CN112259311A - Chip NTC thermistor and preparation method thereof - Google Patents
Chip NTC thermistor and preparation method thereof Download PDFInfo
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- CN112259311A CN112259311A CN202011072236.8A CN202011072236A CN112259311A CN 112259311 A CN112259311 A CN 112259311A CN 202011072236 A CN202011072236 A CN 202011072236A CN 112259311 A CN112259311 A CN 112259311A
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- 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
- H01C7/042—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 mainly consisting of inorganic non-metallic substances
- H01C7/043—Oxides or oxidic compounds
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Abstract
The invention provides a chip NTC thermistor, which comprises negative temperature coefficient oxide thermistor powder and a casting agent carrier, and comprises the following components in percentage by mass: NTC thermistor powder: 50-80%, casting agent carrier: 20 to 40 percent. Wherein: the NTC thermistor powder comprises the following chemical components: Mn0.6Ni0.2-xCo0.2-x.2x (MgAl2) O4, wherein x is 0-20 mol%. The invention adopts the superfine powder technology to synthesize NTC thermosensitive fine powder, and adopts the technologies of tape casting technology, high-precision cutting technology, sintering technology and the like to obtain the chip type NTC thermosensitive resistor, the size of the resistor is 1.0mm multiplied by 0.5 mm; the allowable deviation of the material constant B value is +/-1%, and the resistance value is adjustable. The preparation method has the advantages of good and simple process performance and easy control of product quality.
Description
Technical Field
The invention relates to a chip negative temperature coefficient thermistor and a manufacturing method thereof.
Background
At present, the negative temperature coefficient thermistor is widely applied to the occasions of temperature control, temperature detection, temperature compensation, integrated circuit protection and the like, wherein the chip NTC thermistor can be used for temperature control, temperature detection, temperature compensation and integrated circuit protection in the fields of telecommunication, household appliances, automobiles, medical treatment and the like. In recent years, due to rapid development of these fields, particularly in the mobile communication and automobile industries, the requirements of the chip NTC thermistors used in these industries, particularly as temperature compensated crystal oscillators, have been remarkably increased, and because the production of the chip NTC thermistors, particularly the production of the chip NTC thermistors therein, requires excessive investment and also has many technical process factor constraints, the performance of the chip NTC thermistors, such as low precision, has not been able to meet these requirements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a small-size high-precision multilayer chip negative temperature coefficient thermistor and a manufacturing method thereof.
In order to achieve the purpose, the invention adopts a chemical coprecipitation technology to synthesize fine NTC thermosensitive powder, and adopts casting technology (thin belt casting), high-precision cutting, sintering technology and other process technologies to obtain the chip negative temperature coefficient thermistor. A chip NTC thermistor comprises Negative Temperature Coefficient (NTC) oxide thermistor powder and a casting agent carrier, and comprises the following components in percentage by mass: NTC thermistor powder: 50-80%, casting agent carrier: 20 to 40 percent. Wherein: the NTC thermistor powder comprises the following chemical components: Mn0.6Ni0.2-xCo0.2-x.2x (MgAl2) O4, wherein x is 0-20 mol%; the casting agent carrier comprises the following components in percentage by mass: the organic carrier comprises an organic solvent, a dispersant, a binder, a plasticizer and the like, wherein the organic solvent accounts for 65-80% of the total weight of the casting agent carrier and is a mixture of ethylene glycol, absolute ethyl alcohol, methyl ethyl ketone, isopropanol, ethyl acetate and the like; the dispersant accounts for 1-3% of the total weight of the casting agent carrier and is herring fish oil; the adhesive accounts for 15-30% of the total weight of the casting agent carrier and is a mixture of poly (methyl polyacrylamide), polyvinyl butyral and the like; the plasticizer accounts for 0.5-3% of the total weight of the organic carrier and comprises polyethylene glycol, butyl benzyl phthalate, dibutyl phthalate and the like. A preparation method of a negative temperature coefficient thermistor is characterized by comprising the following steps: (1) according to the proportion of the chemical components of the NTC thermistor powder, metal salt raw materials such as manganese sulfate, nickel sulfate, cobalt sulfate, magnesium sulfate, aluminum sulfate and the like are respectively weighed and mixed, deionized water is added and fully stirred to form a metal salt solution, oxalic acid aqueous solution with the same molar equivalent is added into the stirred metal salt solution, the pH value of the reaction solution is adjusted to 6.5-8.0 by ammonia water to obtain a coprecipitation product, and then the coprecipitation product is washed, dried and ground by deionized water to obtain a Negative Temperature Coefficient (NTC) oxide thermosensitive precipitation precursor; then the precursor powder is put into a muffle furnace for heat treatment at 900-1100 ℃ for 2-6 hours, and the Negative Temperature Coefficient (NTC) oxide heat-sensitive powder is obtained after grinding. (2) Respectively weighing NTC thermosensitive powder and a casting agent according to the mass percent by adopting the casting agent matched with the obtained NTC thermosensitive fine powder material, and grinding and mixing the NTC thermosensitive powder and the casting agent in an agate tank for 24-80 hours to obtain negative temperature coefficient thermosensitive casting slurry; (3) forming a film on the obtained negative temperature coefficient thermosensitive casting slurry on a casting thin belt casting machine, wherein the thickness of a single-layer diaphragm is 20um +/-2 um, the thickness of a multi-layer diaphragm is 500um +/-20 um, and after lamination, hot pressing, linear cutting and high-temperature discharging and bonding, placing the single-layer diaphragm and the multi-layer diaphragm into a sintering furnace for high-temperature sintering at the sintering temperature of 1100-1300 ℃ for 1-8 hours to obtain a sheet NTC thermosensitive sintering body; (4) and preparing an outer electrode from the obtained NTC heat-sensitive sintered body, then carrying out three-layer electroplating, and carrying out heat aging at 125 ℃ for more than 1000 hours to obtain a finished product, namely the chip NTC heat-sensitive resistor with the element size of 1.0mm multiplied by 0.5mm (0402). The NTC thermistor material prepared by the multilayer structure has the constant B of 3400-. .
The invention adopts the superfine powder technology to synthesize NTC thermosensitive fine powder, and adopts the casting technology (thin belt casting), the high-precision cutting technology, the sintering technology and other technologies to obtain the chip type NTC thermosensitive resistor, the size of the resistor is 1.0mm multiplied by 0.5 mm; the allowable deviation of the material constant B value is +/-1%, and the resistance value is adjustable. The preparation method has the advantages of good and simple process performance and easy control of product quality.
Detailed Description
Example 1
A chip NTC thermistor and its preparation method, its ingredient is made up of Negative Temperature Coefficient (NTC) oxide thermistor powder, tape casting agent carrier, the component is made up of the following mass percent content: NTC thermistor powder: 75%, casting agent carrier: 25 percent. And is prepared by the following method:
the method comprises the following steps: (1) according to the chemical component Mn of the NTC thermistor powder0.6Ni0.2Co0.2O4The preparation method comprises the steps of mixing metal salt raw materials such as manganese sulfate, nickel sulfate, cobalt sulfate and the like which are respectively weighed, adding deionized water, fully stirring to form a metal salt solution, adding oxalic acid aqueous solution with the same molar equivalent into the stirred metal salt solution, adjusting the pH value of the reaction solution to 7.0 by using ammonia water to obtain a coprecipitation product, and then washing, drying and grinding the coprecipitation product by using deionized water to obtain a Negative Temperature Coefficient (NTC) oxide thermosensitive precipitation precursor; and then putting the precursor powder into a muffle furnace for heat treatment at 950 ℃ for 4 hours, and grinding to obtain Negative Temperature Coefficient (NTC) oxide heat-sensitive powder. (2) Respectively weighing NTC thermosensitive powder and a casting agent according to the mass percent in the embodiment 1 by adopting the casting agent matched with the obtained NTC thermosensitive fine powder material, and grinding and mixing the NTC thermosensitive powder and the casting agent in an agate tank for 24 hours to obtain negative temperature coefficient thermosensitive casting slurry; (3) forming a film on the obtained negative temperature coefficient thermosensitive casting slurry on a casting thin belt casting machine, wherein the thickness of a single-layer diaphragm is 20um +/-2 um, the thickness of a multi-layer diaphragm is 500um +/-20 um, and after lamination, hot pressing, high-precision cutting and high-temperature discharging and bonding, placing the single-layer diaphragm and the multi-layer diaphragm into a sintering furnace for high-temperature sintering at 1150 ℃ for 4 hours to obtain a sheet type NTC thermosensitive sintering body; (4) preparing an outer electrode from the obtained NTC heat-sensitive sintered body, electroplating three layers, and heat aging at 125 deg.C for more than 1000 hr to obtain a finished product, i.e. a sheet type NTC heat-sensitive sintered body with element size of 1.0mm × 0.5mm × 0.5mm (0402)A sensitive resistor. The NTC thermistor material constant manufactured by the multilayer structure has the material constant B of 3480 and the resistance value of 2.5k omega at 25 ℃.
Example 2
A chip NTC thermistor and its preparation method, its ingredient is made up of Negative Temperature Coefficient (NTC) oxide thermistor powder, tape casting agent carrier, the component is made up of the following mass percent content: NTC thermistor powder: 70%, casting agent carrier: 30 percent. And is prepared by the following method:
the method comprises the following steps: (1) according to the chemical component Mn of the NTC thermistor powder0.6Ni0.15Co0.15·0.1(MgAl2)O4The preparation method comprises the steps of weighing metal salt raw materials such as manganese sulfate, nickel sulfate, cobalt sulfate, magnesium sulfate and aluminum sulfate respectively, mixing, adding deionized water, fully stirring to form a metal salt solution, adding oxalic acid aqueous solution with the same molar equivalent into the stirred metal salt solution, adjusting the pH value of the reaction solution to 7.2 by using ammonia water to obtain a coprecipitation product, and then washing, drying and grinding the coprecipitation product by using deionized water to obtain a Negative Temperature Coefficient (NTC) oxide thermosensitive precipitation precursor; and then putting the precursor powder into a muffle furnace for heat treatment at 1000 ℃ for 5 hours, and grinding to obtain Negative Temperature Coefficient (NTC) oxide heat-sensitive powder. (2) Respectively weighing NTC thermosensitive powder and a casting agent according to the mass percent in the embodiment 1 by adopting the casting agent matched with the obtained NTC thermosensitive fine powder material, and grinding and mixing the NTC thermosensitive powder and the casting agent in an agate tank for 48 hours to obtain negative temperature coefficient thermosensitive casting slurry; (3) forming a film on the obtained negative temperature coefficient thermosensitive casting slurry on a casting thin belt casting machine, wherein the thickness of a single-layer diaphragm is 20um +/-2 um, the thickness of a multi-layer diaphragm is 500um +/-20 um, and after lamination, hot pressing, high-precision cutting and high-temperature discharging and bonding, placing the single-layer diaphragm and the multi-layer diaphragm into a sintering furnace for high-temperature sintering at the sintering temperature of 1200 ℃ for 4 hours to obtain a sheet type NTC thermosensitive sintering body; (4) and preparing an outer electrode from the obtained NTC heat-sensitive sintered body, then carrying out three-layer electroplating, and carrying out heat aging at 125 ℃ for more than 1000 hours to obtain a finished product, namely the chip NTC heat-sensitive resistor with the element size of 1.0mm multiplied by 0.5mm (0402). Made of such a multilayer structureThe NTC thermistor has a material constant B of 3850 and a resistance value of 15 kOmega at 25 ℃.
Example 3
A chip NTC thermistor and its preparation method, its ingredient is made up of Negative Temperature Coefficient (NTC) oxide thermistor powder, tape casting agent carrier, the component is made up of the following mass percent content: NTC thermistor powder: 82%, casting agent carrier: 18 percent. And is prepared by the following method:
the method comprises the following steps: (1) according to the chemical component Mn of the NTC thermistor powder0.6Ni0.1Co0.1·0.2(MgAl2)O4The preparation method comprises the steps of weighing metal salt raw materials such as manganese sulfate, nickel sulfate, cobalt sulfate, magnesium sulfate and aluminum sulfate respectively, mixing, adding deionized water, fully stirring to form a metal salt solution, adding oxalic acid aqueous solution with the same molar equivalent into the stirred metal salt solution, adjusting the pH value of a reaction solution to 7.8 by using ammonia water to obtain a coprecipitation product, and then washing, drying and grinding the coprecipitation product by using deionized water to obtain a Negative Temperature Coefficient (NTC) oxide thermosensitive precipitation precursor; and then putting the precursor powder into a muffle furnace for carrying out heat treatment at 1050 ℃ for 5 hours, and grinding to obtain Negative Temperature Coefficient (NTC) oxide heat-sensitive powder. (2) Respectively weighing NTC thermosensitive powder and a casting agent according to the mass percent in the embodiment 1 by adopting the casting agent matched with the obtained NTC thermosensitive fine powder material, and grinding and mixing the NTC thermosensitive powder and the casting agent in an agate tank for 60 hours to obtain negative temperature coefficient thermosensitive casting slurry; (3) forming a film on the obtained negative temperature coefficient thermosensitive casting slurry on a casting thin belt casting machine, wherein the thickness of a single-layer diaphragm is 20um +/-2 um, the thickness of a multi-layer diaphragm is 500um +/-20 um, and after lamination, hot pressing, high-precision cutting and high-temperature discharging and bonding, placing the single-layer diaphragm and the multi-layer diaphragm into a sintering furnace for high-temperature sintering at 1250 ℃ for 4 hours to obtain a sheet type NTC thermosensitive sintering body; (4) and preparing an outer electrode from the obtained NTC heat-sensitive sintered body, then carrying out three-layer electroplating, and carrying out heat aging at 125 ℃ for more than 1000 hours to obtain a finished product, namely the chip NTC heat-sensitive resistor with the element size of 1.0mm multiplied by 0.5mm (0402). The NTC thermistor with multilayer structure has material constant of 4300 and 25 deg.C resistance50kΩ。
Example 4
A chip NTC thermistor and its preparation method, its ingredient is made up of Negative Temperature Coefficient (NTC) oxide thermistor powder, tape casting agent carrier, the component is made up of the following mass percent content: NTC thermistor powder: 68%, casting agent carrier: 32 percent. And is prepared by the following method:
the method comprises the following steps: (1) according to the proportion of the chemical component Mn0.6Ni0.75Co0.175.0.05 (MgAl2) O4 of the NTC thermistor powder, metal salt raw materials such as manganese sulfate, nickel sulfate, cobalt sulfate, magnesium sulfate, aluminum sulfate and the like are respectively weighed and mixed, deionized water is added, the mixture is fully stirred to form a metal salt solution, oxalic acid aqueous solution with the same molar equivalent is added into the stirred metal salt solution, the pH value of the reaction solution is adjusted to be 7.5 by ammonia water to obtain a coprecipitation product, and then deionized water is used for washing, drying and grinding to obtain a Negative Temperature Coefficient (NTC) oxide thermosensitive precipitation precursor; and then putting the precursor powder into a muffle furnace for heat treatment at 1000 ℃ for 6 hours, and grinding to obtain Negative Temperature Coefficient (NTC) oxide heat-sensitive powder. (2) Respectively weighing NTC thermosensitive powder and a casting agent according to the mass percent in the embodiment 1 by adopting the casting agent matched with the obtained NTC thermosensitive fine powder material, and grinding and mixing the NTC thermosensitive powder and the casting agent in an agate tank for 75 hours to obtain negative temperature coefficient thermosensitive casting slurry; (3) forming a film on the obtained negative temperature coefficient thermosensitive casting slurry on a casting thin belt casting machine, wherein the thickness of a single-layer diaphragm is 20um +/-2 um, the thickness of a multi-layer diaphragm is 500um +/-20 um, and after lamination, hot pressing, high-precision cutting and high-temperature discharging and bonding, placing the single-layer diaphragm and the multi-layer diaphragm into a sintering furnace for high-temperature sintering at the sintering temperature of 1200 ℃ for 3 hours to obtain a sheet type NTC thermosensitive sintering body; (4) and preparing an outer electrode from the obtained NTC heat-sensitive sintered body, then carrying out three-layer electroplating, and carrying out heat aging at 125 ℃ for more than 1000 hours to obtain a finished product, namely the chip NTC heat-sensitive resistor with the element size of 1.0mm multiplied by 0.5mm (0402). The NTC thermistor manufactured by the multilayer structure has a material constant BB of 3670 and a resistance value of 10k omega at 25 ℃.
Claims (2)
1. A chip NTC thermistor comprises the following components in percentage by mass: 50-80% of NTC thermistor powder and 20-40% of casting agent carrier; the NTC thermistor powder comprises the following chemical components: Mn0.6Ni0.2-xCo0.2-x.2x (MgAl2) O4, wherein x is 0-20 mol%; the casting agent carrier comprises the following components in percentage by mass: the organic carrier comprises an organic solvent, a dispersant, a binder and a plasticizer, wherein the organic solvent accounts for 65-80% of the total weight of the casting agent carrier and comprises a mixture of ethylene glycol, absolute ethyl alcohol, methyl ethyl ketone, isopropanol, ethyl acetate and the like; the dispersant is 1-3% of the total weight of the casting carrier and comprises herring oil; the adhesive accounts for 15-30% of the total weight of the casting agent carrier and is a mixture of poly (methyl polyacrylamide), polyvinyl butyral and the like; the plasticizer accounts for 0.5-3% of the total weight of the organic carrier and comprises polyethylene glycol, butyl benzyl phthalate, dibutyl phthalate and the like.
2. The method of claim 1, comprising the steps of:
(1) respectively weighing metal salt raw materials such as manganese sulfate, nickel sulfate, cobalt sulfate, magnesium sulfate, aluminum sulfate and the like, mixing, adding deionized water, fully stirring to form a metal salt solution, adding oxalic acid aqueous solution with the same molar equivalent into the stirred metal salt solution, adjusting the pH value of the reaction solution to 6.5-8.0 by using ammonia water to obtain a coprecipitation product, and then washing, drying and grinding by using deionized water to obtain a negative temperature coefficient oxide thermosensitive precipitation precursor; then the precursor powder is put into a muffle furnace for heat treatment at 900-1100 ℃ for 2-6 hours, and the negative temperature coefficient oxide heat-sensitive powder is obtained after grinding.
(2) Respectively weighing NTC thermosensitive powder and a casting agent by adopting the casting agent matched with the obtained NTC thermosensitive fine powder material, and grinding and mixing the NTC thermosensitive powder and the casting agent in an agate tank for 24-80 hours to obtain negative temperature coefficient thermosensitive casting slurry;
(3) forming a film on the obtained negative temperature coefficient thermosensitive casting slurry on a casting thin belt casting machine, wherein the thickness of a single-layer diaphragm is 20um +/-2 um, the thickness of a multi-layer diaphragm is 500um +/-20 um, and after lamination, hot pressing, high-precision cutting and high-temperature discharging and bonding, placing the single-layer diaphragm and the multi-layer diaphragm into a sintering furnace for high-temperature sintering at the sintering temperature of 1100-1300 ℃ for 1-8 hours to obtain a sheet NTC thermosensitive sintering body;
(4) and preparing an outer electrode from the obtained NTC thermosensitive sintered body, then carrying out three-layer electroplating, and carrying out thermal aging at 125 ℃ for more than 1000 hours to obtain a finished product, namely the chip NTC thermistor with the element size of 1.0mm multiplied by 0.5 mm. The NTC thermistor material prepared by the multilayer structure has the constant B of 3400-.
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| CN1246713A (en) * | 1998-08-28 | 2000-03-08 | 中国科学院新疆物理研究所 | Thermosensitive resistor for measuring wind speed |
| CN1610017A (en) * | 2003-10-21 | 2005-04-27 | 上海春叶实业有限公司 | Multilayer sheet type negative temperature coefficient thermosensitive resistor and producing method thereof |
| CN101318814A (en) * | 2008-07-10 | 2008-12-10 | 中国计量学院 | Hydrothermal reaction method for manufacturing negative temperature coefficient heat-sensitive powder |
| CN104961471A (en) * | 2015-07-03 | 2015-10-07 | 深圳市固电电子有限公司 | Cast film slurry of ultrathin lamination flaky inductor and manufacturing method for cast film of ultrathin lamination flaky inductor |
| CN110106485A (en) * | 2019-05-18 | 2019-08-09 | 中国科学院新疆理化技术研究所 | A kind of negative temperature coefficient heat-sensitive film and preparation method thereof |
| CN111718194A (en) * | 2020-07-02 | 2020-09-29 | 内蒙古科技大学 | Antiferroelectric material, preparation method thereof and capacitor containing antiferroelectric material |
-
2020
- 2020-10-09 CN CN202011072236.8A patent/CN112259311A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1246713A (en) * | 1998-08-28 | 2000-03-08 | 中国科学院新疆物理研究所 | Thermosensitive resistor for measuring wind speed |
| CN1610017A (en) * | 2003-10-21 | 2005-04-27 | 上海春叶实业有限公司 | Multilayer sheet type negative temperature coefficient thermosensitive resistor and producing method thereof |
| CN101318814A (en) * | 2008-07-10 | 2008-12-10 | 中国计量学院 | Hydrothermal reaction method for manufacturing negative temperature coefficient heat-sensitive powder |
| CN104961471A (en) * | 2015-07-03 | 2015-10-07 | 深圳市固电电子有限公司 | Cast film slurry of ultrathin lamination flaky inductor and manufacturing method for cast film of ultrathin lamination flaky inductor |
| CN110106485A (en) * | 2019-05-18 | 2019-08-09 | 中国科学院新疆理化技术研究所 | A kind of negative temperature coefficient heat-sensitive film and preparation method thereof |
| CN111718194A (en) * | 2020-07-02 | 2020-09-29 | 内蒙古科技大学 | Antiferroelectric material, preparation method thereof and capacitor containing antiferroelectric material |
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