Ceramics UK 2019 presentation

1. SO WHAT HAVE WE MADE?
A TESTING OVERVIEW
Dr Richard White
Principal Consultant - Materials
10th July 2019

2. Scope of talk
− Why Analyse?
− Accuracy and Precision
− Stepwise approach to testing
− What are the gaps?

3. Why analyse anything?
− QA
− QC
− Compliance
− Confirmation of raw material quality
− Process Control
− Intermediate step control
− Fit for Purpose
− Does what it says on the tin.

4. What are we going to measure?
ProcessMaterials
Performance
Structure
Raw Materials
Chemistry
Mineralogy
Particle size
Surface area
Porosity
Pore structure
Bonding mechanism
Mineralogy
Surface layer
structure
Strength
Aesthetics
Toughness
Thermal properties
Inertness
Monitor
Milling
Blending
Thermal Cycle
Intermediates
Completion of
reactions

5. How to complete the loop
− Highlights the importance of Sampling and Analysis
− A weak link could compromise the decision made and action taken.
Material ActionDecisionDataSample Analyse

6. Sampling
− Will the sample answer the question posed?
− Is it representative?
− Is it statistically representative?
− Is it uniformly dispersed?
− Has it been contaminated or altered?

7. Analysis
− Will the sample answer the question posed?
− Is it specific?
− Is it sufficiently sensitive?
− Will it measure in the appropriate range?
− Will it work for the specific material concerned?
− Do we know that it works?
− Is it sufficiently accurate?

8. Precision and accuracy
Bias
− High Precision Low Accuracy.

9. Precision and accuracy
− Low Precision High Accuracy.

10. Precision and accuracy
− High Precision High Accuracy.

11. Precision and accuracy
Reality
?

12. Areas of analysis and characterisation
− Chemical Analysis
− Mineralogical Analysis
− Physical Properties
− Microstructure
− Performance properties.

13. Chemical analysis
− Inorganic/Organic?
− Major element - Minor element - Trace element
− Is it bulk or leachable or extractable?
− How fast does it need to be?

14. Chemical analysis

15. Chemical analysis - choice of technique
XRF AAS ICP-OES ICP-MS IC
Range of Elements Na - U Metals Metal ions Mass of ions Anions
Range 0.05-100% 100 ppm to % ppm to % ppb to ppm 0.1 to 10%
Form Powder Solution Solution Solution Solution
Discrimination X-rays
Light
absorbance
Light Emission Mass Time
Overlaps Yes Yes Yes Yes Yes

16. Chemical analysis - results
Wt % A B C D E
SiO2 35.21 30.34 17.59 41.12 14.35
TiO2 0.56 0.69 0.29 1.32 0.27
Al2O3 46.90 64.24 76.02 53.51 79.49
Fe2O3 0.41 0.52 0.21 0.66 0.30
CaO 0.22 0.13 0.15 0.22 0.17
MgO 0.97 1.90 0.19 1.00 0.15
K2O 1.99 1.11 1.17 1.49 1.14
Na2O 1.22 0.31 0.83 0.57 0.93
Mn3O4 0.01 0.04 3.39 0.01 2.90
ZrO2 12.53 0.31 <0.02 0.06 <0.02
Loss 0.17 0.17 0.03 0.06 0.03
Total 100.19 99.76 99.87 100.02 99.73

17. Mineralogical analysis - X-ray diffraction
Unique fingerprint of
mineral structures
Quantification
n λ = 2d sin θ

18. Corundum Al2O3 35.2 0.8
Quartz SiO2 51.2 10.0
Periclase MgO 13.6
Cordierite Al4Mg2Si5O18 100
Spinel MgAl2O4 48.0
Cristobalite SiO2 51.2
Forsterite Mg2SiO4 41.0
Mullite Al6Si2O13 49.0
Steatite Mg3Si4O12 40.8
Andalusite Al2SiO5 55.4
Tridymite SiO2 3.8
Minerology
− Al2O3 35.2%, SiO2 51.2%, MgO 13.6%

19. Physical properties - particle size

20. Microstructural evaluation
− Image of Surface
− Topographic visualisation
− Compositional variations
− Elemental data from regions of interest
− Morphology - size - structure - chemistry.

21. Microstructures

22. Performance evaluation

23. What tests to do?
− Compliance or Regulatory Testing ✓
− Key performance tests for application ✓
− Or identify key influencing properties and measure
− Or tight control of process and monitor all steps and
intermediate points.

24. Your product – we now know that…
− … the chemistry complies
− … the correct mineralogy has formed
− … the physical properties match
− … the microstructure is appropriate
− … It functions correctly
− But?
− Do we really understand the material?
and what makes it work?
− If something goes wrong can we recover?
− Do we know how to improve it?
− How good could it be?

25. Thank you
Contact details
T +44 (0)1782 764262
M +44 (0)7813 344103
E richard.white@lucideon.com
W www.lucideon.com