CN107140982A - A kind of preparation method of negative temperature coefficient heat-sensitive resistance material - Google Patents

A kind of preparation method of negative temperature coefficient heat-sensitive resistance material Download PDF

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CN107140982A
CN107140982A CN201710353229.7A CN201710353229A CN107140982A CN 107140982 A CN107140982 A CN 107140982A CN 201710353229 A CN201710353229 A CN 201710353229A CN 107140982 A CN107140982 A CN 107140982A
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temperature coefficient
negative temperature
ball
sensitive resistance
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侯丹
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/006—Apparatus or processes specially adapted for manufacturing resistors adapted for manufacturing resistor chips
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/30—Apparatus or processes specially adapted for manufacturing resistors adapted for baking
    • 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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    • C04B2235/00—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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract

The present invention relates to a kind of preparation method of negative temperature coefficient heat-sensitive resistance material, La2O3、MnCO3、Al2O3It is placed in zirconium ball ball grinder, the ball milling that adds water obtains slurry；Slurry is dried, and solid powder material is calcined to obtain at 900 1200 DEG C；Solid powder material is placed in zirconium ball grinder, is dried after the ball milling that adds water, compressing, and 1100-1500 DEG C sinter 5 hours, must be substantially free of the negative temperature coefficient heat-sensitive resistance material of Fe, Co, Ni constituent content.Fe, Co, Ni content are extremely low in material prepared by the present invention, solve the problem of existing negative temperature coefficient heat-sensitive resistance material easily magnetizes and has higher magnetic conductivity, the content of gained negative temperature coefficient heat-sensitive resistance material Fe, Co, Ni element is less than 0.005%, magnetic conductivity is close to 1, not easy magnetization and not magnetic conduction, available for the electronic circuit protective element for making noiseproof feature.

Description

A kind of preparation method of negative temperature coefficient heat-sensitive resistance material
Technical field
The present invention relates to negative temperature coefficient heat-sensitive resistance material field, and in particular to is substantially free of Fe, Co, Mn elements it is negative Temperature coefficient thermistor material and preparation method thereof.
Background technology
Into the new century, with the fast development in the fields such as national defence, communication, especially in recent years, to national defence equipment, terminal is led to Interrogate the requirement more and more higher of the electromagnetism antijamming capability of equipment.These requirements, give layout of light current circuit etc. and bring pole Big challenge, big capacitive reactance induction reactance may be impacted to the reliability of communication.Particularly in national defence, by increasing space Capacitive reactance and sense anti-disturbance method are reduced, but so adds the volume of military equipment and the chance of exposure.In the case, it is high The development of the component of the low induction reactance of the low capacitive reactance of reliability is more and more urgent.
Traditional thermistor material is typically made up of the oxide of transition elements manganese cobalt nickel and iron, for example： CN103208340B discloses a kind of manufacture method of power-type negative temperature coefficient thermistor, comprises the following steps：Allotment Thermal sensitive ceramics powder, makes cobaltosic oxide in the thermal sensitive ceramics powder:Manganese dioxide:Nickel oxide:Mole of alundum (Al2O3) Than for 30~60%:40~70%:10~30%:5~20%；By deployed thermal sensitive ceramics powder and adhesive, solvent, increasing Agent, dispersant are moulded, and wears into slurry, wherein, described adhesive is polyvinyl butyral resin, and the solvent is acetic acid The mixture of positive third fat and isobutanol, the plasticizer is o-phthalic acid dibutyl ester, and the dispersant is the formicester of ethanedioic acid two； It is cast the slurry to be allowed to be shaped to film strips, the blank diaphragm of size needed for film strips are cut out；Electrode in being printed on blank film band Thermistor diaphragm is made；Multi-disc blank diaphragm is first stacked, multi-disc thermistor diaphragm, then stacked multi-disc blank film is then stacked Piece, blank diaphragm and thermistor diaphragm after being stacked constitute thermistor green compact；Multiple thermistor monomers are cut into, are arranged Sintered after glue；Two ends upper end electrode.
It is well known that due to the element electronic configuration reason of iron-cobalt-nickel, the magnetic characteristic of this several element is particularly pertinent, contains The thermistor material of these elements easily magnetizes and has higher magnetic conductivity.Material without iron-cobalt-nickel element can just be eliminated This kind of influence, but such material research both at home and abroad at present is seldom.The LaMnO3 of perovskite structure without iron-cobalt-nickel resistance is born Temperature characterisitic, can be by Al, and Mn content adjusts the resistance and B values of material, to reach final use requirement.
The content of the invention
The purpose of the present invention is to be directed to above-mentioned present situation, it is desirable to provide one kind is practically free of Fe, and Co, Ni elements, magnetic conductivity connects Nearly 1, the not preparation method of easy magnetization and non-magnetic negative temperature coefficient heat-sensitive resistance material.
The implementation of the object of the invention is, a kind of preparation method of negative temperature coefficient heat-sensitive resistance material, specific steps It is as follows：
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 5~50, MnCO3Rubbed for 55~110 You are placed in zirconium ball ball grinder ratio, by raw material：Zirconium ball：Water weight ratio is 1:3:2 ratio adds zirconium ball, water, and ball milling 8 hours must be starched Material；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder obtains in 2-8 hours in 900-1200 DEG C of calcining Material；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, by solid powder material：Zirconium ball： Water is 1:3:1.5 weight ratio adds zirconium ball, water, ball milling 8 hours, after under the conditions of 200 DEG C, dry 24h, it is compressing；Exist again 1100-1500 DEG C sinter 5 hours, can arrive negative temperature coefficient heat-sensitive resistance material
The present invention uses La2O3、MnCO3、Al2O3For raw material, raw material is through zirconium ball ball milling, drying, and 900-1200 DEG C is calcined, then Ball milling, drying, sintering, obtains being substantially free of the negative temperature coefficient heat-sensitive resistance material of Fe, Co, Ni element.Because Fe in material, Co, Ni content are less than 0.005%, and it is more to solve traditional thermistor based material containing Fe, Co, Ni, easily magnetize and have compared with The problem of high magnetic conductivity, gained negative tempperature coefficient thermistor material material not easy magnetization, magnetic conductivity is close to 1, not magnetic conduction, and then Solve in light current circuit because of electromagnetic interference problem caused by NTC thermistor magnetization.
Embodiment
The present invention uses La2O3、MnCO3、Al2O3For raw material, raw material is through zirconium ball ball milling, drying, and 900-1200 DEG C is calcined, then Ball milling, drying, sintering, obtains being practically free of the negative temperature coefficient heat-sensitive resistance material of Fe, Co, Ni element.
The present invention is controlled by the content to Al, Mn, to adjust perovskite structure.With resistance negative temperature coefficient LaMnO3Parameter, by La2O3For 100, Al2O3For 5~50, MnCO3For 55~110 mol ratio, work as Al2O3Exceed with MnCO3 During lower range, it is impossible to the perovskite structure stablized and NTC characteristics are weak, do not possess practicality；Work as Al2O3Exceed with MnCO3 During upper range, it is impossible to the perovskite structure stablized, and NTC characteristics are weak, resistivity is too high, do not possess practicality equally.
The present invention is described in detail with specific embodiment below：
Embodiment 1,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 5, MnCO3It is placed in for 100 mol ratio In zirconium ball ball grinder, by weight material：Zirconium ball：Water is 1:3:2 ratio, ball milling 8 hours, obtains slurry；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 6 hours in 1000 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder ball milling 8 hours, after 200 DEG C baking It is dry 24 hours, it is compressing, then sintered 5 hours at 1100 DEG C, it can obtain being practically free of the negative temperature coefficient of Fe, Co, Ni element Thermistor material.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 1.1 Ω cm, B25/50 1587K.
Embodiment 2, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 5, MnCO3It is placed in for 110 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 8 hours in 900 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1200 DEG C sinter 5 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 18 Ω cm, B25/50 2212K.
Embodiment 3, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 25, MnCO3It is placed in for 80 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 2 hours in 1200 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1500 DEG C sinter 5 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 23 Ω cm, B25/50 2311K.
Embodiment 4, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 25, MnCO3Put for 110 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 5 hours in 1100 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1300 DEG C sinter 4 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 78 Ω cm, B25/50 2587K.
Embodiment 5, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 50, MnCO3It is placed in for 55 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 6 hours in 900 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1000 DEG C sinter 5 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 55 Ω cm, B25/50 2492K.
Embodiment 6, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 50, MnCO3It is placed in for 70 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 4 hours in 1000 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1300 DEG C sinter 5 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 1301 Ω cm, B25/50 3315K.
Embodiment 7, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 50, MnCO3It is placed in for 90 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 4 hours in 1100 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1200 DEG C sinter 5 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 8087 Ω cm, B25/50 3782K.
Embodiment 8, be the same as Example 1, unlike,
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 50, MnCO3Put for 110 mol ratio In zirconium ball ball grinder；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 6 hours in 1000 DEG C of calcinings；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, expect by weight：Zirconium ball：Water is 1: 3:1.5 ball millings 8 hours, after 200 DEG C drying, it is compressing 1400 DEG C sinter 5 hours.
Gained negative temperature coefficient heat-sensitive resistance material resistivity 28702 Ω cm, B25/50 4050K.
From the resistivity of above-described embodiment:Fe, Co, Ni constituent content are obtained obtained by of the invention and is less than 0.005% Negative temperature coefficient heat-sensitive resistance material, its magnetic conductivity is close to 1, resistivity 1.1~28702 Ω cm, B25/50：1587~ 4050(K)。

Claims (2)

1. a kind of preparation method of negative temperature coefficient heat-sensitive resistance material, it is characterised in that：
1) with La2O3、MnCO3、Al2O3For raw material, by La2O3For 100, Al2O3For 5~50, MnCO3For 55~110 mol ratio It is placed in zirconium ball ball grinder, by raw material：Zirconium ball：Water weight ratio is 1:3:2 ratio adds zirconium ball, water, and ball milling 8 hours obtains slurry；
2) will be through step 1) slurry of ball milling, in 200 DEG C of drying, solid powder material obtains in 2-8 hours in 900-1200 DEG C of calcining Material；
3) by through step 2) calcining after solid powder material be replaced in zirconium ball grinder, by solid powder material：Zirconium ball：Water is 1:3:1.5 weight ratio adds zirconium ball, water, ball milling 8 hours, after under the conditions of 200 DEG C, dry 24h, it is compressing；Exist again 1100-1500 DEG C sinter 5 hours, obtain negative temperature coefficient heat-sensitive resistance material.
2. a kind of preparation method of negative temperature coefficient heat-sensitive resistance material according to claim 1, it is characterised in that：Gained To the content of negative temperature coefficient heat-sensitive resistance material Fe, Co, Ni element is less than 0.005%, magnetic conductivity is close to 1.
CN201710353229.7A 2017-05-18 2017-05-18 A kind of preparation method of negative temperature coefficient heat-sensitive resistance material Pending CN107140982A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110218087A (en) * 2019-07-05 2019-09-10 威海市科博乐汽车电子有限公司 The preparation method of negative temperature coefficient heat-sensitive resistance material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1348192A (en) * 2000-10-11 2002-05-08 株式会社村田制作所 Semiconductor ceramic with negative resistance temperature coefficient and negative temperature coefficient thermistor
US20090165289A1 (en) * 2007-12-26 2009-07-02 Deng Wen-How Method for fabricating negative temperature coefficient thermistor
CN102627458A (en) * 2012-05-04 2012-08-08 中国科学院新疆理化技术研究所 Wide-warm-area negative temperature coefficient thermistor material
CN103121837A (en) * 2013-03-20 2013-05-29 中国科学院新疆理化技术研究所 Aluminium-doped perovskite phase negative temperature coefficient thermal sensitive ceramic material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1348192A (en) * 2000-10-11 2002-05-08 株式会社村田制作所 Semiconductor ceramic with negative resistance temperature coefficient and negative temperature coefficient thermistor
US20090165289A1 (en) * 2007-12-26 2009-07-02 Deng Wen-How Method for fabricating negative temperature coefficient thermistor
CN102627458A (en) * 2012-05-04 2012-08-08 中国科学院新疆理化技术研究所 Wide-warm-area negative temperature coefficient thermistor material
CN103121837A (en) * 2013-03-20 2013-05-29 中国科学院新疆理化技术研究所 Aluminium-doped perovskite phase negative temperature coefficient thermal sensitive ceramic material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110218087A (en) * 2019-07-05 2019-09-10 威海市科博乐汽车电子有限公司 The preparation method of negative temperature coefficient heat-sensitive resistance material
CN110218087B (en) * 2019-07-05 2021-12-07 威海市科博乐汽车电子有限公司 Preparation method of negative temperature coefficient thermistor material

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Application publication date: 20170908