CN107473715B - Ternary system NTC thermistor material and manufacturing method thereof - Google Patents
Ternary system NTC thermistor material and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a ternary NTC thermistor material and a preparation method thereof, wherein the thermistor material is prepared from manganese nitrate, nickel nitrate and aluminum nitrate as raw materials, and the molar percentages of the components are as follows: manganese: nickel: aluminum is 50-80:25-45: 5-40. The manufacturing method of the thermistor material comprises the following steps: manganese nitrate, nickel nitrate and aluminum nitrate are used as raw materials to prepare an ion mixed solution; preparing a precipitant solution; adding the ionic mixed solution into the precipitant solution to react; repeatedly cleaning the precipitate with deionized water for 3-5 times, and dehydrating with ethanol and filtering to obtain powder; grinding the powder, decomposing at 450 deg.C, and pre-sintering; presintering the powder, and ball-milling the powder into particles; performing ball milling to obtain a blank, performing isostatic pressing on the blank, and sintering to obtain a thermistor ceramic ingot; cutting the thermistor ceramic ingot into ceramic pieces; then, the electrodes are coated and sintered to obtain the thermistor.
Description
Technical Field
The invention relates to a thermistor, in particular to a ternary system NTC thermistor material and a manufacturing method thereof.
Background
NTC (Negative Temperature Coefficient, broadly refers to a semiconductor material or a component with a large Negative Temperature Coefficient) thermistor material is a semiconductor electronic ceramic, and is a sensitive material most widely applied to the field of Temperature measurement. Its characteristics are that its impedance changes with the temperature change, and this corresponding relation determines the temperature coefficient and the microscopic crystal structure of the material. Conversely, the temperature profile of a thermistor is subject to a series of microscopic factors such as its own crystal structure, composition, size, material composition, etc. Therefore, controllability of the material structure and uniformity of the material components play a crucial role in repeatability and stability of thermistor chip production.
In patent documents CN1588576A and CN1588574A, parameters such as pH and concentration of the coprecipitation reaction need to be strictly controlled to complete the precipitation. As is known, the pH is a reaction parameter which is difficult to control without introducing external basic ions, and it is very difficult to control the completion of the reaction by controlling the pH, which makes the repeatability of the process difficult to achieve.
The manganese-nickel-aluminum thermistor is mainly manufactured by Nippon Zhipu company, and because the manganese-nickel spinel phase is a very stable structure, the finished product has good stability, and the manganese-nickel system is insensitive to the component requirement and is suitable for mass production; however, due to the presence of nickel, it is difficult to ensure the reproducibility of nickel precipitation in the conventional co-precipitation method. Adjusting the pH value by ammonia water, wherein each operator can obtain different results in each preparation; sodium ions can be brought in by using a sodium hydroxide solution as a precipitator, so that the characteristics of the product are influenced; however, the solid phase method has the disadvantages that the synthesis temperature of manganese and nickel is higher, particularly the doping of aluminum causes the synthesis temperature to be higher, the sintering density is generally lower, and the product performance is influenced.
Therefore, the invention aims to solve the problem of difficulty in synthesizing the manganese-nickel-aluminum thermistor material system at lower synthesis temperature and excellent repeatability, so that the manganese-nickel-aluminum thermistor material system can be industrially produced.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a manganese-nickel-aluminum ternary NTC thermistor material and a manufacturing method thereof, wherein the material has the advantages of simple process, good repeatability, high stability and industrial production.
In order to achieve the purpose, the invention provides a ternary NTC thermistor material which is prepared from the following raw materials in percentage by mole:
manganese, nickel, aluminium (50-80), 25-45, 5-40).
A manufacturing method of a ternary system NTC thermistor material comprises the following steps:
a. weighing manganese nitrate, nickel nitrate and aluminum nitrate as raw materials in proportion, and dissolving the three raw materials in water to prepare an ionic mixed solution;
b. mixing ammonium bicarbonate, ammonia water, alcohol and water to prepare a precipitator solution;
c. heating the precipitant solution to 40-50 ℃, and adding the ionic mixed solution in the step a into the precipitant solution under vigorous stirring to perform precipitation reaction;
d. after the precipitation reaction is completed, standing for 4-24 hours, taking out the precipitate, repeatedly cleaning the precipitate for 3-5 times by using deionized water, then dehydrating and filtering by using ethanol, and drying at 80-100 ℃ to obtain powder, namely a precursor of the thermistor material;
e. d, grinding the powder obtained in the step d, decomposing the powder at 450 ℃ for 0.5 to 2 hours, and presintering the powder at 950-1150 ℃ for 2 to 4 hours;
f. c, after the pre-sintering in the step e, ball-milling to prepare particles with the particle size of 0.8-3 microns;
g. ball-milling, preforming to obtain blank, isostatic pressing to obtain blank with pressure of 2-3MPa/cm2；
h. Sintering at 1250-1300 ℃ for 2-4 hours after isostatic pressing to obtain a thermistor porcelain ingot;
i. cutting the thermistor porcelain ingot into porcelain pieces with the thickness of 0.3-0.6 mm;
j. and cleaning the ceramic chip, and coating and sintering electrodes on two surfaces of the ceramic chip to obtain the thermistor.
Preferably, the concentration of the ionic mixed liquid is 1-1.5 mol/L.
Preferably, the concentration of ammonium bicarbonate in the precipitant solution is 1.5-3mol/L, and the concentration of ammonia water is 0.2-1 mol/L.
Preferably, the molar ratio of the total of manganese nitrate, nickel nitrate and aluminum nitrate to ammonium bicarbonate in the ionic mixed solution is 1: (2-3).
Preferably, the material of the electrode is one of silver paste, gold paste or palladium paste.
The invention has the following beneficial effects:
1. the invention does not need to strictly control parameters such as pH value, concentration and the like, only needs to slightly add the surfactant, utilizes the amphiprotic characteristic of the aluminum hydroxide, and can obtain the powder with uniform particles under the condition of controlling the stable reaction speed.
2. The invention can prepare the thermistor material with high stability at lower synthesis temperature.
3. The method has simple process, realizes the repeatability of the reaction process by fixing the ratio of the cations to the anions, controlling the feeding speed and controlling the reaction temperature, and can realize industrial production.
Detailed Description
The present invention provides a ternary NTC thermistor material and a method for manufacturing the same, and the following description will be given by taking specific experimental cases as examples to illustrate specific embodiments, it should be understood that the specific embodiments described herein are only for explaining the present invention and are not intended to limit the present invention.
Manganese nitrate, nickel nitrate, aluminum nitrate, ammonium bicarbonate, ammonia, alcohol, absolute ethanol, and silver paste used in the examples of the present invention are commercially available.
Example 1:
a. manganese nitrate, nickel nitrate and aluminum nitrate which are 3mol in total are taken as raw materials, deionized water is added to prepare 1mol/L ionic mixed liquid, wherein the molar percentage of each component is as follows: manganese: nickel: aluminum 60:30: 10.
b. Mixing ammonium bicarbonate, ammonia water, alcohol and water to prepare a precipitator solution, wherein the formula of the precipitator solution is as follows: 6 mol of ammonium bicarbonate, 1mol of ammonia water and 100 ml of alcohol, wherein the concentration of ammonium bicarbonate in the precipitator solution is 2 mol/L.
c. And c, in a water bath with the reaction temperature of 45 +/-1 ℃, uniformly adding the ionic mixed solution in the step a into a precipitant solution under vigorous stirring to perform precipitation reaction, wherein the adding speed is 150 ml/min.
d. And after the precipitation reaction is completed, standing for 8 hours, repeatedly cleaning the precipitate for 3-5 times by using deionized water, then dehydrating and filtering by using ethanol, and drying at 80 ℃ to obtain powder, namely the precursor of the thermistor material.
e. D, grinding the powder obtained in the step d, decomposing for 1 hour at 450 ℃, and presintering for 4 hours at 1100 ℃.
f. After the powder is presintered, the powder is ball-milled into particles with the particle size of 1.9 microns.
g. Performing the ball-milled powder to obtain a blank with a diameter of 40mm and a height of 20mm, and performing isostatic pressing on the blank under a pressure of 2.5MPa/cm2。
h. And (3) sintering for 2 hours at 1280 ℃ after isostatic pressing to obtain the thermistor ceramic ingot.
i. The thermistor porcelain ingot was cut into 0.36mm thick tiles.
j. And cleaning the ceramic chip, and coating and sintering electrodes on two surfaces of the ceramic chip to obtain the thermistor, wherein the electrodes are made of silver paste.
Batching for 8 times according to the steps, and respectively recording data 1A \1B \1C \1D \1E \1F \1G \ 1H.
Example 2:
a. manganese nitrate, nickel nitrate and aluminum nitrate which are 3mol in total are taken as raw materials, deionized water is added to prepare 1mol/L ionic mixed liquid, wherein the molar percentage of each component is as follows: manganese: nickel: aluminum 60:19: 21.
b. Mixing ammonium bicarbonate, ammonia water, alcohol and water to prepare a precipitator solution, wherein the formula of the precipitator solution is as follows: 8 mol of ammonium bicarbonate, 1mol of ammonia water and 100 ml of alcohol, wherein the concentration of ammonium bicarbonate in the precipitator solution is 2 mol/L.
c. And c, in a water bath with the reaction temperature of 48 +/-1 ℃, uniformly adding the ionic mixed solution in the step a into a precipitant solution under vigorous stirring to perform precipitation reaction, wherein the adding speed is 150 ml/min.
d. And after the precipitation reaction is completed, standing for 8 hours, repeatedly cleaning the precipitate for 3-5 times by using deionized water, then dehydrating and filtering by using ethanol, and drying at 90 ℃ to obtain powder, namely the precursor of the thermistor material.
e. D, grinding the powder obtained in the step d, decomposing for 1 hour at 450 ℃, and presintering for 4 hours at 1150 ℃.
f. After the powder is presintered, the powder is ball milled into particles with the particle size of 2.2 microns.
g. Performing the ball-milled powder to obtain a blank with a diameter of 40mm and a height of 20mm, and performing isostatic pressing on the blank under a pressure of 2.5MPa/cm2。
h. And (3) sintering for 2 hours at 1300 ℃ after isostatic pressing to obtain the thermistor ceramic ingot.
i. The thermistor porcelain ingot was cut into 0.36mm thick tiles.
j. And cleaning the ceramic chip, and coating and sintering electrodes on two surfaces of the ceramic chip to obtain the thermistor, wherein the electrodes are made of silver paste.
Batching for 8 times according to the steps, and respectively recording data 2A \2B \2C \2D \2E \2F \2G \ 2H.
Example 3:
a. manganese nitrate, nickel nitrate and aluminum nitrate which are 3mol in total are taken as raw materials, deionized water is added to prepare 1mol/L ionic mixed liquid, wherein the molar percentage of each component is as follows: manganese: nickel: aluminum 56:18: 26.
b. Mixing ammonium bicarbonate, ammonia water, alcohol and water to prepare a precipitator solution, wherein the formula of the precipitator solution is as follows: 6 mol of ammonium bicarbonate, 1mol of ammonia water and 100 ml of alcohol, wherein the concentration of ammonium bicarbonate in the precipitator solution is 1.5 mol/L.
c. And c, in a water bath with the reaction temperature of 40 +/-1 ℃, uniformly adding the ion mixed solution in the step a into a precipitant solution under vigorous stirring to perform precipitation reaction, wherein the adding speed is 150 ml/min.
d. And after the precipitation reaction is completed, standing for 24 hours, repeatedly cleaning the precipitate for 3-5 times by using deionized water, then dehydrating and filtering by using absolute ethyl alcohol, and drying at 100 ℃ to obtain powder, namely the precursor of the thermistor material.
e. D, grinding the powder obtained in the step d, decomposing for 1 hour at 450 ℃, and presintering for 4 hours at 980 ℃.
f. After the powder is presintered, the powder is ball milled into particles with the particle size of 1.0 micron.
g. Performing the ball-milled powder to obtain a blank with a diameter of 40mm and a height of 20mm, and performing isostatic pressing on the blank under a pressure of 3MPa/cm2。
h. And (3) sintering for 4 hours at 1250 ℃ after isostatic pressing to obtain the thermistor porcelain ingot.
i. The thermistor porcelain ingot was cut into 0.36mm thick tiles.
j. And cleaning the ceramic chip, and coating and sintering electrodes on two surfaces of the ceramic chip to obtain the thermistor, wherein the electrodes are made of silver paste.
The materials are prepared for 8 times according to the steps, and the data 3A \3B \3C \3D \3E \3F \3G \3H are respectively recorded.
The data recorded for each experiment in examples 1-3 are shown in table 1. The data in the table are the results of testing the tiles after encapsulation in single-ended glass, wherein the density is measured according to Archimedes' method and the aging at 200 ℃ is the rate of change of resistance before and after exposure to a 200 ℃ environment for 1000 hours.
TABLE 1
As can be seen from Table 1, in the same example, the data of 8 batching experiments have small differences in density, B value constant and resistivity, which indicates that the invention has excellent repeatability; the aging rate of each set of data in examples 1-3 at 200 ℃ is very low, which shows that the ternary NTC thermistor material prepared by the invention has high stability.
Comparing example 1 and example 2, it can be seen that: the concentration of the ion mixed liquid is constant, the mole percentage of aluminum is increased, the mole percentage of nickel is reduced, and the B value constant and the resistivity are both increased.
Finally, it should be noted that: the above-mentioned embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. The ternary system negative temperature coefficient thermistor material is characterized by being prepared from the following raw materials in percentage by mole: manganese, nickel, aluminum (50-80), aluminum (25-45), and manganese (5-40);
the method comprises the following steps:
a. weighing manganese nitrate, nickel nitrate and aluminum nitrate as raw materials in proportion, and dissolving the three raw materials in water to prepare an ionic mixed solution;
b. mixing ammonium bicarbonate, ammonia water, alcohol and water to prepare a precipitator solution;
c. heating the precipitant solution to 40-50 ℃, and adding the ionic mixed solution in the step a into the precipitant solution under vigorous stirring to perform precipitation reaction;
d. after the precipitation reaction is completed, standing for 4-24 hours, taking out the precipitate, repeatedly cleaning the precipitate for 3-5 times by using deionized water, then dehydrating and filtering by using ethanol, and drying at 80-100 ℃ to obtain powder, namely a precursor of the thermistor material;
e. d, grinding the powder obtained in the step d, decomposing the powder at 450 ℃ for 0.5 to 2 hours, and presintering the powder at 950-1150 ℃ for 2 to 4 hours;
f. c, after the pre-sintering in the step e, ball-milling to prepare particles with the particle size of 0.8-3 microns;
g. ball-milling, preforming to obtain blank, isostatic pressing to obtain blank with pressure of 2-3MPa/cm2；
h. Sintering at 1250-1300 ℃ for 2-4 hours after isostatic pressing to obtain a thermistor porcelain ingot;
i. cutting the thermistor porcelain ingot into porcelain pieces with the thickness of 0.3-0.6 mm;
j. cleaning the ceramic chip, and coating electrodes on two surfaces of the ceramic chip to obtain a thermistor;
the concentration of ammonium bicarbonate in the precipitant solution is 1.5-3mol/L, and the concentration of ammonia water is 0.2-1 mol/L.
2. The method of manufacturing a ternary negative temperature coefficient thermistor material of claim 1, wherein the concentration of the ionic liquid mixture is 1 to 1.5 mol/L.
3. The method of manufacturing a ternary negative temperature coefficient thermistor according to claim 1, wherein the molar ratio of the total of manganese nitrate, nickel nitrate and aluminum nitrate to ammonium bicarbonate in the ionic mixture is 1 (2-3).
4. The method of claim 1, wherein the electrode is made of one of silver paste, gold paste, or palladium paste.
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| CN105753473A (en) * | 2016-02-25 | 2016-07-13 | 江苏师范大学 | Preparation method of magneto-optic terbium oxide transparent ceramic |
| CN106390981A (en) * | 2016-09-19 | 2017-02-15 | 常州大学 | Rare earth doped barium titanate nano-powder photocatalyst and preparation method thereof |
| CN106698528A (en) * | 2017-01-25 | 2017-05-24 | 中国科学院新疆理化技术研究所 | Composite oxide material with core-shell structure, and preparation method and application thereof |
| CN106977206A (en) * | 2017-02-22 | 2017-07-25 | 江苏师范大学 | Spraying codepostion prepares the continuation method of high dispersancy nano oxide powder |
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