CN111872370A - Preparation method of NTC thermistor material with ultrafine particle size - Google Patents
Preparation method of NTC thermistor material with ultrafine particle size Download PDFInfo
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- CN111872370A CN111872370A CN202010681084.5A CN202010681084A CN111872370A CN 111872370 A CN111872370 A CN 111872370A CN 202010681084 A CN202010681084 A CN 202010681084A CN 111872370 A CN111872370 A CN 111872370A
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 239000011882 ultra-fine particle Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 49
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004458 analytical method Methods 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 10
- 239000010941 cobalt Substances 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000000779 smoke Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 10
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- SFJBWZNTPHYOEH-UHFFFAOYSA-N cobalt Chemical compound [Co].[Co].[Co] SFJBWZNTPHYOEH-UHFFFAOYSA-N 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- B22F1/0003—
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of an NTC thermistor material with ultrafine particle size, wherein the NTC thermistor material adopts cobalt, nickel and iron powder as raw materials, the preparation method comprises dissolving iron, cobalt and nickel raw material powder in nitric acid analysis solution by nitric acid method, then removing waste liquid, dry-burning and drying to obtain ultramicro-grain-size powder with very high grain-size concentration, then carrying out high-temperature back-burning reduction, finally crushing the hardened powder after back-burning by using a ball-milling method, the method can obtain the powder with both ultrafine particle size and high particle size concentration, and because the particle size of the powder before the back burning is very fine, the hardened powder after the back burning is very easy to crush again, the powder can reach the satisfactory particle size and the higher particle size concentration again only by ball milling for 4-12 hours, the ultrafine particle size powder can be obtained in a short time, and the existence of unstable impurities can be reduced and eliminated.
Description
Technical Field
The invention relates to the technical field of manufacturing of ultrafine-particle-size powder, in particular to a preparation method of an NTC thermistor material with an ultrafine particle size.
Background
Ntc (negative Temperature coefficient) refers to a thermistor phenomenon and a material having a negative Temperature coefficient in which the resistance decreases exponentially with the Temperature rise, and the material is a semiconductor ceramic formed by fully mixing, molding, sintering and other processes of two or more metal oxides of manganese, copper, silicon, cobalt, iron, nickel, zinc and the like, and can be made into a thermistor having a negative Temperature coefficient, and the resistivity and the material constant thereof vary with the material composition ratio, the sintering atmosphere, the sintering Temperature and the structural state. The particle size of the sintered powder is also an important parameter, and generally requires that the powder has a proper ultrafine particle size, and the more uniform the powder is, the better the ultrafine particle size is.
Disclosure of Invention
The invention aims to provide a method for preparing an NTC thermistor material with high speed, high efficiency and high particle size distribution concentration ratio.
The invention is realized by the following steps: the preparation method of the NTC thermistor material with the ultrafine particle size is characterized by comprising the following steps of:
(1) pouring a sufficient amount of nitric acid analysis solution into a beaker, and heating and maintaining the temperature at 55-65 ℃;
(2) firstly, dividing iron powder into a plurality of parts and gradually putting the parts into nitric acid analysis solution, generating bubbles and smoke at the moment, and entering the next step after no bubbles and smoke are generated;
(3) firstly, dividing cobalt powder into multiple parts and gradually putting the multiple parts into nitric acid analysis solution, wherein bubbles and smoke are generated at the moment, and entering the next step after no bubbles and smoke are generated;
(4) firstly, dividing nickel powder into a plurality of parts, gradually putting the parts into nitric acid analysis solution, generating bubbles and smoke at the moment, and entering the next step after no bubbles and smoke are generated;
(5) stopping heating, naturally cooling and precipitating for 1-2 hours, removing the excessive liquid above to leave powder;
(6) transferring the powder in the beaker into a crucible, heating for a period of time, stopping heating when no smoke is generated again, and naturally cooling;
(7) transferring the powder in the crucible into a sagger, putting the sagger into a back burning furnace, heating to 900 ℃ at a constant speed within 4 hours, keeping for 30 minutes, and naturally cooling;
(8) transferring the powder in the sagger to a ball milling tank, and performing ball milling for 4-12 hours by using a ball milling medium with the diameter of 5 and adding pure water;
(9) dehydrating the ball-milled powder, transferring the dehydrated powder into a stainless steel container, and drying the powder in a drying oven at the drying temperature of 110 ℃ for 12 hours;
(10) and sieving the dried powder by using a 60-mesh sieve to obtain a finished product.
The nitric acid analysis solution is concentrated nitric acid with the mass fraction of 65-68%, and the weight ratio of cobalt, nickel and iron powder to the nitric acid analysis solution is 176.8: 58.7: 111.7: 1380.
the parameters of the ball milling process are 250 g of powder, 800 g of ball milling medium and 500 ml of pure water.
Wherein, between the steps (4) and (5), the heating is continued for 3-5 minutes, and then the heating is stopped.
The invention has the beneficial effects that: the preparation method of the NTC thermistor material with the ultrafine particle size comprises the steps of firstly adopting a nitric acid method to dissolve raw material powder of iron, cobalt and nickel in nitric acid analysis liquid in sequence, then removing waste liquid, carrying out dry burning and drying treatment to obtain ultrafine particle size powder with extremely high particle size concentration, then carrying out high-temperature back burning reduction, and finally crushing the hardened powder after back burning by using a ball milling method to obtain the powder with both ultrafine particle size and high particle size concentration.
Drawings
Fig. 1 is a laser particle size analysis result of a final powder product obtained by an example of a preparation method of an NTC thermistor material with an ultrafine particle size according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As an embodiment of the preparation method of the NTC thermistor material with the ultrafine particle size, as shown in fig. 1, the NTC thermistor material adopts cobalt, nickel and iron powder as raw materials, and includes the following steps:
(1) pouring a sufficient amount of nitric acid analysis solution into a beaker, and heating and maintaining the temperature at 55-65 ℃;
(2) firstly, dividing iron powder into a plurality of parts and gradually putting the parts into nitric acid analysis solution, generating bubbles and smoke at the moment, and entering the next step after no bubbles and smoke are generated;
(3) firstly, dividing cobalt powder into multiple parts and gradually putting the multiple parts into nitric acid analysis solution, wherein bubbles and smoke are generated at the moment, and entering the next step after no bubbles and smoke are generated;
(4) firstly, dividing nickel powder into a plurality of parts, gradually putting the parts into nitric acid analysis solution, generating bubbles and smoke at the moment, and entering the next step after no bubbles and smoke are generated;
(5) stopping heating, naturally cooling and precipitating for 1-2 hours, removing the excessive liquid above to leave powder;
(6) transferring the powder in the beaker into a crucible, heating for a period of time, stopping heating when no smoke is generated again, and naturally cooling;
(7) transferring the powder in the crucible into a sagger, putting the sagger into a back burning furnace, heating to 900 ℃ at a constant speed within 4 hours, keeping for 30 minutes, and naturally cooling;
(8) transferring the powder in the sagger to a ball milling tank, and performing ball milling for 4-12 hours by using a ball milling medium with the diameter of 5 and adding pure water;
(9) dehydrating the ball-milled powder, transferring the dehydrated powder into a stainless steel container, and drying the powder in a drying oven at the drying temperature of 110 ℃ for 12 hours;
(10) and sieving the dried powder by using a 60-mesh sieve to obtain a finished product.
The preparation method of the NTC thermistor material with the ultrafine particle size comprises the steps of firstly adopting a nitric acid method to dissolve raw material powder of iron, cobalt and nickel in nitric acid analysis liquid in sequence, then removing waste liquid, carrying out dry burning and drying treatment to obtain ultrafine particle size powder with extremely high particle size concentration, then carrying out high-temperature back burning reduction, and finally crushing the hardened powder after back burning by using a ball milling method to obtain the powder with both ultrafine particle size and high particle size concentration.
In this embodiment, the nitric acid analysis solution is concentrated nitric acid with a mass fraction of 65-68%, the specific gravity is 1.38, and the weight ratio of the cobalt, nickel, iron powder raw material to the nitric acid analysis solution is 176.8: 58.7: 111.7: 1380. the proportion is a material formula with excellent performance, and is particularly suitable for the field of temperature measurement of lithium batteries of new energy vehicles.
Example (c): the data of the product prepared by the above method using 176.8 g of cobalt, 58.7 g of nickel, 111.7 g of iron, and 1000ml of nitric acid analysis solution (1380 g by weight) are shown in the following table:
| laser granularity (um) | Raw material | Powder material after nitric acid method treatment | After ball milling (12 hours) |
| (D10) | 5.42 | 0.19 | 0.72 |
| (D50) | 10.30 | 0.55 | 1.28 |
| (D90) | 18.17 | 1.20 | 3.16 |
The effect of the method is very evident from the above table and figure 1.
In this embodiment, the parameters of the ball milling process are 250 g of powder, 800 g of ball milling medium and 500 ml of pure water, the time is 12 hours, and the processing time is short. The ball milling time can be shortened to 4 hours according to actual conditions and requirements.
In this embodiment, between steps (4) and (5), heating is continued for 3-5 minutes, and then heating is stopped, so as to make the dissolution reaction as complete as possible.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. The preparation method of the NTC thermistor material with the ultrafine particle size is characterized by comprising the following steps of:
(1) pouring a sufficient amount of nitric acid analysis solution into a beaker, and heating and maintaining the temperature at 55-65 ℃;
(2) firstly, dividing iron powder into a plurality of parts and gradually putting the parts into nitric acid analysis solution, generating bubbles and smoke at the moment, and entering the next step after no bubbles and smoke are generated;
(3) firstly, dividing cobalt powder into multiple parts and gradually putting the multiple parts into nitric acid analysis solution, wherein bubbles and smoke are generated at the moment, and entering the next step after no bubbles and smoke are generated;
(4) firstly, dividing nickel powder into a plurality of parts, gradually putting the parts into nitric acid analysis solution, generating bubbles and smoke at the moment, and entering the next step after no bubbles and smoke are generated;
(5) stopping heating, naturally cooling and precipitating for 1-2 hours, removing the excessive liquid above to leave powder;
(6) transferring the powder in the beaker into a crucible, heating for a period of time, stopping heating when no smoke is generated again, and naturally cooling;
(7) transferring the powder in the crucible into a sagger, putting the sagger into a back burning furnace, heating to 900 ℃ at a constant speed within 4 hours, keeping for 30 minutes, and naturally cooling;
(8) transferring the powder in the sagger to a ball milling tank, and performing ball milling for 4-12 hours by using a ball milling medium with the diameter of 5 and adding pure water;
(9) dehydrating the ball-milled powder, transferring the dehydrated powder into a stainless steel container, and drying the powder in a drying oven at the drying temperature of 110 ℃ for 12 hours;
(10) and sieving the dried powder by using a 60-mesh sieve to obtain a finished product.
2. The preparation method of the NTC thermistor material with the ultrafine particle size according to claim 1, wherein the nitric acid analysis solution is concentrated nitric acid with a mass fraction of 65-68%, and the weight ratio of the cobalt, nickel, iron powder raw materials to the nitric acid analysis solution is 176.8: 58.7: 111.7: 1380.
3. the method for preparing the ultra-fine particle size of the NTC thermistor material of claim 1, wherein the parameters of the ball milling process are 250 g of powder, 800 g of ball milling medium and 500 ml of pure water.
4. The NTC thermistor material ultrafine particle size preparation method according to claim 1, further comprising, between steps (4) and (5), continuing heating for 3-5 minutes and then stopping heating.
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