CN111484327B - Strontium, cerium, niobium and tungsten quaternary thermistor material with adjustable temperature zone and B value and preparation method thereof - Google Patents
Strontium, cerium, niobium and tungsten quaternary thermistor material with adjustable temperature zone and B value and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a strontium, cerium, niobium and tungsten quaternary system thermistor material with adjustable temperature zone and B value and a preparation method thereof, wherein the material is prepared from SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 Mixing and grinding, calcining, grinding, cold isostatic pressing and high-temperature sintering are carried out on the raw materials to obtain SrWO 4 ‑xCeNbO 4+δ The thermistor ceramic material has x of 0.1-0.8, and the electrical performance parameters are as follows: b is 400℃/800℃ =4030K‑11109K±4.5%,ρ 400℃ =3.37×10 3 Ω·cm‑3.87×10 9 Omega cm +/-6%. The strontium, cerium, niobium and tungsten quaternary negative temperature coefficient thermistor material obtained by the method can accurately adjust the B value, the temperature measurement interval and the resistivity of a material system by adjusting the x value, and the adjustable temperature zone range is 200-1200 ℃. The material has the advantages of simple preparation process, stable electrical property, good linear relation and good consistency, can carry out temperature measurement, temperature control and circuit compensation in a wider temperature zone, and is a novel negative temperature coefficient thermistor material suitable for manufacturing thermistors in a wide temperature zone.
Description
Technical Field
The invention relates to a strontium, cerium, niobium and tungsten quaternary system thermistor material with an adjustable temperature zone and B value and a preparation method thereof.
Background
The sensitive element and the sensor are considered as electronic technical products with the greatest development prospect, and the development of the sensitive element is significant for improving the international position of the electronic industry in China. Among them, negative Temperature Coefficient (NTC) thermistors are widely used in many aspects such as temperature measurement, control and compensation because of their advantages of high temperature measurement accuracy, good interchangeability, high reliability, low cost, etc. As is well known, wide temperature zone thermistors are typically low B, high resistance, thermally sensitive materials. The spinel-structure NTC is in a non-equilibrium state after being sintered, so that the electrical property of the material is easy to change, and the material has certain limitation, low use temperature and narrow temperature range (-50-300 ℃); the perovskite material has stable structure and good stability at high temperature, and the service temperature range is generally 300-1000 ℃. Therefore, the wide temperature zone thermistor material usually adopts different structural materials to carry out double-phase compounding to form a composite material with low B value and high resistance. At present, materials with the same structure and the same system in the market are difficult to have high-temperature and low-temperature NTC characteristics, and the B value and the temperature measurement temperature region are only limited and controlled by means of doping or compounding. One of the important challenges of modern material science is to develop a new compound and perform modification optimization on the basis, so that the research of the thermistor material with high-temperature or low-temperature NTC characteristics is obtained by adjusting a certain parameter in a system, the research and development range of the material is greatly expanded, and a series of novel NTC thermosensitive materials with potential application values can be designed by utilizing the characteristics of the material under different parameters.
Research finds that the scheelite structure SrWO 4 -xCeNbO 4+δ The thermistor material with NTC characteristic has excellent high temperature mechanical property and high temperature stability. The temperature measurement temperature zone of the material can be greatly widened by adjusting the value x, the application of the material in the temperature measurement field is expanded, and meanwhile, the resistance value and the B value of the thermosensitive material are accurately controlled according to the change trend of the material structure and the change of a conducting mechanism, so that the novel NTC thermosensitive resistance material is obtained. The adjustable temperature range of the invention is 200-1200 ℃, the adjustable temperature range has obvious negative temperature coefficient characteristic, the material has stable electrical property, good linear relation and good consistency, and is suitable for manufacturing the thermistor used in a wide temperature range.
Disclosure of Invention
The invention aims to provide a strontium, cerium, niobium and tungsten quaternary system thermistor material with adjustable temperature zone and B value and a preparation method thereof, wherein the material is prepared from SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 Mixing and grinding, calcining, grinding, cold isostatic pressing and high-temperature sintering are carried out on the raw materials to obtain SrWO with adjustable temperature zone and B value 4 -xCeNbO 4+δ The thermistor ceramic material is a strontium, cerium, niobium and tungsten quaternary thermistor material, and the B value, the temperature measuring interval and the resistivity of a material system can be accurately adjusted by adjusting the x value, wherein x is more than or equal to 0 and less than or equal to 0.8, and the x value is more than or equal to 0The electrical property parameters are as follows: b 400℃/800℃ ＝4030K-11109K±4.5％,ρ 400℃ ＝3.37×10 3 Ω·cm-3.87×10 9 Omega cm +/-6%, and adjustable temp range of 200-1200 deg.C. The temperature-zone and B-value adjustable strontium, cerium, niobium and tungsten quaternary thermistor material prepared by the invention has the characteristic of negative temperature coefficient, the material has the advantages of simple preparation process, stable electrical property, good linear relation and good consistency, can carry out temperature measurement, temperature control and line compensation in a wider temperature zone, and is a novel negative temperature coefficient thermistor material suitable for manufacturing wide-temperature-zone thermistors.
The invention relates to a strontium, cerium, niobium and tungsten quaternary thermistor material with adjustable temperature zone and B value, which has the chemical general formula: srWO 4 -xCeNbO 4+δ Wherein x is more than or equal to 0.1 and less than or equal to 0.8, and is prepared from raw material SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 And (4) preparing.
The preparation method of the strontium, cerium, niobium and tungsten quaternary system thermistor material with the temperature zone and the B value adjustable comprises the following steps:
a. with SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 As raw material, has the chemical formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to SrCO 3 :CeO 2 :Nb 2 O 5 :WO 3 Weighing the following components in a molar ratio of = 1.1-0.8;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1100-1200 ℃ for 3-5h, grinding for 4-6h, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at the concentration of 15-30Kg/cm 2 Pressing the blocks into blocks for 1-3min, performing cold isostatic pressing on the formed blocks, maintaining the pressure at 250-300MPa for 1-3min, and sintering the blocks at 1250-1350 ℃ for 3-6h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. coating platinum paste electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1000-1100 ℃ for 1-2 hours to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
The invention relates to a strontium, cerium, niobium and tungsten quaternary system thermistor material with adjustable temperature zone and B value and a preparation method thereof, which adopts a solid phase method to mix, grind, calcine and regrind analytically pure strontium carbonate, analytically pure cerium dioxide, analytically pure niobium pentoxide and analytically pure tungsten trioxide, repeat the process twice to obtain a negative temperature coefficient thermistor powder material, then form the powder by sheet cold isostatic pressing, coat and burn platinum slurry electrodes on the front and back surfaces after high-temperature sintering to obtain a thermistor, and the electrical performance parameters are as follows: b is 400℃/800℃ ＝4030K-11109K±4.5％,ρ 400℃ ＝3.37×10 3 Ω·cm-3.87×10 9 Omega cm +/-6%, and adjustable temp range of 200-1200 deg.C. The thermistor material has the advantages of simple preparation process, stable electrical property, good linear relation and good consistency, can carry out temperature measurement, temperature control and circuit compensation in a wider temperature zone, and is a novel negative temperature coefficient thermistor material suitable for manufacturing wide temperature zone thermistors.
The invention relates to a strontium, cerium, niobium and tungsten quaternary system thermistor material with adjustable temperature zone and B value, which is characterized in that:
the strontium tungstate is selected as a main component because the strontium tungstate has excellent thermal stability and chemical stability, has a stable structure at room temperature and high temperature and has a high practical value.
When the sintering temperature is a definite value, the B value and the temperature measuring interval of the current chemical formula material can be changed by adjusting the value of x.
The innovation points of the invention are as follows:
(1)SrWO 4 -xCeNbO 4+δ the material can effectively adjust the B value of the material and greatly change the temperature measuring interval by adjusting the x value.
(2) CeNbO in the heat-sensitive material 4 Has double functions: one is with CeNbO 4 Increase so that Ce 3+ Increase in content of the component (B) to cause the loadThe concentration of the fluid is increased, and the conductivity is increased; second is CeNbO 4 The increase of the content distorts the crystal lattice, resulting in CeNbO having a mixed conduction mechanism of ionic and p-type 4.08 It appears that the resistivity of the material is greatly changed.
Drawings
FIG. 1 shows SrWO according to the present invention 4 -xCeNbO 4+δ Resistivity versus temperature of the material.
Detailed Description
Example 1
a. Has the chemical general formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to the mol ratio SrCO 3 :CeO 2 :Nb 2 O 5 :WO 3 Weighing the following components in parts by weight of =1, 0.1;
b. b, calcining the oxide powder obtained in the step a at 1200 ℃ for 5 hours, grinding for 6 hours, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at the concentration of 30Kg/cm 2 Pressing the block for 1min, performing cold isostatic pressing on the formed block, maintaining the pressure at 300MPa for 3min, and sintering the block at 1350 ℃ for 6h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. and d, coating platinum slurry electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1100 ℃ for 2 hours to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
The obtained strontium, cerium, niobium and tungsten quaternary system thermal sensitive ceramic material is subjected to electrical property test to obtain an electrical parameter B 400℃/800℃ ＝11109K±4.2％，ρ 400℃ ＝3.87×10 9 Omega cm +/-5.6%, and the temp measuring interval of said material is 400-1200 deg.C.
Example 2
a. Has a chemical formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to the mol ratio SrCO 3 :CeO 2 :Nb 2 O 5 :WO 3 Weighing a material (1) = 1;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1150 ℃ for 4h, grinding for 6h, and repeating the process twice to obtain thermistor powder;
c. b, mixing the thermistor powder obtained in the step b at a ratio of 30Kg/cm 2 The pressure of the raw material is pressed into a block for 2min, the formed block is subjected to cold isostatic pressing, the pressure is maintained at 250MPa for 3min, and then the block is sintered at 1300 ℃ for 5h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. coating platinum paste electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1100 ℃ for 1h to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
The obtained strontium, cerium, niobium and tungsten quaternary system thermal sensitive ceramic material is subjected to electrical property test to obtain an electrical parameter B 400℃/800℃ ＝8768K±4.5％，ρ 400℃ ＝1.17×10 8 Omega cm +/-5.2%, and the temp measuring interval of said material is 300-1100 deg.C.
Example 3
a. Has the chemical general formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to the molar ratio SrCO 3 :CeO 2 :Nb 2 O 5 :WO 3 Weighing a material (1) = 1.4;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1100 ℃ for 3h, grinding for 5h, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at a ratio of 20Kg/cm 2 The pressure of the raw material is pressed into a block for 2min, the formed block is subjected to cold isostatic pressing, the pressure is maintained at 250MPa for 2min, and then the block is sintered for 4h at the temperature of 1250 ℃ to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. and d, coating platinum slurry electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1100 ℃ for 1h to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
The obtained strontium, cerium, niobium and tungsten quaternary system thermal sensitive ceramic material is subjected to electrical property test to obtain an electrical parameter B 400℃/800℃ ＝4411K±3.9％，ρ 400℃ ＝1.72×10 4 Omega cm +/-4.6%, and the temp measuring interval of said material is 200-1000 deg.C.
Example 4
a. Has the chemical general formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to the molar ratio SrCO 3 :CeO 2 :Nb 2 O 5 :WO 3 Weighing a material (1) =1:0.6, placing the material in an agate mortar, grinding the material for 6 hours, and fully and uniformly mixing the material to obtain oxide powder with the average particle size of 1.297 mu m;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1100 ℃ for 3h, grinding for 6h, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at a ratio of 15Kg/cm 2 Pressing the blocks into blocks for 3min, performing cold isostatic pressing on the formed blocks, maintaining the pressure at 300MPa for 1min, and sintering the blocks at 1250 ℃ for 3h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. and d, coating platinum slurry electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1000 ℃ for 1h to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
The obtained strontium, cerium, niobium and tungsten quaternary system thermal sensitive ceramic material is subjected to electrical property test to obtain an electrical parameter B 400℃/800℃ ＝4030K±4.3％，ρ 400℃ ＝5.74×10 3 Omega cm +/-6%, and the temp measuring range of said material is 200-800 deg.C.
Example 5
a. Has the chemical general formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to the molar ratio SrCO 3 :CeO 2 :Nb 2 O 5 :WO 3 ＝1:0.8Weighing 0.4, placing in an agate mortar for grinding for 6 hours, and fully and uniformly mixing to obtain oxide powder with the average particle size of 1.215 micrometers;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1100 ℃ for 3h, grinding for 4h, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at a ratio of 15Kg/cm 2 Pressing the blocks into blocks for 3min, performing cold isostatic pressing on the formed blocks, maintaining the pressure at 300MPa for 1min, and sintering the blocks at 1250 ℃ for 3h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. and d, coating platinum slurry electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1000 ℃ for 1h to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
The obtained strontium, cerium, niobium and tungsten quaternary system thermal sensitive ceramic material is subjected to electrical property test to obtain an electrical parameter B 400℃/800℃ ＝4235K±4.0％，ρ 400℃ ＝3.37×10 3 Omega cm +/-5.2%, and the temp measuring interval of said material is 200-800 deg.C.
Example 6
The electric parameters and the temperature measuring interval of the material can be effectively adjusted by adjusting the molar ratio of the raw materials in any one of the temperature zones and the strontium, cerium, niobium and tungsten four-element thermistor materials with adjustable B values in the embodiments 1 to 5. The material has the characteristics of simple preparation process, stable electrical property, good linear relation and good consistency, can carry out temperature measurement, temperature control and line compensation in a wider temperature zone, and is a novel negative temperature coefficient thermistor material suitable for manufacturing wide temperature zone thermistors.
Claims (2)
1. SrWO 4 -xCeNbO 4+δ The quaternary thermistor material is characterized in that the chemical general formula of the material is as follows: srWO 4 -xCeNbO 4+δ Wherein x is more than or equal to 0.1 and less than or equal to 0.8, and is prepared from raw material SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 Preparing;
the electrical performance parameters of the thermistor material are as follows: b 400℃/800℃ ＝4030K-11109K±4.5％，ρ 400℃ ＝3.37×10 3 Ω·cm-3.87×10 9 Omega cm +/-6%, and the adjustable temperature zone range is 200-1200 ℃;
the thermistor material is prepared by adopting a method comprising the following steps:
a. with SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 As a raw material, has a chemical formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to SrCO 3 ∶CeO 2 ∶Nb 2 O 5 ∶WO 3 Weighing the powder according to the molar ratio of 1:0.1-0.8:0.05-0.4:1, grinding the powder in an agate mortar for 6-8 hours, and fully and uniformly mixing the powder to obtain oxide powder with the average particle size of 1.215-1.530 mu m;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1100-1200 ℃ for 3-5h, grinding for 4-6h, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at a ratio of 15-30Kg/cm 2 Pressing the blocks into blocks for 1-3min, performing cold isostatic pressing on the formed blocks, maintaining the pressure at 250-300MPa for 1-3min, and sintering the blocks at 1250-1350 ℃ for 3-6h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. and d, coating platinum slurry electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1000-1100 ℃ for 1-2 hours to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
2. SrWO 4 -xCeNbO 4+δ The preparation method of the quaternary thermistor material is characterized by comprising the following steps of:
a. with SrCO 3 、CeO 2 、Nb 2 O 5 And WO 3 As raw material, has the chemical formula of SrWO 4 -xCeNbO 4+δ The raw materials are mixed according to SrCO 3 ∶CeO 2 ∶Nb 2 O 5 ∶WO 3 ＝1∶0.1-0.8∶0.05-0.4∶1, grinding the mixture in an agate mortar for 6 to 8 hours, and fully and uniformly mixing the mixture to obtain oxide powder with the average particle size of 1.215 to 1.530 mu m;
b. b, calcining the oxide powder obtained in the step a at the temperature of 1100-1200 ℃ for 3-5h, grinding for 4-6h, and repeating the process twice to obtain thermistor powder;
c. c, mixing the thermistor powder obtained in the step b at a ratio of 15-30Kg/cm 2 Pressing the blocks into blocks for 1-3min, performing cold isostatic pressing on the formed blocks, maintaining the pressure at 250-300MPa for 1-3min, and sintering the blocks at 1250-1350 ℃ for 3-6h to obtain the strontium, cerium, niobium and tungsten quaternary ceramic material;
d. and d, coating platinum slurry electrodes on the front surface and the back surface of the ceramic material obtained in the step c, and annealing at the temperature of 1000-1100 ℃ for 1-2 hours to obtain the strontium, cerium, niobium and tungsten quaternary thermistor material with an adjustable temperature zone and an adjustable B value.
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