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Texas Instruments Synthesis and characterization of nickel manganite Application notes
Signal Conditioning: Thermistors
Texas Instruments Incorporated
Synthesis and characterization of nickel
manganite from different carboxylate
precursors for thermistor sensors
By R.K. Kamat, Electronics Section, Department of Physics, Goa University, Goa, India (email: rkkamat@unigoa.ernet.in),
G.M. Naik, Electronics Section, Department of Physics, Goa University, Goa, India (email: gmnaik@unigoa.ernet.in),
and V.M.S. Verenkar, Department of Chemistry, Goa University, Goa, India (email: vmsv@unigoa.ernet.in)
Introduction
The thermistor sensor is a widely used temperature transducer synthesized with a ceramic-like semiconductor
material. Its basic temperature-sensing mechanism is the
population of charge carriers in the conduction band.
Initially the thermistor was designed for use during World
War II, but since then it has continuously evolved for
applications such as thermometers, temperature controllers, automatic gain control, and time-delay circuits. Its
number of applications is increasing rapidly, encompassing
office automation equipment, air conditioners, and other
domestic appliances. Recently the thermistor has come
into the limelight due to its use in portable phones, car
phones, and transceivers. Expanding applications in delicate communications equipment and the rapid influx of
such equipment into the consumer market has forced
thermistor manufacturers to consider improving the specifications. In this article the authors investigate various
thermistor anomalies from a materials point of view.
Figure 1 shows thermistor samples we manufactured in
various sizes. The small samples are suitable for applications where speed of measurement is crucial.
The thermistor sensor offers various advantages: high
sensitivity; availability in a large range of resistance values
(useful from a power dissipation point of view); ability to
Figure 1. Thermistor samples
operate over a wide temperature range in a solid, liquid, or
gaseous environment; adaptable size and shape for a wide
variety of mechanical environments; ability to withstand
electrical and mechanical stress; and low cost. At the same
time, this sensor has several limitations: lack of interchangeability; poor linearity and precision; limited range;
instability at high temperatures; hysteresis; and low resolution. With the advent of microprocessors and microcontrollers, most of these drawbacks are no longer a problem
except for lack of interchangeability. The authors investigate remedies for the bottlenecks posed by thermistors in
References 16, 17, and 18. On several occasions we observed
that the thermistor-based circuit needs tuning when it is
changed. The reasons for lack of interchangeability are
loose manufacturing standards and manufacturers’ ignorance of standard material characterization tools used to
check completion of solid-state reactions (formation).
Materials used
At present the thermistor materials of interest and use are
mixed metal oxides (especially spinels) of manganese,
nickel, cobalt, copper, iron, and titanium. The authors of
References 1–5 show an interest in transition metal manganite, Mn3-xMxO4 [(0 < x < 1) and M = nickel, cobalt,
etc.]. Nickel manganite, NiMn2O4, is a popular material for
thermistors despite its poor stability at high temperature.
The electrical conductivity is due to hopping between
Mn3+ and Mn4+ ions in the octahedral sub-lattice of the
spinel structure. In this article the carboxylate precursor
method, used for the first time to synthesize NiMn2O4, is
described. The different carboxylates used for precursor
formation are fumarate, succinate, oxalate, tartarate, and
malonate. The precursors as well as the NiMn2O4 obtained
by thermal decomposition of these precursors have been
characterized by X-ray diffraction, infrared analysis, and
thermal analysis to study the formation and working.
Preparation
Different nickel manganese carboxylate precursors were
prepared by using salts of carboxylic acid and metal chlorides. Following is a description of how the metal chloride
solution and the precursors were prepared.
Preparation of metal chloride solution
Around 11.8854 g of NiCl2.6H2O (0.5M) was accurately
weighed on a Mettler balance and dissolved in distilled
water. Similarly, 19.79056 g of MnCl2.4H2O (1M) was also
accurately weighed and dissolved in acidified water [to
prevent formation of Mn(OH)2]. Both salt solutions were
52
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February 2001
Analog Applications Journal
Signal Conditioning: Thermistors
Texas Instruments Incorporated
then mixed together to make the volume 100 ml in a standard volumetric flask. This metal chloride solution was
then used for the preparation of the nickel manganese
carboxylate precursors.
Preparation of nickel manganese fumarate (NMF)
weighed and placed in silica crucibles, then heated in an
oven for 20 minutes at various temperature ranges until
the precursors exhibited no further weight loss. TGA was
done on an STA 1500 instrument in air at a heating rate of
10ºC/min. DTA was recorded on an STA 1500 instrument
in air at a heating rate of 10ºC/min.
Sodium fumarate was accurately weighed at 32.008 g (2M)
and dissolved in distilled water; the total volume was
made 100 ml in a standard flask. This solution was then
heated to 80ºC. The hot metal chloride solution was added
drop-by-drop, with constant stirring, to this hot fumarate
solution. The precipitate of nickel manganese fumarate
that formed was filtered in a Buchner funnel using a
Whatmann filter No. 41. It was washed with distilled water
until it was free of chloride ions, then dried with diethyl
ether and stored in a desiccator.
X-ray diffraction of the sintered and decomposed products
was carried out on Philips X-ray Diffractometer model PW
3710 with Cu Kα radiation and nickel as a filter. The studies were carrried out to confirm the completion of solid
state reaction, observe the impurity phases, and determine
lattice constants, interplanar distances, octahedral and
tetrahedral site radii, bond length, X-ray density, etc. The
various parameters were calculated using standard values.
Preparation of other precursors
Formula fixation
The other precursors—nickel manganese succinate
(NMS), nickel manganese oxalate (NMO), nickel manganese tartarate (NMT), and nickel manganese malonate
(NMM)—were also prepared in the same manner as
described for NMF by using sodium succinate, ammonium
oxalate, sodium tartarate, and sodium malonate, respectively, along with metal chloride.
Characterization
The nickel manganese carboxylate precursors were characterized by chemical analysis. The NiMn2O4 obtained by
thermal decomposition of the carboxylate precursors was
also characterized by X-ray diffraction and IR analysis.
The results of all the characterizations are summarized in
Tables 1-9.
X-ray diffraction (XRD) analysis
Based on the characterization results previously described,
a formula for each precursor was fixed as follows:
NMF: NiMn2(C4H2O4)3.41/2H2O
NMS: NiMn2(C4H4O4)3.10H2O
NMO: NiMn2(C2O4)3.61/2H2O
NMT: NiMn2(C4H4O6)3.8H2O
NCM: NiMn2(C3H2O4)6.3H2O
Pellet formation
Some of the steps in thermistor manufacture are shown in
Figure 2. The thermistors were fabricated by preheating,
presintering, grinding, and shaping them to the desired
geometry and by a final sintering at elevated temperature.
The thermally decomposed product of the precursors was
preheated in a silica crucible to 400ºC to drive off
Chemical analysis
The percentage of nickel and manganese in the precursors
was estimated by using the standard methods described in
Reference 23. The elemental analysis was carried out on
an AAS 201 Chemito GBC902, double-beam atomic
absorption spectroscope. The wavelengths used for nickel
and manganese estimation were 352.4 nm and 403.1 nm,
respectively. The standard solutions prepared for nickel
and manganese were in the range of 6 to 25 µg/ml and 7 to
27 µg/ml, respectively.
Continued on next page
Figure 2. Some steps in thermistor manufacture
IR analysis
IR analysis of the precursors and their decomposed products was carried out on Shimadzu FTIR instrument model
8101A. The pellets used for reading spectra were prepared
by mixing 1 to 2 mg of the sample with a pinch of KBr.
The IR spectra in the range of 400 to 4600 cm-1 was
recorded at room temperature.
Density measurement
The pycnometric density measurement of the precursors
and their decomposed products was determined at room
temperature with CCl4 as the medium by using the formula
psample = (weight of the sample)/(weight of the liquid
displaced/density of the liquid).
Thermal analysis
The physical and chemical properties of the precursors
were monitored by using thermal analysis techniques like
isothermal weight loss studies, thermogravimetry analysis
(TGA), and differential thermal analysis (DTA). For
calculating the weight loss, precursors were accurately
The light-colored powder at the top is raw precursor. Below that is
pre-sintered powder before and after it is finely ground and filtered.
The weight loss that results is evident. Compressing the sintered
precursor in a hydraulic press produces the finished thermistor.
53
Analog Applications Journal
February 2001
Analog and Mixed-Signal Products
Signal Conditioning: Thermistors
Texas Instruments Incorporated
of carboxylate ions was seen in the range of
1550 to 1625 cm-1 and 1350 to 1400 cm-1, respectively,
with ∆ν (νasys - νsys) separation of ~190 to 240 cm-1, indicating the monodentate linkage of both carboxylates in
the dianions. Thus the carboxylates coordinated to the
metal as bidentate ligand via both carboxylate groups.
Almost all the hydrate nickel manganese carboxylate precursors decomposed below 400ºC to form NiMn2O4. Most
of the dehydration took place below 250ºC, while the
decarboxylation of anhydrous precursors occurred
between 250 and 400ºC. XRD confirmed the formation of
NiMn2O4. The lattice parameter values of all the samples
agreed well with the reported ones. The IR data of
NiMn2O4 showed high-frequency band ν1 between 600
and 620 cm-1 and low-frequency band between 450 and
460 cm-1. The I-V characterization of all the samples up to
200ºC with four-probe setup revealed their thermistor
behavior. The low value of resistivity at room temperature
was attributed to the presence of moisture.
Continued from previous page
moisture. The preheated product was mixed thoroughly
by grinding and then was compressed under 5 tons per
square inch of pressure in a hydraulic press in a round die.
These pellets were then heated to 900ºC under a controlled temperature profile using a PID controller. The
final products were disc thermistors with diameters of
1 mm (0.04 in.) to 3 mm (0.12 in.), targeting low-cost
thermometry applications for domestic use.
Results and conclusion
This article presents our work on the preparation of nickel
manganese carboxylates by various precursor methods;
viz., nickel manganese fumarate, nickel manganese
succinate, nickel manganese oxalate, nickel manganese
tartarate, and nickel manganese malonate. Various characterization tools were applied to these precursors to verify
the formation. The asymmetric and symmetric stretching
Table 1. Infrared data of hydrated nickel manganese carboxylates
CARBOXYLATES
NMF
NMS
NMO
NMT
NCM
ν(H2O)
3475
3400
3400
INFRARED DATA
νasym(O-C-O)
1580
1560
1550
3400
3400
3400
1625
1575
1575
νsym(O-C-O)
1390
δ(O-C-O)
800
cm–1
ν(M-O) + ν(C-C)
590
1350
1400
1360
1380
1400
800
660
—
840
800
840
495
575
565
530
—
—
—
ν(CH=CH)
990
Table 2. Chemical analysis, total weight loss and density of hydrated nickel manganese carboxylates
CARBOXYLATES
NMF
NMS
NMO
NMT
NCM
CHEMICAL ANALYSIS
MANGANESE (%)
CALC.
OBS.
CALC.
9.9176
17.855
18.5663
8.4217
14.28
15.7657
10.6768
20.8
19.98
7.7545
15.34
14.5168
11.1003
16.02
20.7804
NICKEL (%)
OBS.
9.4315
10.8211
9.8526
6.95
11.00
TOTAL WEIGHT LOSS (%)
OBS.
60.62
66.63
57.46
69.45
56.14
CALC.
60.70
66.65
57.38
69.72
56.01
DENSITY
(gcm –3)
1.7929
2.0192
2.1585
1.7304
1.7534
Table 3. Isothermal weight loss and TGA/DTA of nickel manganese carboxylates
CARBOXYLATES
NMS
TGA (AIR)
TEMPERATURE
WT. LOSS
RANGE (°C)
(%)
RT–91.22
0.62
DTA PEAKS
EXO/ENDO PEAKS
(°C)
91.22–176.8
26.002
135.27 (endo)
176.8–396.76
28.596
331.7 (exo hump)
387.44 (broad exo)
396.76–526
526–790
11.081–0.376
TEMPERATURE
RANGE (°C)
RT–100
100–120
120–140
140–250
250–380
602.04 (exo)
ISOTHERMAL WEIGHT LOSS
WT. LOSS
REMARKS
(%)
16.80
Loss of 61/2 H2O
6.40
Loss of 21/2 H2O
4.66
22.24
Loss of 1 H2O
11.93
Decarboxylation to form NiMn2O4
54
Analog and Mixed-Signal Products
February 2001
Analog Applications Journal
Signal Conditioning: Thermistors
Texas Instruments Incorporated
Table 4. Isothermal weight loss studies of hydrated nickel
manganese carboxylates
CARBOXYLATES
NMF
NMO
NMT
NMM
TEMPERATURE
RANGE (°C)
RT–120
120–140
140–250
250–280
RT–100
100–160
160–200
200–280
RT–100
100–120
120–180
180–225
225–250
250–380
RT–120
120–170
170–180
180–260
260–380
Table 5. X-ray diffraction data of NiMn2O4 (NMF)*
SR. NO.
1
2
3
4
5
6
2θ (°)
30.25
35.55
43.20
53.60
57.05
62.80
dobs (A°)
2.9545
2.5252
2.0941
1.7098
1.6143
1.4795
dcalc (A°)
2.9611
2.5252
2.0938
1.7096
1.6132
1.4805
HKL
220
311
400
422
333
440
Table 6. X-ray diffraction data of NiMn2O4 (NMS)*
2θ (°)
18.33
30.16
35.54
37.17
43.20
53.61
62.78
75.35
dobs (A°)
4.8481
2.9676
2.5298
2.4226
2.0976
1.7122
1.4825
1.2634
* Lattice parameter a = 8.39005
Structure—cubic
dcalc (A°)
4.8441
2.9664
2.5298
2.4221
2.0975
1.7127
1.4832
1.2649
REMARKS
21/2
Loss of
H2O
Loss of 1 H2O
Loss of 1 H2O
Decarboxylation to form NiMn2O4
Loss of 41/2 H2O
Loss of 1/2 H2O
Loss of 11/2 H2O
Decarboxylation to form NiMn2O4
Loss of 4 H2O
Loss of 1 H2O
Loss of 2 H2O
Loss of 1 H2O
Decarboxylation to form NiMn2O4
Loss of 1/2 H2O
Loss of 11/2 H2O
Loss of 1 H2O
Decarboxylation to form NiMn2O4
Table 7. XRD data of NiMn2O4 obtained from carboxylates (NMO)*
* Lattice parameter a = 8.39805
Structure—cubic
SR. NO.
1
2
3
4
5
6
7
8
WEIGHT LOSS
(%)
7.61
2.69
3.21
48.19
14.74
1.64
4.92
36.39
10.11
2.38
4.17
2.33
3.53
46.70
1.73
4.90
2.75
32.65
3.90
HKL
111
220
311
222
400
422
440
622
SR. NO.
1
2
3
4
5
6
7
8
9
10
2θ (°)
18.36
30.13
35.49
37.15
43.14
53.53
57.23
62.84
74.15
75.18
dobs (A°)
4.8289
2.9705
2.5333
2.4238
2.1002
1.7146
1.6124
1.4813
1.2809
1.2658
dcalc (A°)
4.8449
2.9705
2.5333
2.4254
2.1003
2.7151
1.6169
1.4853
1.2813
1.2666
HKL
111
220
311
222
400
422
333
440
533
622
* Lattice parameter a = 8.397742
Structure—cubic
Table 8. X-ray diffraction data of NiMn2O4 (NMT)*
SR. NO.
1
2
3
4
5
6
2θ (°)
30.15
35.45
43.25
53.70
57.10
62.70
dobs (A°)
2.9641
2.5321
2.0918
1.7068
1.6130
1.4817
dcalc (A°)
2.9692
2.5321
2.0995
1.7143
1.6162
1.4845
HKL
220
311
400
422
333
440
* Lattice parameter a = 8.38848
Structure—cubic
Table 9. X-ray diffraction data of NiMn2O4 (NMM)*
SR. NO.
1
2
3
4
5
2θ (°)
35.53
37.34
43.37
57.31
63.01
dobs (A°)
2.5308
2.4122
2.0898
1.6103
1.4778
* Lattice parameter a = 8.37677
Structure—cubic
dcalc (A°)
2.5308
2.4230
2.0984
1.6154
1.4838
HKL
311
222
400
333
440
Continued on next page
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February 2001
Analog and Mixed-Signal Products
Signal Conditioning: Thermistors
Texas Instruments Incorporated
Continued from previous page
References
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14. S.K. Sarkar, M.L. Sharma and S.K. Lahairi, “Resistivity
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Related Web sites
amplifier.ti.com
A web page of Sensor Scientific, Inc.:
www.sensorsci.com/letter.htm
Western Electronic Components, a U.S.-based thermistor
manufacturer:
www.wecc.com/
Manufacturer of a wide variety of NTC and PTC
thermistors and current surge limiters:
www.ametherm.com/
56
Analog and Mixed-Signal Products
February 2001
Analog Applications Journal
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