CN110218087A - The preparation method of negative temperature coefficient heat-sensitive resistance material - Google Patents
The preparation method of negative temperature coefficient heat-sensitive resistance material Download PDFInfo
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- CN110218087A CN110218087A CN201910603573.6A CN201910603573A CN110218087A CN 110218087 A CN110218087 A CN 110218087A CN 201910603573 A CN201910603573 A CN 201910603573A CN 110218087 A CN110218087 A CN 110218087A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
Abstract
The invention discloses a kind of preparation method of negative temperature coefficient heat-sensitive resistance material, solve the problems, such as that existing thermistor material inevitably introduces the element of iron-cobalt-nickel.Technical solution of the raw material of following molfraction ratio by being made: La2O3 is 22.5~47.5, CaCO3It is 45~95 for 5~55, Mn, ZrO2Be 5~55, and control raw material in Fe less than 0.001, Co less than 0.001, Ni less than 0.001.Raw material of the present invention is simple, does not add Fe, any element or its compound in tri- kinds of elements of Co, Ni, can realize the adjusting of wide scope room temperature resistance value and material constant B value by CaZrO3, the content adjustment of LaMn3, performance is stablized, and Applicable temperature range is wide.
Description
Technical field
The present invention relates to a kind of thermistor material field, specifically a kind of negative temperature coefficient heat-sensitive resistance material
Preparation method.
Background technique
It is especially in recent years, anti-to the electromagnetism of terminal called equipment with the fast development in the fields such as communication into the new century
The requirement of interference performance is higher and higher.These requirements, the design layout etc. for awarding light current route bring great challenge, big appearance
Anti- induction reactance may be impacted to the reliability of communication.In the case, the component of the low induction reactance of the low capacitive reactance of high reliability is ground
It makes more and more urgent.Traditional thermistor material is generally made of the oxide of transition elements manganese cobalt nickel and iron, many institute's weeks
Know, due to the element electronic configuration of iron-cobalt-nickel, the magnetic characteristic of these types of element is particularly pertinent, the material containing these elements
It is easy magnetization and has higher magnetic conductivity, the material without iron-cobalt-nickel element eliminates the need for this kind of influence, but due to transitional member
The addition of plain sheet cobalt nickel element is conducive to the raising of product stability, as the omission of this dvielement is also meaned to thermistor material
The influence for expecting stability aspect performance, under the premise of not influencing, even improving negative temperature coefficient heat-sensitive resistance material performance, no
Addition iron-cobalt-nickel element is the direction of those skilled in the art's research.
As application number 201910235582.4 discloses a kind of material with resistance negative temperature coefficient (NTC) thermistor
Material, it is characterized in that the material at being grouped into Zn1-x-2yAlxCuyMoyO, wherein 0.001≤x≤0.03,0 y≤0.01 <.This
The NTC thermistor material of invention is formed by main component of zinc oxide, described at being grouped as containing for middle each element by changing
Amount achieve the purpose that adjust thermistor element room temperature resistivity and material constant B value, realize wide scope room temperature resistance value and
The adjusting of material constant B value.Although the material does not contain iron-cobalt-nickel element, due to Zn high-temperature volatile is strong, the material
There is consistency etc. in material.
For another example the patent No. 201410460757.9 discloses negative temperature coefficient heat-sensitive resistance material and preparation method thereof.The heat
The chemical general formula of quick resistance material is CexMnxSi1-xO2x+2, wherein 0.65 < x < 1；B100 DEG C of its material constant/200 DEG C=
(5400~5880) K ± 10%, 25 DEG C of the electricalresistivityρ=Ω cm ± 10% of (3.6~97) × 105,250 DEG C of ρ=(250~
8000) Ω cm ± 10%.The resistance kelvin relation curve of the thermistor material has good line in entire temperature test section
Property, it has stable high-temperature performance, Applicable temperature range is wide, and can continuously adjust thermistor material by adjusting the content of Si in system
Room temperature resistivity.In the technical solution due to SiO2 glass, there are problems that ageing stability.
Summary of the invention
The purpose of the present invention is to solve above-mentioned technical problem, provide that a kind of raw material is simple, does not add Fe, Co, Ni tri-
Any element or its compound in kind element, can pass through CaZrO3, and wide scope room temperature resistance value is realized in the content adjustment of LaMn3
With the adjusting of material constant B value, performance is stablized, the preparation side of the wide negative temperature coefficient heat-sensitive resistance material of Applicable temperature range
Method.
Technical solution is made of the raw material of following molfraction ratio: La2O3 is 22.5~47.5, CaCO3 is 5~55, Mn
Be 5~55 for 45~95, ZrO2, and control raw material in Fe less than 0.001, Co less than 0.001, Ni less than 0.001.
The raw material is made by following step:
A. it is raw material with La2O3, MnCO3, CaCO3, ZrO2, be 22.5~47.5, CaCO3 by La2O3 is 5~55, Mn
After the molfraction ratio mixing for being 5~55 for 45~95, ZrO2 plus water for ball milling is at slurry；
B. the slurry is obtained into solid powder material after drying, calcining；
C. it is dried after the solid powder material being added water for ball milling again, sintering obtains negative temperature coefficient heat after compression moulding
Quick resistance material.
In the step a and c, the ball milling condition are as follows: material: ball: water 1:3:3, Ball-milling Time are 8 hours.
In the step b, the drying temperature is 250 DEG C, and the calcination temperature is 900-1200 DEG C, and the time is that 2-8 is small
When, preferably 6 hours.
In the step c, sintering temperature is 1100-1500 DEG C (preferably 1130 DEG C), and sintering time is 5 hours.
The problem of for background technique, inventor furthers investigate raw material, is not introducing Fe, Co, Ni tri-
Under the premise of kind element, select with La2o3, CaCO3、MnCO3、ZrO2For raw material, wherein La2o3 can be synthesized with MnCO3 into calcium
Titanium ore LaMnO3, CaCO3 can and ZrO2CaZrO3 is synthesized, LaMnO3 resistance and B value are small, CaZrO3 shape that can be big with resistance value
At solid solution, the adjusting of wide scope room temperature resistance value and material constant B value is realized by changing the two content, due to containing rare earth
Element La is solved and is not added Fe in background technique, Co, when Ni element the problem of existing stability.
The utility model has the advantages that
Raw material of the present invention is simple, does not add Fe, and any element or its compound in tri- kinds of elements of Co, Ni can pass through
The content adjustment of CaZrO3, LaMn3 realize that wide scope room temperature resistance value and material constant B value, regulation performance are stablized, applicable for temperature
It is wide to spend range.
Specific embodiment
Embodiment of the method:
A. it is raw material with La2O3, MnCO3, CaCO3, ZrO2, be 22.5~47.5, CaCO3 by La2O3 is 5~55, Mn
After the molar ratio mixing for being 5~55 for 45~95, ZrO2 plus water for ball milling is at slurry, the ball milling condition are as follows: material: ball: water 1:
3:3, Ball-milling Time are 8 hours；
B. the slurry is obtained into solid powder material after drying, calcining, the drying temperature is 250 DEG C, described to forge
Burning temperature is 900-1200 DEG C, and the time is 2-8 hours；
C. it is dried after the solid powder material being added water for ball milling again, sintering obtains negative temperature coefficient heat after compression moulding
Quick resistance material, the ball milling condition are as follows: material: ball: water 1:3:3, Ball-milling Time are 8 hours, and the drying temperature is 250
DEG C, the calcination temperature is 900-1200 DEG C, and the time is 2-8 hours；
Using each embodiment and performance of the above method referring to following table:
Claims (5)
1. a kind of preparation method of negative temperature coefficient heat-sensitive resistance material, which is characterized in that by the raw material of following molfraction ratio
Be made: La2O3 is 22.5~47.5, CaCO3It is 45~95 for 5~55, Mn, ZrO2It is less than for 5~55, Fe less than 0.001, Co
0.001, Ni less than 0.001.
2. the preparation method of negative temperature coefficient heat-sensitive resistance material as described in claim 1, which is characterized in that the raw material warp
Following step is crossed to be made:
A. it is raw material with La2O3, MnCO3, CaCO3, ZrO2, be 22.5~47.5, CaCO3 by La2O3 is 5~55, Mn 45
The molfraction that~95, ZrO2 are 5~55 after mixing than adding water for ball milling at slurry；
B. the slurry is obtained into solid powder material after drying, calcining；
C. it is dried after the solid powder material being added water for ball milling again, sintering obtains negative temperature coefficient thermistor power after compression moulding
Hinder material.
3. the preparation method of negative temperature coefficient heat-sensitive resistance material as claimed in claim 2, which is characterized in that the step a
In c, the ball milling condition are as follows: material: ball: water 1:3:3, Ball-milling Time are 8 hours.
4. the preparation method of negative temperature coefficient heat-sensitive resistance material as claimed in claim 2 or claim 3, which is characterized in that the step
In rapid b, the drying temperature is 250 DEG C, and the calcination temperature is 900-1200 DEG C, and the time is 2-8 hours.
5. the preparation method of negative temperature coefficient heat-sensitive resistance material as claimed in claim 4, which is characterized in that the step c
In, sintering temperature is 1100-1500 DEG C, and sintering time is 5 hours.
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| CN201910603573.6A CN110218087B (en) | 2019-07-05 | 2019-07-05 | Preparation method of negative temperature coefficient thermistor material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548159A (en) * | 2020-05-16 | 2020-08-18 | 中国科学院新疆理化技术研究所 | Zirconate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112960979A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Zirconate system high-temperature negative temperature coefficient thermistor material and preparation method thereof |
| CN114920555A (en) * | 2022-05-16 | 2022-08-19 | 中国科学院新疆理化技术研究所 | Preparation method of manganese-doped calcium zirconate high-temperature negative temperature coefficient thermistor material |
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| JPH08167501A (en) * | 1994-12-12 | 1996-06-25 | Matsushita Electric Ind Co Ltd | Positive thermistor and its manufacture |
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2019
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Patent Citations (5)
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| JPH08167501A (en) * | 1994-12-12 | 1996-06-25 | Matsushita Electric Ind Co Ltd | Positive thermistor and its manufacture |
| KR100366334B1 (en) * | 2000-07-29 | 2002-12-31 | 삼화전자공업 주식회사 | Thermistor with multi function and the manufacturing method |
| CN1374667A (en) * | 2001-03-07 | 2002-10-16 | 株式会社村田制作所 | Multi-layer ceramic capacitor and its producing method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548159A (en) * | 2020-05-16 | 2020-08-18 | 中国科学院新疆理化技术研究所 | Zirconate system negative temperature coefficient thermistor material and preparation method thereof |
| CN112960979A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Zirconate system high-temperature negative temperature coefficient thermistor material and preparation method thereof |
| CN114920555A (en) * | 2022-05-16 | 2022-08-19 | 中国科学院新疆理化技术研究所 | Preparation method of manganese-doped calcium zirconate high-temperature negative temperature coefficient thermistor material |
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Denomination of invention: Preparation method of negative temperature coefficient thermistor material Effective date of registration: 20230203 Granted publication date: 20211207 Pledgee: Longquan Branch of China Construction Bank Co.,Ltd. Pledgor: WEIHAI KEBOLE AUTOMOTIVE ELECTRONICS CO.,LTD. Registration number: Y2023980031955 |