CN108288529A - Preparation method of negative low-aging-rate negative temperature coefficient thermistor ceramic material - Google Patents
Preparation method of negative low-aging-rate negative temperature coefficient thermistor ceramic material Download PDFInfo
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- CN108288529A CN108288529A CN201810052930.XA CN201810052930A CN108288529A CN 108288529 A CN108288529 A CN 108288529A CN 201810052930 A CN201810052930 A CN 201810052930A CN 108288529 A CN108288529 A CN 108288529A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 230000032683 aging Effects 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- 150000001768 cations Chemical class 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 239000011230 binding agent Substances 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 229910052718 tin Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 238000005469 granulation Methods 0.000 claims abstract 2
- 230000003179 granulation Effects 0.000 claims abstract 2
- 238000000465 moulding Methods 0.000 claims abstract 2
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 239000007858 starting material Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003979 granulating agent Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 claims 1
- 238000001764 infiltration Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract 3
- 239000000463 material Substances 0.000 description 11
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 description 5
- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910016897 MnNi Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- 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
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Abstract
The invention discloses a preparation method of a negative low-aging-rate negative temperature coefficient thermistor ceramic material, wherein the nominal chemical composition of the thermistor ceramic material is Mn3-x-y-zNixFeyMzO4, and M represents Cu, Ti, Sn and Al; the method is characterized in that oxides forming cations are used as initial raw materials, the raw materials are subjected to ball milling, multiple times of calcination are carried out, organic binders are added for granulation and molding, the raw materials are fired to form the sheet sample, silver electrodes are arranged on two end faces of the sheet sample after the sheet sample is fired, and after the electrodes are fired and infiltrated, the cylindrical surface of the sample without the electrodes is sealed by medium-temperature glass glaze in an oxygen-enriched environment. The thermistor ceramic material prepared by the preparation process has the resistivity of 3-1000 omega-m at 25 ℃, the B value of 3000-4000K at a temperature region of 25-85 ℃ and the one-week aging rate of-3.0-0.1% at 150 ℃.
Description
Technical field
The present invention relates to the preparation fields of negative temperature coefficient thermal-sensitive ceramic material, especially a kind of to bear low ageing rate negative temperature
The preparation method of coefficient thermal resistor ceramic material.
Background technology
Negative temperature coefficient (NTC) thermal sensitive ceramics is mainly used in thermometric, temperature-compensating and inhibits surge current.NTC at present
Thermal sensitive ceramics main problem is stability problem, i.e. problem of aging.The aging of General N TC thermal sensitive ceramicses is with the time used
Extend, resistance value becomes larger.Chinese patent focuses mostly on about the research and development of NTC thermal sensitive ceramicses and is forming variation by material at present
The resistance value or B values of controlled material, as Chinese patent (CN200910060128.6, CN200710172253.7,
CN200710113771.1, CN200710113773.0, CN201210182425.X) to disclose a kind of high B values of low-resistivity negative
Temperature coefficient thermistor material and preparation method；Chinese patent (CN201210181462.9, CN200910013605.3,
CN200910113608.4, CN 201010131358.X) disclose a kind of high resistivity and low B value negative tempperature coefficient thermistor
Material and preparation method.Above NTC thermal sensitive ceramic material of the invention with p-type conductance is under the conditions of normal ageing, material resistance value
Become larger at any time.
Present invention is generally directed to MnNiFeO4The temperature sensitive ceramic material of base p-type, at preparation method appropriate and sealing-in heat
Science and engineering skill, which obtains, bears low ageing rate negative temperature coefficient thermistor ceramic material.General preparation method, it is normal pressure-sintered to be obtained
MnNiFeO4Thermal sensitive ceramics resistivity at room temperature is in 80-500 Ω m, B values in 3000-4000K, and ageing rate Δ ρ/ρ is in 2-5%.
Invention content
The purpose of the present invention is to provide a kind of preparations for bearing low ageing rate negative temperature coefficient thermistor ceramic material
Method.
Above-mentioned purpose is realized by following scheme：
A kind of preparation method for bearing low ageing rate negative temperature coefficient thermistor ceramic material, thermal resistor ceramics
The nominal chemical composition of material is Mn3-x-y-zNixFeyMzO4, and M represents Cu, Ti, Sn, Al, x:0.9-1.1；y:0.9-1.1；
z:0.03-0.1；It is to be milled to certain fineness to form the oxide of cation as starting material, by repeatedly calcining, add
It is fired under certain temperature system after certain organic binder granulating and forming, after being burnt into sheet sample, silver electricity in both ends of the surface
Pole after burning electrode, covers at electrodeless place at cylinder with medium temperature glass glaze sealing-in under oxygen-enriched environment.
The preparation method for bearing low ageing rate negative temperature coefficient thermistor ceramic material, includes the following steps：
(1) it using the oxide for forming cation as starting material, using alcohol as abrasive media, is milled under 300 mesh sieve, obtains
Powder drying after ball milling is for use；
(2) powder after gained ball milling is 800-900 DEG C through being sintered into phase, first time calcination temperature twice, soaking time
4-6 hours；Second of calcination temperature is 950-1050 DEG C, soaking time 4-6 hours, every time through dry ball milling to 300 after calcining
Under mesh sieve；
(3) it is granulated to being sintered into the ceramic powder after phase, the use of solid content is the water-soluble of 3-10wt%PVA or CMC
Liquid is granulating agent, and granulating agent dosage is 2-6wt%；
(4) dry-pressing formed, pressure 150-250MPa after being granulated；
(5) using atmospheric air atmosphere, the temperature schedule of sintering is the sintering processing of dry-pressing formed rear green body：With per minute
1-1.5 DEG C is raised to 300 DEG C, keeps the temperature 1 hour；800 DEG C are raised to 2-3 DEG C per minute later, keeps the temperature 1 hour；Later with per minute
3-4 DEG C is raised to 1240-1280 DEG C, keeps the temperature 4-6 hours；850 DEG C are dropped to 1 DEG C per minute later, then is dropped with 10-20 DEG C per minute
To room temperature；
(6) electrode is burnt：Sintered sheets sample brushes 850 DEG C of silver pastes, is raised to 850 DEG C with 2-3 DEG C per minute, keeps the temperature 0.5 hour, then
Room temperature is dropped to 10-20 DEG C per minute；
(7) thermal resistor sealing-in：In atmosphere furnace, it will be sealed with medium temperature glass glaze at electrodeless covering under oxygen-enriched environment
It connects.
Wherein, described in step (7) under oxygen-enriched environment by the cylinder of electrodeless covering with cryogenic glass glaze sealing-in,
In glass-glazed firing temperature at 620-680 DEG C；Oxygen-enriched environment is：Oxygen content 22-40%vol.
The preparation method for bearing low ageing rate negative temperature coefficient thermistor ceramic material, design principle are：Institute
The thermal resistor ceramic material of preparation can make the crystal boundary of sample and phase boundary director's time be in oxygen-enriched by the oxygen-enriched sealing-in of medium temperature
Acceptor state, then its can balance grain boundary acceptor state in application process to the resistance variations caused by micropore diffusion.
Beneficial effects of the present invention are：
The present invention is by the Mn3-x-y-zNixFeyMzO4 systems thermal sensitive ceramics prepared by the preparation process, by oxygen-enriched
Sealing-in obtains the thermal resistor material for bearing low ageing rate negative temperature coefficient；The material obtained is 3- in 25 DEG C of resistivity
The B values of 1000 Ω m, 25-85 DEG C of warm area are 3000-4000K, and 150 DEG C of one week ageing rates are -3.0~-0.1%.
Specific implementation mode
Embodiment 1：Name group becomes Mn0.97NiFeSn0.03O4(x=1, y=1, z=0.03) bears low ageing rate negative temperature
The preparation of coefficient thermal resistor ceramic material:
1, quality formula：With MnO2、Ni2O3、Fe2O3、SnO2For starting material, Mn is calculated0.97NiFeSn0.03O4Batch
Quality formula be：
MnO2：Ni2O3：Fe2O3:SnO2=33.53%:32.89%：31.78%:1.80%；
2, ball milling：With material：Alcohol：Ball=1:0.8:1.8 ratio wet ball grindings 10 hours, after crossing 300 mesh sieve, drying waits for
With；
3, it calcines twice：First time calcination temperature is 850 DEG C, and soaking time 6 hours is taken out after cooling, with material：Ball=1:
300 mesh sieve is crossed after 1.4 dry ball millings 3 hours waits for second of calcining；Second of calcination temperature is 950 DEG C, soaking time 6 hours,
It is taken out after cooling, with material：Ball=1:1.4 dry ball millings 3 hours are crossed after 300 mesh sieve for use；
4, it is granulated：By powder quality than 5wt%, be added a concentration of 10wt%PVA aqueous solutions, be granulated by hand, cross 180 mesh
Sieve；
5, it is molded：It is molded with uniaxial tension, briquetting pressure 300MPa, the piece sample of Φ 8mm × (1.5~2.5) mm is made；
6, it is burnt into：It seems in resistance furnace that piece sample blanks body, which is put into Elema, and sintering temperature curve is as follows：
- 300 DEG C of room temperature, 1.5 DEG C/min of heating rate；
300 DEG C -300 DEG C, keep the temperature 60min；
300 DEG C -800 DEG C, 2.5 DEG C/min of heating rate；
800 DEG C -800 DEG C, keep the temperature 60min
800 DEG C -1250 DEG C, 4 DEG C/min of heating rate；
1250 DEG C -1250 DEG C, keep the temperature 300min；
1250 DEG C -800 DEG C, 1 DEG C/min of rate of temperature fall minute；
800 DEG C-room temperature, 10 DEG C/min of rate of temperature fall minute.
7, silver ink firing：Firing temperature is used to coat the two sides of tile for 850 DEG C of silver paste, silver ink firing soaking time is 30min.
8, sealing-in：In atmosphere furnace by electrodeless covering cylinder with cryogenic glass glaze sealing-in, oxygen content
30%vol, 650 DEG C of sealing temperature.
9, electric performance test：Sample is placed in 25 ± 0.1 DEG C and 85 ± 0.1 DEG C of constant temperature oil baths and measures its resistance value, is counted
Calculate resistivity, B values, 150 DEG C of one week ageing rate Δ ρ/ρ25℃, sample tests such as table 1：
1 Mn of table0.97NiFeSn0.03O4Sample tests
Embodiment 2：Name group becomes MnNiFe0.94Cu0.06O4(x=1, y=0.94, z=0.06) bears low ageing rate subzero temperature
Spend the preparation of coefficient thermal resistor ceramic material：
1, the quality formula of the present embodiment thermal resistor ceramic material batch：
MnO2：Ni2O3：Fe2O3：CuO=34.84%:33.15%：30.11%：1.90%；
2, the identical techniques of 2-9 in embodiment 1 are pressed, the oxygen content for only changing the step sealing-in in 8 is 22%vol, sealing-in
Temperature is 620 DEG C, remaining process is all identical, prepared sample tests such as the following table 2.
2 MnNiFe of table0.94Cu0.06O44Sample tests
Embodiment 3：Name group becomes Mn0.97NiFe0.94Ti0.09O4(x=1, y=0.94, z=0.09) bears low ageing rate
The preparation of negative temperature coefficient thermistor ceramic material：
1, the formula of the present embodiment thermal resistor ceramic material batch：
MnO2：Ni2O3：Fe2O3：TiO2=33.51%:31.88%：30.78%：3.83%.
2, the identical techniques of 2-8 in embodiment 1 are pressed, by the identical techniques of 2-9 in embodiment 1 are implemented, are only changed the step in 8
The oxygen content of sealing-in is 40%vol, and sealing temperature is 640 DEG C, remaining process is all identical, sample tests such as following table
3：
3 Mn of table0.97NiFe0.94Ti0.09O4Sample tests
Embodiment 4：Name group becomes MnNi0.97FeAl0.03O4(x=0.97, y=1, z=0.03) bears low ageing rate subzero temperature
Spend the preparation of coefficient thermal resistor ceramic material：
1, the formula of the present embodiment thermal resistor ceramic material batch：
MnO2：Ni2O3：Fe2O3：Al2O3=30.10%:28.64%：27.65%：13.61%.
2, the identical techniques of 2-8 in embodiment 1 are pressed, by the identical techniques of 2-9 in embodiment 1 are implemented, are only changed the step in 8
The oxygen content of sealing-in is 25%vol, and sealing temperature is 680 DEG C, remaining process is all identical, sample tests such as following table
4：
4 MnNi of table0.97FeAl0.03O4Sample tests
Claims (4)
1. it is a kind of bear low ageing rate negative temperature coefficient thermistor ceramic material preparation method, which is characterized in that its be with
The oxide of composition cation is starting material, is milled to certain fineness, by repeatedly calcining, certain organic binder is added to be granulated
It is fired under certain temperature system after molding, after being burnt into sheet sample, silver electrode in both ends of the surface, after electrode burning infiltration, in richness
Under oxygen environment by the cylinder of electrodeless covering with medium temperature glass glaze sealing-in.
2. a kind of preparation side bearing low ageing rate negative temperature coefficient thermistor ceramic material according to claim 1
Method, which is characterized in that the chemical composition of the thermal resistor ceramic material is Mn3-x-y-zNixFeyMzO4, and wherein M is represented
Cu, Ti, Sn, Al, x:0.9-1.1, y:0.9-1.1, z:0.03-0.1.
3. a kind of preparation side bearing low ageing rate negative temperature coefficient thermistor ceramic material according to claim 1
Method, which is characterized in that include the following steps：
（1）Using the oxide for forming cation as starting material, using alcohol as abrasive media, it is milled under 300 mesh sieve, obtains ball milling
Powder drying afterwards is for use；
（2）Powder after gained ball milling is 800-900 DEG C through being sintered into phase, first time calcination temperature twice, and soaking time 4-6 is small
When；Second of calcination temperature is 950-1050 DEG C, soaking time 4-6 hours, is sieved every time through dry ball milling to 300 mesh after calcining
Under；
（3）It is granulated to being sintered into the ceramic powder after phase, using solid content be 3-10wt%PVA or the aqueous solution of CMC is to make
Granula, granulating agent dosage are 2-6wt%；
（4）It is dry-pressing formed after granulation, pressure 150-250MPa；
（5）The sintering processing of green body is using atmospheric air atmosphere, the temperature schedule of sintering after dry-pressing formed：With 1- per minute
1.5 DEG C are raised to 300 DEG C, keep the temperature 1 hour；800 DEG C are raised to 2-3 DEG C per minute later, keeps the temperature 1 hour；Later with 3-4 per minute
It DEG C is raised to 1240-1280 DEG C, keeps the temperature 4-6 hours；850 DEG C are dropped to 1 DEG C per minute later, then is dropped to 10-20 DEG C per minute
Room temperature；
（6）Burn electrode：Sintered sheets sample brushes 850 DEG C of silver pastes, is raised to 850 DEG C with 2-3 DEG C per minute, keeps the temperature 0.5 hour, then with every
10-20 DEG C of minute drops to room temperature；
（7）Thermal resistor sealing-in：In atmosphere furnace, under oxygen-enriched environment by electrodeless covering with medium temperature glass glaze sealing-in.
4. a kind of preparation method for bearing low ageing rate negative temperature coefficient thermistor ceramic material according to claim 3,
It is characterized in that, step（7）It is described to cover at electrodeless place at cylinder with cryogenic glass glaze sealing-in under oxygen-enriched environment, wherein
Glass-glazed firing temperature is at 620-680 DEG C；Oxygen-enriched environment is：Oxygen content 22-40%vol.
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| CN201196910Y (en) * | 2008-05-29 | 2009-02-18 | 成都宏明电子股份有限公司 | Packaging body used for sheet-type multilayer ceramic capacitor and sheet-type multi-layer piezoresistor |
| US7992285B2 (en) * | 2007-12-26 | 2011-08-09 | Industrial Technology Research Institute | Method for fabricating negative temperature coefficient thermistor |
| CN102674826A (en) * | 2012-06-05 | 2012-09-19 | 安徽建筑工业学院 | Low-resistivity high-B-value negative temperature coefficient heat-sensitive ceramic material and preparation process thereof |
| CN103632781A (en) * | 2013-12-13 | 2014-03-12 | 深圳顺络电子股份有限公司 | Chip component tip packaging paste and preparation method of chip component |
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|---|---|---|---|---|
| US7992285B2 (en) * | 2007-12-26 | 2011-08-09 | Industrial Technology Research Institute | Method for fabricating negative temperature coefficient thermistor |
| CN201196910Y (en) * | 2008-05-29 | 2009-02-18 | 成都宏明电子股份有限公司 | Packaging body used for sheet-type multilayer ceramic capacitor and sheet-type multi-layer piezoresistor |
| CN102674826A (en) * | 2012-06-05 | 2012-09-19 | 安徽建筑工业学院 | Low-resistivity high-B-value negative temperature coefficient heat-sensitive ceramic material and preparation process thereof |
| CN103632781A (en) * | 2013-12-13 | 2014-03-12 | 深圳顺络电子股份有限公司 | Chip component tip packaging paste and preparation method of chip component |
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