During this week’s there has been a change in direction to which the previous
experiments allowed us to enhance our experience in the coating and electrolysis of
the test pieces. Now the experiments shall be the following
Acetone / Graphene Solution
Experiment
Spray + Burn 1 Layer 3 Layers Spray
1
Layer
3
Layers
+ Gr = None
+ Gr =
None
+ Gr = 10%
+ Gr =
10%
+ Gr = 30%
+ Gr =
30%
Key:
+ Gr =
Added
Graphite
Spray Atomization
Burn = Burnished
79. 79
Therefore 12 sample pieces shall be made show the difference between burnishing
and not, the percentage of graphite added and the layers made. They shall be
controlled using an atomizer to completely expose the sample. The reason for
unburnished is due to the effect on complex parts which will not be easily burnished.
Updated Gantt Chart
06/01/2015 13/01/2015 20/01/2015 27/01/2015
Homo
Sol
Ap Sol
on TP
Rec Con
Elec
Plate
Rec Con
2
Key:
Homo
Sol = Homogenize the Solution
Ap Sol
on TP Apply Solution on Test pieces
Rec Con
= Record the electric conductivity
Elec
Plate = Electroplate sample pieces at set procedures
Rec Con
2= Record the electric conductivity of plated sample
The updated gantt chart shall replace the original for these new experiments due to
new findings.
13/01/2015
From the updated Gantt chart, the high shear homogenization of the Graphite
solution was unavailable due to the homogenizer lacking the required RPM to
produce graphene. Therefore is was put on at 2000 RPM for 2 hours.
This solution was then split to 3 solutions with the required percentage of ABS; 1st
with 0%, 2nd with 25% and 3rd with 50%. The percentage of ABS is in regards to
chemicals added to acetone therefore the 25% ABS had 75% of graphene and so
on.
During the application of the mixtures, there has been a failure during electroplating
which is do with the lack of conductive coating which, I suspect is a problem during
atomizing where graphene is blocking the pipe.
80. 80
Therefore from the results the new goals shall be to:
Find nozzle capable of spraying solution without clogging
Apply brushing solution on
Find the benefits of adding ABS into solution
Electroplate successfully
14/01/2015
During the failure of creating a high electrically conductive surface on the samples,
the problem has been amended by buffering each layer individually then applying a
new layer. This proved to be a highly positive method which produced a resistance
reading of 50 ohms from a 40ml Acetone / 2g Graphite solution with no ABS.
The added content of ABS has proved to be unsuitable for this application due to
buffering aligning the Graphite to increase conductivity the ABS prevents this and
whilst buffering results in a paste which is easily removed from the surface therefore
no ABS shall be used but buffering individual layers shall be used.
The application methods of spraying and brushing have both proved to be effective
whilst buffering each layer, to which spraying produced a smoother more
homogenous surface.
Gantt Chart Electrical Conductive Coating
Samples
14/01/2015 15/01/2015 16/01/2015 17/01/2015 18/01/2015
Ap
GrAcS
Cr Mix
Key:
Ap
GrAcS = Apply Graphite / Acetone Solution
Cr Mix = Create Mixtures of Graphite / Acetone
Gantt Chart Electroplating
Samples
14/01/2015 15/01/2015 16/01/2015 17/01/2015 18/01/2015
Rec
ROhms
ElecPlate
Key:
81. 81
Rec
Rohms Record resistance readings from conductive samples
ElecPlate Electroplate the sample pieces
Spray +
Burn 1 Layer
3
Layers Spray 1 Layer
3
Layers
+ Gr =
None
+ Gr =
None
+ Gr =
10%
+ Gr =
10%
+ Gr =
30%
+ Gr =
30%
These shall be started from the scheduled plan to which shall be updated within the
project diary and Gantt charts.
19/01/2015
During the graphite application the spraying developed problems due to only the fine
graphite passing through the nozzle with the larger parts becoming clogged and
causing problems therefore I have resorted to applying directly via brushing and
burnishing between layers.
The electroplating has become a success by producing a sample piece entirely
plated with a full coverage of 25Ω/10mm2. This was over an 8 hour period at 18v.
However, during the success of the nickel plating a sample piece, the uniformity of
the application increased but due to the increased voltage a greater amount of heat
1 Layer 2 Layer 3 Layer
10mm 4200 3500 1200
20mm 10000 7000 2000
4200
3500
1200
-2000
0
2000
4000
6000
8000
10000
12000
14000
16000
18000
20000
RESISTANCERATINGINOHMS
APPLIED LAYERS OF CONDUCTIVE SOLUTION
Conductive Resistance of Coating
Application
82. 82
was produced from crocodile clips; therefore considering faradays law, I shall reduce
the voltage to 6v and add 5 grams of copper sulphate to the solution; this shall in
theory speed up plating due to the copper sulphate and create a more even plate
due to the lower voltage.
20/01/2015
During the process of having the voltage at 6v with the addition of copper sulphate;
this proved successful with majority coverage of copper with very clear copper coat
upon the sample pieces.
Therefore to improve the homogenous of the coating a rotary buffer has been
purchased due to the realization that the quality of the coating is in direct correlation
to the quality of the buffered graphite; in theory this shall improve the speed of
coating (Due to a lower resistance from buffering) and quality of coat.
23/01/2015
The rotary buffer has arrived to which has significantly reduced the resistance of the
initial conductive coating from 300 Ohms (Buffered using Tissue) to 70 Ohms
(Buffered using rotary polisher) therefore the speed of plating shall significantly
improve.
Just placed a rotary buffered sample piece to be electroplated and in under 5
minutes @ 10 volts it has been fully plated, however the copper plate is easily wiped
off. This is due to the voltage increasing the heat of the graphite particles therefore
enabling them to be removed.
I shall no commence by comparing the copper coatings to the sample pieces, but
reduce the voltage.
24/01/2015
During reduction of the voltage from 10v to 1v for 10 minutes, the quality and the
adhesion of the coating has improved which backs up the theory of the graphite
particles being heated up and being easily removed, reducing the voltage reduces
the heat therefore enabling a better coat.
26/01/2015
A successful sample piece with a high quality coating has been developed using the
following method:
1v for 30 minutes
Remove sample piece, dry off and leave for 15 minutes at room temperature
1.5v for 30 minutes
Remove sample piece, dry off and leave for 15 minutes at room temperature
83. 83
2v for 30 minutes
Sample piece should have a high quality coat after finally drying.
This method has proved better than fully exposing the sample piece for 1.5hrs due to
the coating having time to cure.
This shall now be tried out on a complex part (the Owl) to check how well it coats
uneven surfaces.
30/01/2015
Due to the recent success of results on the sample piece, different polymer materials
and solvents to adapt the methods to become universal or slight tweaks dependent
upon materials / chemicals used therefore below shows a table of 4 solvents with
multiple polymers that are applicable, however due to safety and performance
Acetone is the solvent which is highly recommended.
Also the complex part coating has not yet been initiated but has been prepared for
electroplating exposure (Been rotary buffered to an acceptable resistance)
SEM training has been scheduled for the 2nd February in JB014 at 11am.
02/02/2015
SEM training has been completed today to which basic data on the most recent
sample piece using the 3 stage submersion in the electroplating tank.
With meeting with Hadley we discussed the processes and why the copper coating
was easily scratched off and we concluded that it was due to the electroplating
solution due to comparing plating techniques with multiple previously made
experiments.
This showed that currently, the samples were being electroplated for 2 hours,
however other groups who have completed a similar experiment expose there
samples for 4 hours therefore double the exposure time shall be made and a
commercial electroplating copper solution shall be used in conjunction with existing
methods just a change of the solution.
84. 84
03/02/2015
An Excel spreadsheet shall be developed showing the difference of resistance
(10mm2 & 20mm2) in ohms, from each electroplating method previously mentioned.
07/02/2015
The conductive coating has reached its peak capability in regards to combination of
electroplating solution and conductive paint. The assumed constraint is the
electroplating solution which when in process of plating, produces small hydrogen
bubbles on the surface which slightly disrupts the graphite layer. Therefore when the
surface is scratched removes the copper, so either adjustment of the conductive
paint, electroplating solution or anode.
The multiple layers of conductive coats have found to give a significantly reduced
resistance but decrease the wear resistance upon plating.
13/02/2015
Electroplating solution has been researched to which Midas Bright Electro-forming
Copper Solution (Copper Sulphate Solution) has shown great promise in increasing
wear resistance and maintaining the copper upon the coat.
20/02/2015
85. 85
Research into multiple conductive paints that replaces, the first proposed idea is to
replace acetone with lacquer or primer, following the same procedures the see if
there is a better result from a different a solvent.
The Midas electroplating solution has been ordered to which experiments using this
shall begin on or around the 28/02/2015.
22/02/2015/
A grey primer / graphite conductive paint has been produced, with burnishing
between layers… It has been noticed at this early stage that the resistance is not as
low as acetone, but still low producing a 600Ω/10mm2 , it is assumed due to the
impurities within the grey primer this may help in bonding the conductive coating to
the ABS sample, therefore helping the copper.
It has been placed in the safe electroplating solution @1.5 volts for 4 hours.
After 4 hours of electroplating on the primer / acetone solution the same has
achieved roughly 75% coverage with a noticeable increase in copper
electrodeposition. The sample shall remain electroplating for a further 4 hours to
assure full coverage.
The test has shown that the grey primer / graphite solution has a decreased post-
burnished resistance but from the post-plating sequence has shown an increased
wear resistance than the acetone counterpart.
During burnishing there is a noticeable difference between the grey primer / graphite
solution and the acetone / graphite solution, therefore, both burnished samples shall
have SEM images and a composition test to notice the difference between them.
26/02/2015
The SEM machine has been booked for 05/03/2015 at 11pm to gather composition
and imaging data to identify the bonding connection on a nano scale.
The grey primer / graphite solution has been deemed successful due to the
significantly increased quality of copper coat and material property capabilities. The
following are the materials and parameters used for the successful sample:
Grey Primer – Autotek (MSDS supplied)
Graphite Powder
Burnished between layers @ 2000RPM
Incremental increase in voltage from 1V to 5V over 16 Hours
86. 86
Incremental Rotation of Component during electroplating phase
Now that a standard procedure, that successfully works has been identified, fine
tuning of this process shall commence. With 3D printed components being produced
for functional applications of this process i.e. coated polymer cogs
02/03/2015
The SEM images developed have shown to be highly helpful in showing the
electrically conductive properties of the sample. (See the SEM images of the two
samples below) Notice on the 2 samples below that Grey Primer / Graphite Solution
appears brighter than the Acetone / Graphite Solution, this isn’t due to the adjusting
of the brightness but the conductivity of the sample piece, a good way to graphically
represent the electrical resistance.
95%+ Acetone / Graphite Solution SEM Image @ 50 Microns (Below)
Grey Primer / Graphite Solution SEM Image @ 50 Microns (Below)
87. 87
05/03/2015
From recent research I have found, having the correct grain growth is key to
developing a uniformed coat. This is to do with the solutions PH Levels, Temperature
and composition. So therefore I found a paper showing 55 degrees is optimum
temperature for nickel coating, so I applied this to copper and it failed, causing a
slight bubbling effect within the sample. Therefore from the failed sample, I have
placed an order for the copper brightener which should cause the most significant
increase in quality.
10/03/2015
The Brightener has arrived to which the following electroplating solution was created:
32g Oxalic Acid
10g Trisodium Phosphate
4g Ammonium Sulphate
950mL Distilled Water
3g Copper Sulphate
This created a shiny copper coating on a grey primer sample piece within 15 minutes
@ 1V.
The component was then soaked in a 200ml water / 3g Brightener Solution for 15
minutes.
88. 88
The next step shall be to create high quality copper coats
13/03/2015
The brightener solution needs to be dissolved within the solution @ 50c while
stirring, therefore a litre batch shall be made. Using the formula below.
1. Copper sulfate "powder" is actually made up of very fine crystals. The recipes
on the web contain instructions for mixing acid copper plating solutions using
both liquid copper sulfate (CuSO4) and crystalline copper sulfate pentahydrate
(CuSO4•5H2O). Go to: Acid Copper Plating Solution .
Specifically, you want 10 to 12 oz of copper sulfate crystals per gallon of
plating solution. To make up a single gallon of acid copper electrolyte, add:
o 25 oz (weight) or 1.6 cups (volume) 98% sulfuric acid to 3 quarts (12
cups) of COLD deionized. The solution will heat up VERY rapidly as
you add the acid so be VERY CAREFUL!!!
o Heat the solution to 60C (140F) and slowly stir in 10 oz. of copper
sulfate flakes. Stir until ALL of the crystals are dissolved.
o Add 0.63 cc of 35% HCl (hydrochloric acid) and 19 cc of Copper Gleam
PCM+.
o You have added a little less copper sulfate than you actually need but
the anodes, when they activate, will quickly make up the difference.
http://www.ami.ac.uk/courses/topics/0223_plate/index.html
16/03/2015
It has been found that the copper anode used initially was too high in contaminants
to cause a quality coating, therefore a high quality copper anode is recommended (at
least 95%).
89. 89
8.3 ProjectPlan and Specification
Project – MP 3997
Project: HB9 Functional Coatings for 3D Printed Parts
Tutor: Dr Hadley Brooks
Project Specification and Plan
Report By: Jonathan Ambrose
91. 91
Specification
Introduction
The project shall be based on embedding a surface hard coating upon a 3D printed part to
induce strength and durability.
This shall be done by using the theory behind applying a coating on a part by adjusting
treatments on sample parts to successfully produce a part which is cheaper, stronger and
more durable than it’s in use counter-part.
This studies main task is to embed the polymer part surface with a ferrous component and
successfully apply a metallic coating which shall improve the parts properties substantially;
whilst keeping the process simple, cheap and effective.
Aims
To achieve a surface coating upon a 3D engineered printed part, which shall have superior
strength during application; compared to a mass produced counter-part.
Information
Use of hardware such as the 3D FDM(fused deposition model) printer, Acetone Bath,
Electrolysis Bath and Equipment; and any other technical equipment to satisfy the needs of
the project.
Use of software such as SolidWorks, AutoCAD, ANSYS, FEA add-ons, MatLab; and any
other technical software to satisfy the needs of the project.
Theory
The theory behind the project is that to apply a surface coating to a 3D prototyped part. This
shall be achieved using a coating method for embedding the surface with ferrous material
mixed in the solution; once the ferrous material has been embedded into the part, the
coatings shall begin via PVD (physical vapour deposition) or CVD (chemical vapour
deposition).
Design
The design of the component shall be that of a mass manufactured part which requires strict
testing analysis; for example a propeller requires a fire test to ensure under certain
conditions it remains stable, however with one or more coatings; this shall be reduced and
substantially improve the components properties under usage.
Manufacture
The design shall be conceived using an appropriate CAD package and various amounts of
static and thermal analysis to ensure the component performs as needed; Inspire shall be
92. 92
integrated within the model to reduce weight and stress concentrations and allow for a
structurally viable component. Once the design has been verified to be feasible from data
using FEA, the component can then be prototyped using an in-house 3D printer.
Test
Sample parts shall be tested using appropriate material property testing equipment.
FEA integrated CAD packages shall be used to verify statistically, that under thermal and
static analysis it performs well within the factor of safety.
Risk
The embedding process may not embed the component evenly or may not allow the shell to
be an effective shell of the component.
The component may need multiple nanocomposite coatings to provide sufficient protection
and operational satisfaction; this is due to component legislation involved for passing
operational tests.
Plan
Main Tasks
Research Methods of surface coating and electrolysis application
Research into Coating Material to apply to ABS
Create sample parts using variable methods for impregnation
Perform Material Testing on a solid plastic, coated and solid metal component
Use FEA testing to check how component acts under force
From testing results, decide whether to produce component and apply best method
Compare and contrast in use component with prototype coated part
Time Scale
The time scale of the project shall include a Gantt chart on the assigned week date. It is
assumed that during the period of this project the activities within shall change and alter due
to unforeseen circumstances. The following are the tasks to be completed within the
scheduled instances for each report (in bold). (See Project Gantt chart)
Plan and Specification – 7th November 2014
Research Methods of surface coating and electrolysis application
Research into Coating Material to apply to ABS
Interim Report – 5th December 2014
Create sample parts using variable methods for impregnation
Perform Material Testing on a solid plastic, coated and solid metal component
Interview – 19th January 2015
Use FEA testing to check how component acts under force
From testing results, decide whether to produce component and apply best method
93. 93
Compare and contrast in use component with prototype coated part
Final Report – 1st May 2015
Interdependency between Tasks
The tasks dependent on being achieved to move on flow in a linear way other than a
complicated multi-task project.
The tasks can be split into four groups:
- Initial Stage
- Prototype Stage
- Coating Stage
- Testing Stage
The Initial Stage; Research, design and analysis are the first tasks to be completed before
any practical procedures can take place.
Then from the research, design and analysis the Prototype Stage can begin to which the
component can become developed with preparation for the coatings application beginning
in conjunction with the 3D printer.
The Coating Stage can begin once the coating preparation and research is complete. And
finally the Testing Stage can begin which compares and contrasts a similar industrial
component in regards to material properties and operation usage.
Critical Paths
See Appendix for Gantt chart and Critical Path.
Milestones
The milestones achieved shall be the following:
1. Completion of relevant research on coatings, embedding and electrolysis
2. Successful sample parts
3. Best method of coating application achieved
4. Create and coat prototype component
5. Compare and Contrast via Material Properties of Prototype
Indication of Resource Needs
Multiple resources shall be used when needed; this shall be indicated when a milestone has
been completed. The following are the milestones completed and the resources needed.
Complete milestone 1 and gain access to the Tribological Lab for Electrolysis research
Once milestone 1 is complete, the next resource will be the 3D printer to complete
milestone 2.
After the completion of milestone 2, the Ferrous Solution and Vapour Deposition will be
needed.
The coating material and application machines (electrolysis) will be needed once this is
complete from the results milestone 3 can be complete.
94. 94
Once the best method from the results is found and the processes have been
successful the prototype phase can be initiated with best method applied to this.
Then comparison to in use component shall be made to compare material properties.
97. 8.6 SEM Training Manual
FIRSTLY…
You have to book a time slot using the booking form in the SEMroom.
You must have relevant COSHH forms for your samples.
You must complete training before using the SEM. Contact Jim, Tamar or Hannah.
Remember to dispose of your sample accordingly and tidy up once you are finished.
SAMPLEPREPERATION
STICKY CARBON PAD
SAMPLE
ALUMINIUM STUB
1. Your sample must be dry.
2. From the drawer take an aluminium
stub and attach a sticky carbon pad on
top. Peel off the top layer and add your
sample on top.
3. If the sample is a powder use the air
duster to remove any loose particles.
4. Be careful notto overload the pad, think
about what you are looking for in your
sample.
5. If the sample is conducting no further
preparation is needed.
6. If the sample is non-conducting the
sample may need to be sputter coated
with gold.
98. 98
SPUTTER COATING
1. Place your aluminium stub with sample on into the sputter coater chamber. If you have
several samples run them in the coater at the same time.
2. Make sure that the lid of the sputter coater chamber is properly aligned over the seals
otherwise it will not start.
3. Press “Start” on the base unit. The display will countdown and the chamber will go into
vacuum. A purple glow will appear during the coating.
4. Whenthe machine hasfinishedthe chamberwillventandyouwill be able to lift the lid and
remove your sample ready for the SEM.
PUTTING YOUR SAMPLEIN THE SEM CHAMBER
1. The SEMmust always be in vacuum when not in use.
2. The chamber must firstly be vented. “Un-Pause” the
chambercamera byclickinginthe chambercamera box and
clicking the “Pause” icon on the top toolbar. The green
pause button will then disappear.
3. Click the “Vent” icon on the top right hand side and click
“Yes” in the pop up window.
4. Aftera fewminutesthe vacuum status on the bottom right
hand side will turn red and say “Vented”. You may now
open the chamber door and place your stub on the stage
using the gloves and tweezers provided.
5. Close the chamber and click “Pump”. Wait for the vacuum
status to go from “Pumping” to “Vacuum”. This will take
around 5 minutes.
99. 99
SPOT
SIZE
BEST USE
1,2 Very High Resolution (small
structures e.g. nano-particles)
3,4,5 Standard Imaging
6,7,8 EDAX, BSE
VIEWING YOUR IMAGE ON SCREEN
1. “UN-Pause” the top left box. The blue bar at the
bottom of the box indicates that it is active.
2. Click on the “HV” button on the right hand side and
choose a spot size using the table below. Use 20kV
voltage.
3. An image will begin to appear. Make sure the
magnification is at 50x to begin with. The
magnification can be altered by using the + and –
keys on the keyboard.
100. 100
9,10 Not Used
ACTIONS MOUSE/KEYBOARD
ZOOM + AND – KEYS ON KEYBOARD
CENTRE AREA OF INTEREST DOUBLE CLICK LEFT MOUSE BUTTON ON
SPECIFIC AREA
FOCUS CLICK AND HOLD RIGHT MOUSE BUTTON
AND MOVE LEFT OR RIGHT ACCORDINGLY
PRODUCING A GOOD QUALITY IMAGE
1. Firstlyadjustthe brightness/contrast.The simplestwaytobeginthis is to use the “auto adjust” icon on
the top lefthandside tool bar.You can thenuse the brightnessandcontrastbars on the right hand side
of the screen to make further adjustments.
2. Take into consideration your spot size (use the table to help).
3. You can adjust the rate at which the image refreshes. Use the Hare + and Tortoise – icons on the top
tool bar to increase or decrease the rate. Hint: higher refresh rate = poorer quality.
4. To focus on your sample hold down the right mouse button in the active box and slowly move left or
right according to your on screen image OR
5. Clickon the reduced area button on the top toolbar and use step 4 within the smaller box. To apply to
the whole image click outside the smaller box.
6. You will have to refocus your image every time magnification is altered.
7. To navigate around your sample double click the left mouse button on areas of interest.
ASTIGMATISM (correcting changes inthe beamshape)
1. Focus the image as well as possible.
2. Select the reduced area icon.
3. Bring the image out of focus in one direction and check for astigmatic distortion (image out of focus
unevenly).
4. Do the same in the opposite direction and look for a different distortion.
5. Bring the focus to the midpoint between the distortions.
6. Hold down the shift key and the right mouse button and a four headed arrow will appear.
7. Move this arrow slowly around the screen until the best focus is obtained.
It takes time and practice to produce a good quality image.You may have to carry out the steps
101. 101
HOW TO SAVEYOUR IMAGE
1. Firstly pause the active box usingthe “Pause”iconon the top tool bar. The icon will remain orange
until the final refresh is complete.
2. Once the pause icon is green click “File” and choose “Save As” from the drop down menu.
3. If you have not yetcreateda folderwithyourname doso and save all yourimages into said folder.
4. To save this onto a USB unplug the keyboard from the USB port at the back of the computer (do
not remove the mouse as it will break) and use that port.
5. Once you have copiedyourfilesontoyourUSB “safely remove hardware” otherwise the files may
not save on your USB.
6. Don’t forget to plug the keyboard back in once you have removed your USB.
CHANGING YOUR SAMPLE
1. Reduce magnificationto50x.
2. Change spotsize to 5 and turn off HV.
3. Pause the active box.
4. Ventthe chamber.
5. Carefullyremoveyoursample whenthe
chamberhas vented.
6. Insertnew sample andfollow instructionsas
detailedpreviously.
ENDING YOUR SESSION
1. Reduce magnification to 50x.
2. Change spot size to 5 and turn off HV.
3. Pause the active box.
4. Vent the chamber.
5. Carefully remove your sample when the
chamber has vented
6. Close the chamber door.
7. DON’T FORGET click on “Pump” to put the
chamber back into vacuum.
8. Select the box with the camera of the
inside of the chamber and pause it.
REMEMBER
If you are finishedwithyour sample remove
sticky pad from stub and dispose of
according to your COSHH.
Return stub to plastic bag.
If you need to carry out further SEM work
leave your sample stub in the sample box
provided.
Do not forgetto dispose once finished with.
Make sure the SEM room is clean and tidy
before you leave.
Any further questions contact Jim, Tamar or
Hannah.
109. 109
8.9 MaterialSafety Data Sheets (MSDS)
The following pages are split into individual
MSDS booklets for every material and chemical
used within the project.
