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1. Student : M. Imam Mawardi
Advisor : Yih-Chien Chen
LiNiVO4

2. Experimental Procedure
Prepare Material :
Li2Co3(99%)
NiO(99.97%)
O5V2(99.6%)
Material weighing
process
Ground with zirconium ball in
distilled alcohol for 12 h and then
dried
Calcination at 625 for
2h ,increasing temp for 4 ℃
per Min
Ground with zirconium ball in
distilled alcohol for 12 h, then
dried at 100 ℃ for 4 hour
XRD (calcine)
Added PV
Aas a binder
and sieved with a 200 mesh
Press into pellets with 10 mm in
diameter and 5 mm in thickness
under the pressure of 4000 kg/cm2
Sintering at 625 -700
℃ ,per step 5 ℃
XRD
(Sintering )
Bulk Density
Refinement
Dielectric properties εr Q x f

3. Calcined Processing
.We have 6 samples that to test with the different temperature ,increasing by 4
degree per minute .powder
SAMPLE
1
SAMPLE
2
SAMPLE
3
SAMPLE
4
SAMPLE
5
SAMPLE
6
Step 1 300℃
for 1.15
hour
400℃
for 1.40
hour
450℃
for 1.53
hour
500℃
for 2.05
hour
550℃
for 2.18
hour
600℃
for 2.30
hour
Step 2 stable 300
for
4 hour
stable 400
for
4 hour
stable 450
for
4 hour
stable 500
for
4 hour
stable 550
for
4 hour
stable 600
for
4 hour
BACK

4. XRD of LiNiVO4
Calcining
Temperature
(℃)
2 Theta
(degree)
300 43.312
400 43.270
450 43.182
500 36.138
550 36.140
600 36.113
The X-ray diffraction patterns of LiNiVO4 ceramics
calcined for 4 h .
BACK
Ionic Radius
Li1+ 0.76 Å
Ni2+ 0.69 Å
V5+ 0.54 Å
O2- 1.40 Å

5. XRD of LiNiVO4
Calcining
Temperature
(℃)
2 Theta
(degree)
550 36.140
600 36.113
625 36.05
650 36.15
The X-ray diffraction patterns of LiNiVO4 ceramics
calcined for 4 h .
BACK
Ionic Radius
Li1+ 0.76 Å
Ni2+ 0.69 Å
V4+ 0.58 Å
O2- 1.40 Å

6. Percentage Phase
Temp
(° C)
Main
Phase
(a.u)
Second Phase
(a.u)
Percentage Phase
(%)
LiNiVO4
NiO LiVO3 V4O9 Main
Phase
NiO LiVO3 V4O9
300 0 675 141 68 0 76.4 15.95 7.69
400 79 753 314 112 6.28 59.9 24.96 8.9
450 488 345 559 77 33.22 23.5 38.05 5.24
500 1126 316 201 36 67.06 18.8 11.97 2.14
550 1310 229 123 43 76.83 13.4 7.214 2.52
600 1806 25 120 0 92.57 1.28 6.151 0
625 1573 0 0 44 97.279 0 0 2.72
650 1664 0 0 47 97.253 0 0 2.75

7. Sintering Percentage size
Temp Before After Percentage(%)
625
5.05 4.93 97.67
10.03 9.86 98.28
650
5.06 4.93 97.33
10.01 9.81 98.00
675
5.01 4.88 97.46
10.07 9.69 96.23
700
5.03 4.82 95.83
10.06 9.54 94.86

8. NOTED
 SEARCHING THE TEMP OF SINTERING WITH THE PAPER REFERENCE ,
 TEMPERATURE INCREASING PER 5 DEGREE PER MENIT

9. Data Measurement
Name D L f01 IL1 BW1/2 K
625@1 9.96 4.50 16.788 -25.158 39.725 6.96637
2 10.01 4.78 16.206 -18.699 30.174 6.90583
3 10.00 4.90 16.072 -18.486 31.5785 6.81490
650@1 9.87 4.85 17.072 -17.047 99.395 6.16286
2 9.88 4.80 17.157 -17.047 99.395 6.17514
3 9.84 4.70 17.280 -17.047 99.395 6.26920
675@1 9.77 4.64 16.961 -19.608 35.675 6.56794
2 9.77 4.79 17.250 -19.608 35.675 6.17801
3 9.78 4.82 17.196 -19.608 35.675 6.16460
700@1 9.57 4.71 17.198 -20.300 38.071 6.45543
2 9.57 4.59 17.096 -19.478 35.0885 6.74901
3 9.64 4.69 17.223 -18.768 50.6 6.43268

10. Data Measurement εr
Name D L f01 IL1 BW1/2 K
625
1 9.96 4.50 16.788 -25.158 39.725 6.96637
2 10.01 4.78 16.206 -18.699 30.174 6.90583
3 10.00 4.90 16.072 -18.486 31.5785 6.81490
650
1 9.87 4.85 17.072 -17.047 99.395 6.16286
2 9.88 4.80 17.157 -17.047 99.395 6.17514
3 9.84 4.70 17.280 -17.047 99.395 6.26920
675
1 9.77 4.64 16.961 -19.608 35.675 6.56794
2 9.77 4.79 17.250 -19.608 35.675 6.17801
3 9.78 4.82 17.196 -19.608 35.675 6.16460
700
1 9.57 4.71 17.198 -20.300 38.071 6.45543
2 9.57 4.59 17.096 -19.478 35.0885 6.74901
3 9.64 4.69 17.223 -18.768 50.6 6.43268

11. Data Bulk Density

12. Data Bulk Density
Sintering Temperature (°C) No W water(g) W wet in air(g) W dry in air(g) BULK
DENSITY
625
1 0.872 1.245 1.138 4.278
2 0.821 1.174 1.07 4.297
3 0.886 1.266 1.157 4.269
4 0.818 1.169 1.067 4.285
650
1 0.901 1.271 1.175 4.288
2 0.899 1.267 1.168 4.342
3 0.883 1.251 1.173 4.045
4 0.899 1.276 1.173 4.281
675
1 0.885 1.236 1.152 4.315
2 0.898 1.258 1.173 4.265
4 0.903 1.26 1.178 4.284
700
1 0.885 1.22 1.159 4.230
2 0.876 1.207 1.145 4.257
3 0.896 1.236 1.171 4.258

13. 97.0
97.2
97.4
97.6
97.8
98.0
98.2
98.4
98.6
98.8
99.0
99.2
625 650 675 700
Relative Density
Data Relative Density

14. Name
εr Q Q x f
625
1 7.2 361.5 4252
2 6.2 237.5 2292
3 6.6 334.0 3277
650
1 7.1 335.3 3088
2 9.9 134.9 1267
3 9.7 100.1 931
675
1 7.5 127.3 1199
2 7.6 85.2 806
3 6.9 173.8 1652
700
1 10.1 241.6 2225
2 10.3 84.4 790
3 7.3 107.3 1004
Data εr and Q x f

15. Data εr and Q x f
0
500
1000
1500
2000
2500
3000
625 650 675 700
Qxf
0.0
2.0
4.0
6.0
8.0
10.0
12.0
625 650 675 700
Dielectric Constant

17. Data XRD (Sintering)
Sintering
(℃)
2 Theta
(degree)
Intensity(
a.u)
625 36.25 1205
650 36.3 1258
675 36.2 1455
700 36.25 1423
Ionic Radius
Li1+ 0.76 Å
Ni2+ 0.69 Å
V5+ 0.54 Å
O2- 1.40 Å

18. Percentage Phase
Temp
(° C)
Main Phase
(a.u)
Second Phase
(a.u)
Percentage Phase
(%)
LiNiVO4 NiO NiV2O6 Main Phase
NiO NiV2O6
625 1205 66 - 94.80 5.19 -
650 1258 53 - 95.95 4.04 -
675 1455 70 - 95.40 4.59 -
700 1423 67 80 90.64 4.26 5.09

19. Refirement 625 ° C
Parameter
X2 2.005
Rwp 7%
wp 5%

20. Refirement 700 ° C
Parameter
X2 1.837
Rwp 6.8%
wp 5%

21. Planning Pva Burning with 600 ° C
D=10mm
h=5 mm
D=10mm
h=3 mm
XRD Tcf SEM εr

22. Planning Sintering Temperature
0 ° C
600 ° C , 2 h
Sintering Temperature ° C , 4h
Sintering
Temperature(°
C)
625
650
675
700
5° C/m
5° C/m

23. Data Bulk Density
Sintering Temperature (°C) No T water(gf) T wet in air(gf) T dry in air(gf) Bounfary BULK DENSITY
625
1 0.905 1.273 1.186 0.281 4.220640569
2 0.906 1.272 1.184 0.278 4.258992806
3 0.904 1.269 1.18 0.276 4.275362319
4 2.168 3.141 2.817 0.649 4.340523883
650
1 0.907 1.268 1.185 0.278 4.262589928
2 0.907 1.270 1.185 0.278 4.262589928
3 0.907 1.266 1.184 0.277 4.274368231
4 2.163 3.141 2.823 0.66 4.277272727
675
1 0.910 1..267 1.188 0.278 4.273381295
2 0.904 1.257 1.178 0.274 4.299270073
3 0.908 1.265 1.186 0.278 4.26618705
4 2.171 3.122 2.836 0.665 4.264661654
700
1 0.892 1.227 1.164 0.272 4.279411765
2 0.898 1.232 1.173 0.275 4.265454545
3 0.899 1.236 1.175 0.276 4.257246377
4 2.192 3.103 2.860 0.668 4.281437126

24. Theory Temp(° C) Bulk
Relative
Density(%)
4.326 625 4.251665231 98.3
4.326 650 4.266516029 98.6
4.326 675 4.281965864 99.0
4.326 700 4.267370896 98.6
98.2
98.3
98.4
98.5
98.6
98.7
98.8
98.9
99.0
99.1
625 650 675 700
Percentage(%)
Temperature ° C
Relative Density
Pattern of Relative Density

25. Result with Cavity Measurement
Temp no εr Q Q x f
700
1 10.1 241.6 2225
2 10.3 84.4 790
3 7.3 107.3 1004
Q=1/0.00285=350.877
Qxf =350.877*14.749=5175.08

26. S.T(° C) εr Q Q x f
625 16.5 813 13,276
650 16.6 598.8 9724.55
675 16.54 813 13,454.47
700 18.2 719.42 11,471.9
Result with Cavity Measurement

27. 16
16.5
17
17.5
18
18.5
600 625 650 675 700 725
εr
5,000
6,000
7,000
8,000
9,000
10,000
11,000
12,000
13,000
14,000
600 625 650 675 700 725
Qxf
4.25
4.255
4.26
4.265
4.27
4.275
4.28
4.285
600 625 650 675 700 725
Bulk density

28. Result with resonator Measurement
TEMP NO D L F01 IL1 BW1/2 F02 IL2 BW2/2 K Q
625
1 10.01 4.56 15.848 -32.65 27.174 11.175 -6.1695 53.02 7.67346 155.85
2 10 4.56 15.839 -35.9 48.319 11.162 -6.43 40.548 7.68812 615.156
650
1 9.97 4.51 15.815 -31.918 33.466 11.255 -6.2226 51.945 7.839 184.8
2 9.98 4.44 15.799 -34.251 41.568 11.143 -5.907 51.68 8.001 246.3
675
1 9.95 4.40 15.802 -30.686 26.423 11.078 -5.3117 50.325 8.118 194.26
2 9.9 4.35 15.786 -30.014 32.718 11.166 -5.398 42.699 8.571 249.405
700
1 9.66 4.44 15.466 -37.960 24.017 11.028 -5.2364 42.699 8.5715 249.405
2 9.67 4.40 15.465 -34.986 40.91 10.768 -4.511 151.225 8.66498 56.0676

29. 4.25
4.255
4.26
4.265
4.27
4.275
4.28
4.285
600 625 650 675 700 725
Bulk density
7.6
7.8
8
8.2
8.4
8.6
8.8
600 625 650 675 700 725
K
0
500
1000
1500
2000
2500
3000
3500
4000
4500
620 630 640 650 660 670 680 690 700 710
Qxf