CN106278226A - A kind of preparation method of ternary system negative temperature coefficient heat-sensitive resistance material - Google Patents

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

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Publication number
CN106278226A
CN106278226A CN201610677632.0A CN201610677632A CN106278226A CN 106278226 A CN106278226 A CN 106278226A CN 201610677632 A CN201610677632 A CN 201610677632A CN 106278226 A CN106278226 A CN 106278226A
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temperature
resistance
ternary system
temperature coefficient
system negative
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姚金城
刘旭
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26Shaped 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 ferrites
    • C04B35/265Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-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
    • H01C7/04Non-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
    • H01C7/042Non-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
    • H01C7/043Oxides or oxidic compounds

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Inorganic Chemistry (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
  • Thermistors And Varistors (AREA)

Abstract

The present invention relates to the preparation method of a kind of ternary system negative temperature coefficient heat-sensitive resistance material, the method is by Co, Mn, the oxide composition of tri-kinds of metallic elements of Fe, prepare through wet ball grinding, pre-burning, molding, the techniques such as sintering obtain high stable ternary system negative temperature coefficient heat-sensitive resistance material, the performance parameter of the ternary system negative temperature coefficient heat-sensitive resistance material obtained by the method for the invention be measuring resistance (25 DEG C of resistance) be 1,002 1797 Ω, material constant is 3671K 3994 K, at temperature 150 DEG C after aging 500 h, resistance fluctuating is 0.16 0.19 %.There is preferable stability, concordance and interchangeability, can be widely applied to the occasions such as temperature survey, temperature-compensating, surge current suppression.

Description

A kind of preparation method of ternary system negative temperature coefficient heat-sensitive resistance material
Technical field
The present invention relates to the preparation method of a kind of electronic devices and components, be specifically related to a kind of high stability ternary system negative temperature system The preparation method of number thermistor material.
Background technology:
Negative temperature coefficient (NTC) critesistor is widely used in various industry and domestic environments, for surge current suppression, Carry out temperature survey and temperature controls and to other loop compensations, and because it has high sensitivity, high stability, low cost etc. Feature is widely used.In recent years, due to the demand of the electrical appliance industries such as air-conditioning, electric refrigerator, microwave oven, to NTC temperature-sensitive on market The requirement of the indexs such as the stability of resistor, precision improves day by day.
In actual use, the resistance value of NTC thermistor can be affected by external environment and be occurred certain Drift, deviates initial resistivity value.The drift of this resistance value, can directly influence NTC thermistor use accuracy with make Use the life-span.So, prepare the research emphasis that the NTC thermistor that resistance fluctuating is little, stability is high is relevant staff And difficult point.
Negative tempperature coefficient thermistor, with 3d transiting group metal elements as key component, as manganese, copper, cobalt, ferrum, nickel, Zinc etc..According to composition of raw materials wherein containing two or more metal-oxide mixing.Material group on general industry Architectonical has binary system material Ni-Mn-O system, and Cu-Mn-O system etc., ternary system thermal sensitive ceramic material mainly has Mn-Ni-Co- O system, Mn-Ni-Cu-O system, Mn-Ni-Fe-O system, Mn-Ni-Zn-O system etc., broadly fall into Mn-Ni base critesistor material Material, but the use of Co-Mn sill but rarely has report.Different materials system has different resistivity and material constant, tool There is different applications.So developing good stability, the Co-Mn base NTC thermistor with practical value can be supplemented The deficiency of other material system, significant.
Summary of the invention:
The preparation method of the present invention a kind of ternary system negative temperature coefficient heat-sensitive resistance material, the method is by Co, Mn, Fe tri- The oxide composition of kind of metallic element, prepares through wet ball grinding, pre-burning, molding, the technique such as sintering obtain high stable ternary system and bears Temperature coefficient thermistor material, by the property of the ternary system negative temperature coefficient heat-sensitive resistance material that the method for the invention obtains Can parameter be measuring resistance (25 DEG C of resistance) be 1002-1797 Ω, material constant is 3671K-3994K, old at temperature 150 DEG C After changing 500h, resistance fluctuating is less than 0.2%.There is preferable stability, concordance and interchangeability, can be widely applied to temperature The occasions such as degree measurement, temperature-compensating, surge current suppression.
A kind of ternary system negative temperature coefficient heat-sensitive resistance material preparation method of the present invention, follows these steps to carry out:
A, in molar ratio Co: Mn: Fe=0.8-2.0: 0.8-1.3: 0.2-0.9 weigh Co2O3、MnO2、Fe2O3Three kinds of oxidations Thing powder mix homogeneously, then oxide powder, deionized water and the dehydrated alcohol in mass ratio 4: 1: 1: 1 by agate ball, weighed Carrying out batch mixing, put into planetary ball mill high-energy ball milling, the time is 8-24h, then by powder good for ball milling in temperature 50-100 DEG C dry 6-12h, grind the 200-300 mesh that sieves and become powder body;
B, the powder body sieved in step a being sequentially passed through calcining, temperature is 700-1000 DEG C, and temperature retention time is 1-4h, pressure Sheet molding, isostatic cool pressing, pressure is 100-400MPa, and the dwell time is 1-5min, sintering, and temperature is 1100-1300 DEG C, insulation Time is 1-4h, electrode coated, put solder taul, i.e. obtain performance parameter be 25 DEG C of resistance of measuring resistance be 1002-1797 Ω, material Material constant is 3671K-3994K, and at temperature 150 DEG C after aging 500h, resistance fluctuating is the high stability ternary of 0.16-19% Series negative temperature coefficient thermistor material.
Detailed description of the invention
Embodiment 1
A, weigh Co for 0.8:1.3:0.9 in molar ratio2O3、MnO2、Fe2O3Three kinds of oxide powder mix homogeneously, then will Agate ball, the oxide powder weighed, deionized water and dehydrated alcohol carry out batch mixing for 4:1:1:1 in mass ratio, put into planet Formula ball mill high energy ball grinds 8h, and then powder good for ball milling dries at temperature 100 DEG C 6h, grinds 200 mesh that sieve and becomes powder Body;
B, the powder body that sieves in step a is calcined 1h, compression molding, isostatic cool pressing under 400MPa temperature 1000 DEG C 1min, temperature 1300 DEG C sintering 1h, electrode coated, put solder taul, i.e. obtaining performance parameter is that measuring resistance (25 DEG C of resistance) is 1002 Ω, material constant is 3671K, at temperature 150 DEG C after aging 500h, the high stability of resistance fluctuating average out to 0.18% Ternary system negative temperature coefficient heat-sensitive resistance material.
Embodiment 2
A, weigh Co for 2.0:0.8:0.2 in molar ratio2O3、MnO2、Fe2O3Three kinds of oxide powder mix homogeneously, then will Agate ball, the oxide powder weighed, deionized water and dehydrated alcohol carry out batch mixing for 4:1:1:1 in mass ratio, put into planet Formula ball mill high energy ball grinds 24h, and then powder good for ball milling dries under temperature 50 C 12h, grinds 250 mesh that sieve and becomes powder Body;
B, the powder body that sieves in step a is calcined 4h temperature 700 DEG C, compression molding, isostatic cool pressing 5min under 100MPa, Temperature 1100 DEG C sintering 4h, electrode coated, put solder taul, i.e. obtain performance parameter be measuring resistance (25 DEG C of resistance) be 1797 Ω, material constant is 3994K, at temperature 150 DEG C after aging 500h, the high stability ternary of resistance fluctuating average out to 0.19% Series negative temperature coefficient thermistor material.
Embodiment 3
A, weigh Co for 1.4:1.05:0.55 in molar ratio2O3、MnO2、Fe2O3Three kinds of oxide powder mix homogeneously, then The oxide powder, deionized water and the dehydrated alcohol that by agate ball, weigh carry out batch mixing for 4:1:1:1 in mass ratio, put into row Planetary ball mill high energy ball grinds 12h, and then powder good for ball milling dries at temperature 80 DEG C 8h, grinds 300 mesh that sieve and becomes Powder body;
B, the powder body that sieves in step a is calcined 3h temperature 900 DEG C, compression molding, isostatic cool pressing 3min under 300MPa, Temperature 1200 DEG C sintering 3h, electrode coated, put solder taul, i.e. obtain performance parameter be measuring resistance (25 DEG C of resistance) be 1453 Ω, material constant is 3721K, the high stability ternary system subzero temperature of the resistance fluctuating average out to 0.16% of 150 DEG C of aging 500h Degree coefficient heat-sensitive resistance material.

Claims (1)

1. the preparation method of a ternary system negative temperature coefficient heat-sensitive resistance material, it is characterised in that follow these steps to carry out:
A, in molar ratio Co: Mn: Fe=0.8-2.0: 0.8-1.3: 0.2-0.9 weigh Co2O3、MnO2、Fe2O3Three kinds of oxidate powders Expect mix homogeneously, then the oxide powder, deionized water and the dehydrated alcohol in mass ratio 4: 1: 1: 1 that by agate ball, weigh are carried out Batch mixing, puts into planetary ball mill high-energy ball milling, and the time is 8-24 h, is then dried in temperature 50-100 DEG C by powder good for ball milling Dry 6-12 h, grinds the 200-300 mesh that sieves and becomes powder body;
B, the powder body sieved in step a being sequentially passed through calcining, temperature is 700-1000 DEG C, and temperature retention time is 1-4 h, tabletting Molding, isostatic cool pressing, pressure is 100-400 MPa, and the dwell time is 1-5 min, sintering, and temperature is 1100-1300 DEG C, protects Temperature the time be 1-4 h, electrode coated, put solder taul, i.e. obtain performance parameter be 25 DEG C of resistance of measuring resistance be 1002-1797 Ω, material constant is 3671 K-3994 K, and at temperature 150 DEG C after aging 500 h, resistance fluctuating is the height of 0.16-0.19% Stability ternary system negative temperature coefficient heat-sensitive resistance material.
CN201610677632.0A 2016-08-17 2016-08-17 A kind of preparation method of ternary system negative temperature coefficient heat-sensitive resistance material Pending CN106278226A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109485402A (en) * 2018-12-14 2019-03-19 中国科学院新疆理化技术研究所 A method of improving manganese ferro-cobalt base thermal sensitive ceramics agglutinating property
CN109516780A (en) * 2018-11-29 2019-03-26 镇江爱豪科思电子科技有限公司 A kind of high-stability negative temperature coefficient heat-sensitive resistance material and preparation method thereof
CN113936858A (en) * 2020-07-13 2022-01-14 广东美的白色家电技术创新中心有限公司 Temperature-sensing resistor paste, preparation method thereof, steam generator and household appliance
CN113979728A (en) * 2021-11-09 2022-01-28 中国科学院新疆理化技术研究所 Preparation method of double perovskite type and yttrium oxide compounded negative temperature coefficient thermistor material

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CN102122552A (en) * 2010-12-08 2011-07-13 深圳顺络电子股份有限公司 Negative temperature coefficient thermal resistor with variable thermosensitive index
CN102775154A (en) * 2012-08-01 2012-11-14 孝感华工高理电子有限公司 Manufacturing method of negative temperature coefficient ceramic thermistor
CN105152644A (en) * 2015-07-10 2015-12-16 明光旭升科技有限公司 NTC thermistor chip material, chip, resistor and sensor, and making methods thereof
CN105622083A (en) * 2014-10-31 2016-06-01 陕西高华知本化工科技有限公司 Preparation method of thermistor

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CN102122552A (en) * 2010-12-08 2011-07-13 深圳顺络电子股份有限公司 Negative temperature coefficient thermal resistor with variable thermosensitive index
CN102775154A (en) * 2012-08-01 2012-11-14 孝感华工高理电子有限公司 Manufacturing method of negative temperature coefficient ceramic thermistor
CN105622083A (en) * 2014-10-31 2016-06-01 陕西高华知本化工科技有限公司 Preparation method of thermistor
CN105152644A (en) * 2015-07-10 2015-12-16 明光旭升科技有限公司 NTC thermistor chip material, chip, resistor and sensor, and making methods thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109516780A (en) * 2018-11-29 2019-03-26 镇江爱豪科思电子科技有限公司 A kind of high-stability negative temperature coefficient heat-sensitive resistance material and preparation method thereof
CN109485402A (en) * 2018-12-14 2019-03-19 中国科学院新疆理化技术研究所 A method of improving manganese ferro-cobalt base thermal sensitive ceramics agglutinating property
CN113936858A (en) * 2020-07-13 2022-01-14 广东美的白色家电技术创新中心有限公司 Temperature-sensing resistor paste, preparation method thereof, steam generator and household appliance
CN113979728A (en) * 2021-11-09 2022-01-28 中国科学院新疆理化技术研究所 Preparation method of double perovskite type and yttrium oxide compounded negative temperature coefficient thermistor material

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