CN101719404A - Ternary-system chip negative temperature coefficient thermal resistor - Google Patents
Ternary-system chip negative temperature coefficient thermal resistor Download PDFInfo
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Abstract
The invention relates to a ternary-system chip negative temperature coefficient thermal resistor, which uses manganese nitrate, nickel nitrate and cobalt nitrate as raw materials and ammonium bicarbonate as precipitator, is prepared by a liquid-phase co-precipitation method, and comprises the following steps: improving the agglomeration phenomenon of the precipitated particles by controlling the molar ratio of nitrate to precipitator ammonium bicarbonate, the reaction temperature and the pH value, washing out the impurities in the product by modes of water washing and alcohol washing to obtain superfine and uniform thermal resistor powder, drying, calcining to obtain evenly dispersed mixed oxide powder of Mn, Ni and Co, briquetting and moulding the powder, isopressing, sintering under high temperature, slicing by a semiconductor to obtain a thermal resistor chip, and encapsulating with epoxy resin to obtain the ternary-system chip negative temperature coefficient thermal resistor with high performance which has the characteristics of good uniformity, high stability, capability of repeatability and interconversion, and is suitable for temperature measurement, control and line compensation in the household appliance field such as refrigerators, air conditioners and the like.
Description
Technical field
The present invention relates to a kind of employing liquid-phase coprecipitation and prepare ternary-system chip negative temperature coefficient thermal resistor.
Background technology
Negative temperature coefficient (NTC) thermistor has high sensitivity, miniature characteristics, very big at many household electrical appliances, information industry requirement, along with electronic information technology and digitized high speed development, the NTC thermistor temperature sensor has been proposed the requirement of miniaturization, lightweight, slimming, and high accuracy, interchangeable NTC thermistor element become the main flow direction of development.But adopt high temperature solid-state method to prepare large batch of NTC thermistor material at present usually, its raw material is a metal oxide, the calcining heat of presoma is higher, powder granularity is inhomogeneous and powder active is low, be difficult to guarantee the accurate stoichiometric proportion of material in the process of this external grinding, cannot say for sure not introduce impurity, so use this method to make the existing certain limitation of high-precision NTC thermistor powder.In order to produce the NTC thermistor element of precision height, good reliability, one of its key will be improved from the synthetic method of material exactly, obtains component homogeneous, activity is higher, particle diameter is tiny powder granule.
The present invention is directed to the high accuracy of needing badly at present, interchangeable NTC components and parts are background, according to the demand to thermistor B value, resistance and reliability is foundation, carried out design and optimization by aspects such as raw material, prescription, preparation method and sintering process, the present invention at first studies the prescription of material, makes parameter, stability and the precision aspect of element reach higher requirement; In addition the dropping of precipitation reagent is controlled in proper order, and the later stage pH value of solution is controlled, make that the loss of each metal ion reaches minimum in the solution, thereby accurately controlled the stoichiometric proportion of each component in reaction.The present invention carries out in conjunction with deionized water and absolute ethyl alcohol dual mode the washing of presoma in addition, can effectively avoid sneaking into of foreign ion, and can avoid the generation of agglomeration.
Summary of the invention
The object of the invention is, develop a kind of ternary-system chip negative temperature coefficient thermal resistor, this resistor is by manganese nitrate, nickel nitrate, cobalt nitrate is a raw material, with carbonic hydroammonium is precipitation reagent, the employing liquid-phase coprecipitation is made, mol ratio by control nitrate and precipitation reagent carbonic hydroammonium, reaction temperature and pH value, to improve the agglomeration of deposit seed, again through washing and the alcohol mode of washing with the impurity flush away in the product, obtain fine, uniform thermistor powder, drying again, calcining obtains finely dispersed Mn, Ni, Co mixed oxide powder is with the powder compound stalk forming, Deng static pressure, high temperature sintering, semiconductor is cut, scribing obtains thermistor chip, can obtain high performance ternary-system chip negative temperature coefficient thermal resistor through epoxy encapsulation again; This resistor has high, the characteristics repeatably of high conformity, stability, and ceramic material has " little, smart, steady, quick " and interchangeable characteristics through product, is applicable to temperature survey, control and the line build-out of field of household appliances such as refrigerator, air-conditioning.
Ternary-system chip negative temperature coefficient thermal resistor of the present invention, be with analytically pure manganese nitrate, nickel nitrate, cobalt nitrate is a raw material, with carbonic hydroammonium is precipitation reagent, adopt liquid-phase coprecipitation, with manganese nitrate, nickel nitrate, cobalt nitrate is dissolved in the ionized water, be mixed with mixed solution, again carbonic hydroammonium is added deionized water and be mixed with precipitant solution, ammonium bicarbonate soln slowly is added drop-wise in the metal nitrate mixed solution, with ammoniacal liquor control pH value, leave standstill, with deionized water and absolute ethanol washing suction filtration, oven dry is ground again, thermal decomposition, grind again, calcining, grinding the back pre-molding is green compact, through isostatic cool pressing, high temperature sintering, semiconductor is cut, scribing obtains thermistor chip, adopts epoxy resin that chip is sealed, can obtain ternary-system chip negative temperature coefficient thermal resistor, wherein each component molar percentage is: Mn: Ni: Co=Mn: Ni: Co=30-70: 1-15: 29-55.
The preparation method of described ternary-system chip negative temperature coefficient thermal resistor follows these steps to carry out:
A, take by weighing raw material manganese nitrate, nickel nitrate, cobalt nitrate at first respectively, mix and dissolve in the deionized water, be mixed with mixed solution;
B, analytically pure carbonic hydroammonium is dissolved in the deionized water, fully stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 30-50 ℃, and pH value is controlled at 7.8-9, does not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 400-600 ℃ of thermal decomposition 1.5-3h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 700-900 ℃ of calcining 1.5-3h;
F, the powder after the step e calcining is ground once more, powder is with 30-40Kg/cm
2Pressure carry out compound stalk forming, the time is 1-10min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 1-10min under the 300-400MPa at pressure, in 1100-1200 ℃ of high temperature sintering 1-3h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, employing semiconductor cutting technique, ceramic block material section, blackening electrode, scribing with sintering promptly get thermistor chip;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
Step a manganese nitrate, nickel nitrate, cobalt nitrate mixed solution control metal ion molar concentration are 1mol/L.
It is 1.25mol/L that step b carbonic hydroammonium is dissolved in the deionized water control molar concentration.
Step e powder granule size is 50-120nm.
Ternary-system chip negative temperature coefficient thermal resistor of the present invention, dropping order, pH value, temperature and calcining heat by control reaction solution concentration and precipitation reagent, finely dispersed Mn, Ni, Co mixed oxide powder have been prepared, powder granule has greatly improved reactivity, repeatability, consistency and the stability of material at 50-120nm.Oxide powder is through sintering porcelain into, and through advanced person's semiconductor cut, the scribing technology obtains thermistor chip, in order to reduce of the influence of encapsulation process temperature to chip, choose epoxy resin as encapsulant, the thermistor element of this kind encapsulant encapsulation heat-resisting, moisture-proof is good, insulating properties, long-time stability are good, but cost is low and continuous batch production, have greatly improved rate of finished products, interchangeability, stability and the reliability of thermistor.
Ternary-system chip negative temperature coefficient thermal resistor of the present invention, its characteristics are:
The concentration ratio of mixed nitrate solution and precipitation reagent carbonic hydroammonium all has a significant impact the B value and the resistance of material.It is 1.25: 1 that the present invention selects carbonic hydroammonium and metal ion mol ratio, the powder granularity that makes disperses, good uniformity, the material that obtains behind forming and sintering becomes porcelain good, use the B value of the negative tempperature coefficient thermistor element of this material to be 3920K ± 1%, 25 ℃ of resistances are 1.0-4.0K Ω ± 3%, and element has good stability, characteristics that precision is high.
The mode that adopts the ammonium bicarbonate precipitation agent in nitrate solution, to drip, adopt this kind mode to make reactant liquor be under the pH reaction condition of broad, because under the different acidity condition, metal ion exists with multi-form in the nitrate solution, make different metal ions earlier, back and the complexing of ammonium radical ion, along with the increase pH value of carbonic hydroammonium increases gradually, the acidity of solution weakens, in entire reaction course, can make the abundant and precipitation reagent complexing of metal ion, avoid certain metal ion species not have complete reaction and cause ion to run off, cause the B value and the resistance of material not to repeat.
Control the pH value in the 7.8-9 scope in the strictness of reaction later stage, mainly be since this moment most metal ions react completely, in order to guarantee the precise chemical structure metering ratio of various compositions, in the reaction later stage pH value is maintained fixed, make the loss concentration minimum of each metal ion species, greatly improved repeatability, consistency and the stability of thermistor material.
In order to prevent suction filtration, washing process generation agglomeration and to remove ion unnecessary in the solution, the present invention selects to use deionized water wash five times earlier, with major part can water soluble ions elder generation's flush away, after this adopting absolute ethanol washing three times, its main purpose is to remove the water of coordination between adsorbed water and Chemical Physics, in order to eliminate OH
-Hydrogen bond action between the group reduces the influence of agglomeration to product, and some insoluble organic compounds in this external application ethanol flush away product is eliminated the influence of impurity to product purity, thereby reduced the influence of impurity to thermo-sensitive material B value and resistance.
Adopt epoxy resin as encapsulating material, use the resistor B value of this material package can not be subjected to the influence of package temperature, when adopting the epoxy resin technology encapsulation, the size of chip should be at the volume=length of side * length of side * thickness (1.0＜length of side＜1.5mm wherein, 0.3＜thickness＜0.4mm), the thermistor parameter that obtains is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
The negative temperature coefficient thermistor of employing epoxy encapsulation is heat-resisting, moisture-proof is good, insulating properties, long-time stability are good, but cost is low and continuous batch production, improve rate of finished products, interchangeability, stability and the reliability of thermistor, make the negative temperature coefficient thermistor rate of finished products by traditional handicraft less than 20% 30%-40% that brings up to technology of the present invention.
Embodiment
Embodiment 1
A, pure with the 3mol analysis, molar percentage is: Mn: Ni: Co=30: 15: 55 manganese nitrate, nickel nitrate, cobalt nitrate are raw material, mix and dissolve in the deionized water, be mixed with the ion mixed solution of 1.0mol/L, control metal ion molar concentration is 1mol/L;
B, be dissolved in the deionized water with the analytically pure carbonic hydroammonium of 4.5mol, abundant stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution of 1.25mol/L, and the control molar concentration is 1.25mol/L;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 30 ℃, with the variation of acidometer test pH value, and regulates pH7.8 with ammoniacal liquor under the vigorous stirring, do not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 400 ℃ of thermal decomposition 1.5h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 700 ℃ of calcining 1.5h, the powder granule size is 50nm;
F, the powder after the step e calcining is ground once more, powder is with 30Kg/cm
2Pressure carry out compound stalk forming, the time is 1min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 1min under the 300MPa at pressure, in 1200 ℃ of high temperature sintering 3h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, adopting the semiconductor cutting technique, is the thin slice of 0.30mm with the ceramic block material slice thickness of sintering, with thin slice two sides blackening Ag-Pd electrode, promptly obtains the chip of 1.0 * 1.0mm again through scribing;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
This resistor has the high and interchangeable characteristics of precision, is applicable to temperature survey, control and the line build-out of field of household appliances such as refrigerator, air-conditioning.
Embodiment 2
A, pure with the 3mol analysis, molar percentage is: Mn: Ni: Co=50: 13: 37 manganese nitrate, nickel nitrate, cobalt nitrate raw material, mix and dissolve in the deionized water, be mixed with the ion mixed solution of 1.0mol/L, control metal ion molar concentration is 1mol/L;
B, be dissolved in the deionized water with the analytically pure carbonic hydroammonium of 4.5mol, abundant stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution of 1.25mol/L, and the control molar concentration is 1.25mol/L;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 40 ℃, with the variation of acidometer test pH value, and regulates the pH value 8.3 with ammoniacal liquor under the vigorous stirring, do not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 500 ℃ of thermal decomposition 2h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 800 ℃ of calcining 2h, the powder granule size is 80nm;
F, the powder after the step e calcining is ground once more, powder is with 35Kg/cm
2Pressure carry out compound stalk forming, the time is 5min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 5min under the 350MPa at pressure, in 1150 ℃ of high temperature sintering 2h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, adopting the semiconductor cutting technique, is the thin slice of 0.35mm with the ceramic block material of sintering through slice thickness, with thin slice two sides blackening Ag-Pd electrode, obtains the chip of 1.2 * 1.2mm again through scribing;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
This resistor has the high and interchangeable characteristics of precision, is applicable to temperature survey, control and the line build-out of field of household appliances such as refrigerator, air-conditioning.
Embodiment 3
A, analyze purely with 3mol, molar percentage is: Mn: Ni: Co=70: 1: 29 manganese nitrate, nickel nitrate, cobalt nitrate raw material, and mix and dissolve in the deionized water,, being mixed with the ion mixed solution of 1.0mol/L, control metal ion molar concentration is 1mol/L;
B, be dissolved in the deionized water with the analytically pure carbonic hydroammonium of 4.5mol, abundant stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution of 1.25mol/L, and the control molar concentration is 1.25mol/L;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 50 ℃, with the variation of acidometer test pH value, and regulates the pH value 9 with ammoniacal liquor under the vigorous stirring, do not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 600 ℃ of thermal decomposition 3h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 900 ℃ of calcining 3h, the powder granule size is 120nm;
F, the powder after the step e calcining is ground once more, powder is with 40Kg/cm
2Pressure carry out compound stalk forming, the time is 10min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 10min under the 400MPa at pressure, in 1100 ℃ of high temperature sintering 1h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, adopting the semiconductor cutting technique, is the thin slice of 0.4mm with the ceramic block material of sintering through slice thickness, with thin slice two sides blackening Ag-Pd electrode, obtains the chip of 1.5 * 1.5mm again through scribing;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
This resistor has the high and interchangeable characteristics of precision, is applicable to temperature survey, control and the line build-out of field of household appliances such as refrigerator, air-conditioning.
Embodiment 4
A, analyze purely with 3mol, molar percentage is: Mn: Ni: Co=40: 8: 52 manganese nitrate, nickel nitrate, cobalt nitrate raw material, and mix and dissolve in the deionized water,, being mixed with the ion mixed solution of 1.0mol/L, control metal ion molar concentration is 1mol/L;
B, be dissolved in the deionized water with the analytically pure carbonic hydroammonium of 4.5mol, abundant stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution of 1.25mol/L, and the control molar concentration is 1.25mol/L;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 35 ℃, with the variation of acidometer test pH value, and regulates the pH value 8.0 with ammoniacal liquor under the vigorous stirring, do not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 450 ℃ of thermal decomposition 2.5h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 750 ℃ of calcining 2.5h, the powder granule size is 60nm;
F, the powder after the step e calcining is ground once more, powder is with 32Kg/cm
2Pressure carry out compound stalk forming, the time is 3min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 3min under the 320MPa at pressure, in 1180 ℃ of high temperature sintering 2.5h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, adopting the semiconductor cutting technique, is the thin slice of 0.32mm with the ceramic block material of sintering through slice thickness, with thin slice two sides blackening Ag-Pd electrode, obtains the chip of 1.2 * 1.2mm again through scribing;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
This resistor has the high and interchangeable characteristics of precision, is applicable to temperature survey, control and the line build-out of field of household appliances such as refrigerator, air-conditioning.
Embodiment 5
A, analyze purely with 3mol, molar percentage is: Mn: Ni: Co=60: 5: 35 manganese nitrate, nickel nitrate, cobalt nitrate raw material, and mix and dissolve in the deionized water,, being mixed with the ion mixed solution of 1.0mol/L, control metal ion molar concentration is 1mol/L;
B, be dissolved in the deionized water with the analytically pure carbonic hydroammonium of 4.5mol, abundant stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution of 1.25mol/L, and the control molar concentration is 1.25mol/L;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 45 ℃, with the variation of acidometer test pH value, and regulates the pH value 8.7 with ammoniacal liquor under the vigorous stirring, do not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 550 ℃ of thermal decomposition 3h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 850 ℃ of calcining 2h, the powder granule size is 100nm;
F, the powder after the step e calcining is ground once more, powder is with 38Kg/cm
2Pressure carry out compound stalk forming, the time is 8min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 8min under the 380MPa at pressure, in 1120 ℃ of high temperature sintering 1.5h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, adopting the semiconductor cutting technique, is the thin slice of 0.38mm with the ceramic block material of sintering through slice thickness, with thin slice two sides blackening Ag-Pd electrode, obtains the chip of 1.2 * 1.2mm again through scribing;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
This resistor has the high and interchangeable characteristics of precision, is applicable to temperature survey, control and the line build-out of field of household appliances such as refrigerator, air-conditioning.
Claims (5)
1. ternary-system chip negative temperature coefficient thermal resistor, it is characterized in that it being with analytically pure manganese nitrate, nickel nitrate, cobalt nitrate is a raw material, with carbonic hydroammonium is precipitation reagent, adopt liquid-phase coprecipitation, with manganese nitrate, nickel nitrate, cobalt nitrate is dissolved in the ionized water, is mixed with mixed solution, again carbonic hydroammonium is added deionized water and be mixed with precipitant solution, ammonium bicarbonate soln slowly is added drop-wise in the metal nitrate mixed solution,, leaves standstill with ammoniacal liquor control pH value, again with deionized water and absolute ethanol washing suction filtration, thermal decomposition is ground in oven dry, grind again, calcining, grinding the back pre-molding is green compact, through isostatic cool pressing, high temperature sintering, semiconductor is cut, scribing obtains thermistor chip, adopts epoxy resin that chip is sealed, and can obtain ternary-system chip negative temperature coefficient thermal resistor; Wherein each component molar percentage is: Mn: Ni: Co=30-70: 1-15: 29-55.
2. according to the preparation method of the described ternary-system chip negative temperature coefficient thermal resistor of claim 1, it is characterized in that following these steps to carrying out:
A, take by weighing raw material manganese nitrate, nickel nitrate, cobalt nitrate at first respectively, mix and dissolve in the deionized water, be mixed with mixed solution;
B, analytically pure carbonic hydroammonium is dissolved in the deionized water, fully stirring and dissolving is mixed with the ammonium bicarbonate precipitation agent solution;
C, the ammonium bicarbonate precipitation agent solution slowly is added drop-wise in the step a mixed solution, stirs, the control heating-up temperature is at 30-50 ℃, and pH value is controlled at 7.8-9, does not stop stirring in the course of reaction;
D, reacted precipitated liquid is left standstill 24h, adopt deionized water wash 5 times earlier after, use absolute ethanol washing again 3 times, put into baking oven and under 80 ℃, carry out dried;
E, with the powder after the steps d dried, grind dispersion treatment, powder at 400-600 ℃ of thermal decomposition 1.5-3h, is further ground, and, promptly obtains MnNiCoO ternary system thermistor nm-class oxide powder at 700-900 ℃ of calcining 1.5-3h;
F, the powder after the step e calcining is ground once more, powder is with 30-40Kg/cm
2Pressure carry out compound stalk forming, the time is 1-10min, and the block materials of moulding is carried out isostatic cool pressing, is pressurize 1-10min under the 300-400MPa at pressure, in 1100-1200 ℃ of high temperature sintering 1-3h, makes the negative temperature coefficient thermosensitive ceramics block materials then;
G, employing semiconductor cutting technique, ceramic block material section, blackening electrode, scribing with sintering promptly get thermistor chip;
H, with the epoxy sealing chip for preparing, can obtain ternary-system chip negative temperature coefficient thermal resistor, its parameter is B
25/50=3920K ± 1%, R
25 ℃=1.0-4.0K Ω ± 3%.
3. according to the described method of claim 2, it is characterized in that step a manganese nitrate, nickel nitrate, cobalt nitrate mixed solution control metal ion molar concentration are 1mol/L.
4. according to the described method of claim 2, it is characterized in that step b carbonic hydroammonium is dissolved in that the control molar concentration is 1.25mol/L in the deionized water.
5. according to the described method of claim 2, it is characterized in that step e powder granule size is 50-120nm.
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2009
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Cited By (13)
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| CN102249649A (en) * | 2011-04-28 | 2011-11-23 | 华南理工大学 | Thermal sensitive ceramic and preparation method thereof |
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| CN102285789B (en) * | 2011-05-31 | 2013-10-16 | 中国科学院新疆理化技术研究所 | Pb-containing four-component system thermosensitive resistor with negative temperature coefficient |
| CN105140505A (en) * | 2015-06-30 | 2015-12-09 | 贵州省分析测试研究院 | Preparation method for cobalt-manganese-nickel oxides |
| CN105575569B (en) * | 2016-02-26 | 2018-07-27 | 深圳市固电电子有限公司 | The preparation method of thermistor chip |
| CN105575569A (en) * | 2016-02-26 | 2016-05-11 | 深圳市固电电子有限公司 | Thermistor chip and preparation method thereof |
| CN106876069A (en) * | 2017-03-13 | 2017-06-20 | 中国科学院新疆理化技术研究所 | The uniform co-precipitation preparation method of manganese cobalt nickel based negative temperature coefficient thermistor material |
| CN107473715A (en) * | 2017-09-27 | 2017-12-15 | 深圳市特普生传感有限公司 | A kind of ternary system NTC thermistor material and its manufacture method |
| CN107473715B (en) * | 2017-09-27 | 2020-11-20 | 深圳市特普生传感有限公司 | Ternary system NTC thermistor material and manufacturing method thereof |
| CN109053158A (en) * | 2018-08-28 | 2018-12-21 | 深圳市汇北川电子技术有限公司 | Thermal sensitive ceramic powder, NTC heat sensitive chip, temperature sensor and preparation method |
| CN109053158B (en) * | 2018-08-28 | 2021-11-05 | 深圳市汇北川电子技术有限公司 | Thermosensitive ceramic powder, NTC thermosensitive chip, temperature sensor and preparation method |
| CN111872370A (en) * | 2020-07-15 | 2020-11-03 | 深圳市惠拓电子材料有限公司 | Preparation method of NTC thermistor material with ultrafine particle size |
| CN112992449A (en) * | 2020-12-09 | 2021-06-18 | 中国科学院新疆理化技术研究所 | Low-temperature spinel oxide negative temperature coefficient thermistor and preparation method thereof |
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| CN101719404B (en) | 2011-03-16 |
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