CN102674826A - Low-resistivity high-B-value negative temperature coefficient heat-sensitive ceramic material and preparation process thereof - Google Patents
Low-resistivity high-B-value negative temperature coefficient heat-sensitive ceramic material and preparation process thereof Download PDFInfo
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- CN102674826A CN102674826A CN201210182425XA CN201210182425A CN102674826A CN 102674826 A CN102674826 A CN 102674826A CN 201210182425X A CN201210182425X A CN 201210182425XA CN 201210182425 A CN201210182425 A CN 201210182425A CN 102674826 A CN102674826 A CN 102674826A
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Abstract
The invention discloses a low-resistivity high-B-value negative temperature coefficient heat-sensitive ceramic material and a preparation process thereof. The nominal chemical composition of the heat-sensitive ceramic material is (MnNiFe)1-x/3MxO4, wherein M represents titanium, copper, tin, cobalt and zinc. The process comprises that an oxide which constitutes a positive ion serves as a mixed batch of a starting material is subjected to ball milling to a certain degree of fineness, calcinations is conducted twice, a certain organic binding agent is added for pelleting molding, and then the heat-sensitive ceramic material is produced by firing under a certain negative pressure condition. According to the heat-sensitive ceramic material and the preparation process, titanium ions, copper ions, tin ions, cobalt ions and zinc ions of variable valencies on a high-temperature negative pressure condition are added appropriately on the basis of current conventional MnNiFeO4 series of ceramic materials, and the low-resistivity high-B-value negative temperature coefficient heat-sensitive ceramic material is obtained by a negative pressure sintering method. The resistivity of the obtained material at 25 DEG C is 3-75 omega.m, and the B-value in a temperature range of 25-85 DEG C is 3600-4500K.
Description
Technical field
The present invention relates to NTC thermal sensitive ceramic material and preparation field, especially a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material and preparation method thereof.
Background technology
Low-resistivity high B-value negative temperature coefficient NTC thermal sensitive ceramics belongs to power type thermal resistance, is mainly used in temperature compensation and suppresses surge current.Chinese patent (CN101118793A) discloses a kind of low-resistivity high B-value negative temperature coefficient negative tempperature coefficient thermistor chip, and this patent is through adding TiO
2, Cr
2O
3, Nb
2O
5, WO
3, Pr
6O
11The low-resistivity diaphragm that middle 2-3 kind oxide compound is processed Mn-Ni-Cu system, prepared resistivity of material is in tens Ω m scopes, and the B value is below 3000.Chinese patent (CN101157550A) discloses the high B value of a kind of low-resistance Mn-Ti-Cu system spinel structure thermistor material.It is base material that this material adopts the Mn-Ti-Cu oxide compound, adds the additive that Zn-Ca-Nb forms, and the quality of materials proportioning is MnO
2: TiO
2: CuO=(65-75): (5-15): (10-20), additive quality proportioning is ZnO:CaO:Nb
2O
5=30:60:10.The resistivity of prepared material in the time of 25 ℃ is 20-100 Ω cm, and the B value of 25 ℃ of-50 ℃ of warm areas is 2600-3300K.Chinese patent (CN101618959A) discloses a kind of low-resistivity high B-value negative temperature coefficient negative temperature coefficient thermistor composition.The said material of patent mainly is made up of the Mn-Co-Cu-O oxide compound, and adds Fe
2O
3-C-TiO
2-Cr
2O
3Synthetics, Mn wherein
2O
4: Co
3O
4: CuO: synthetics=(31%-41%): (35%-40%): (19%-26%): (1.5%:5.5%).This thermo-sensitive material is 5-20 Ω cm 25 ℃ resistivity, and the B value is below 3600.It is temperature-sensitive chip stupalith that Chinese patent (publication number CN101183578) discloses the high B value of a kind of low-resistance Co base binary Mn-Co.It is base material that this patent adopts binary Mn-Co oxide compound, so that one or more are additive in silicon, calcium, magnesium, the zirconium.Mn:Co=0.4 ~ 0.9:1 wherein, content of additive is controlled at 0.3 ~ 10%.The resistivity of prepared material is at 300 ~ 500 Ω m, and the B value is at 3800 ~ 4250K.Though this based material is realized the high B value of low-resistance, the cost of Co oxide compound that uses higher.
Chinese patent (CN101123134A) discloses a kind of compound low-resistivity, high B-value negative temperature coefficient thermistor and preparation method thereof.The chip of this element is the composite structure of folder one floor height B value thermal resistor layer between two conductive formations, and conductive formation is made up of Mn-Ni-Cu-Ca, the mol ratio Mn:Ni:Cu:Ca between its element=2.6:1.3:1.8:0.3; High B value layer is that Mn:Co:Cu:Ti:Nb=3.6:1.4:0.6:0.2:0.2 forms by weight percent.Adopt and prick the low resistance diaphragm and the high B value diaphragm that forms high B value layer that membrane technique is processed conductive formation respectively, and the superimposed compound film sheet of processing, NTCR is processed in high-temperature calcination.The prepared resistivity of material of this method can reach a few Ω m, B value 4100K, but preparation technology's relative complex.
With reference to the characteristics and deficiency of above invention technical background, selection of the present invention is the relatively low MnNiFeO of cost
4Series ceramic material.General preparation method, the normal pressure-sintered MnNiFeO that obtains
4The thermal sensitive ceramics resistivity at room temperature is at 80 ~ 500 Ω m, and the B value is at 2800～3300K.
Summary of the invention
The object of the present invention is to provide a kind of at existing conventional MnNiFeO
4Titanium, copper, tin, cobalt, zine ion through suitably being added on variable valence under the high temperature negative pressure state on the basis of series ceramic material, low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material that obtains through the negative pressure sintering processing and preparation method thereof.
Above-mentioned purpose realizes through following scheme:
A kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material is characterized in that: the nominal chemical constitution of this thermal sensitive ceramic material is (MnNiFe)
1-x/3M
xO
4, M represents titanium, copper, tin, cobalt, zinc.
Described a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material, it is characterized in that: the span of described x is 0 ~ 0.24.
Described a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material, it is characterized in that: the optimization range of described x is 0.06 ~ 0.15.
The preparation method of described low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material; It is characterized in that: it is that the metering by chemical constitution is that starting raw material is mixed with admixtion than to form cationic, oxidized thing; With its ball milling to certain fineness; Through twice calcining, add under certain condition of negative pressure, to fire behind certain organic binder bond granulating and forming and form.
The preparation method of said a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material is characterized in that:
(1) be that starting raw material is mixed with admixtion to form cationic, oxidized thing, under water ball milling to 400 mesh sieve, the powder oven dry behind the ball milling is for use;
(2) warp of the powder behind the gained ball milling is sintered into phase twice, and calcining temperature is 800 ~ 900 ℃ for the first time, soaking time 4 ~ 10 hours; Calcining temperature is 950 ~ 1050 ℃ for the second time, soaking time 4 ~ 10 hours; Calcine after under dry ball milling to 400 mesh sieve at every turn;
(3) ceramic powder after being sintered into is mutually carried out granulation, using solid content is that the aqueous solution of 3 ~ 10wt%PVA or CMC is granulating agent, and the granulating agent consumption is 1 ~ 6wt%;
(4) dry-pressing formed after the granulation, pressure is 250MPa ~ 350MPa;
(5) sintering processing of dry-pressing formed back base substrate adopts the air negative pressure mode, and vacuum degree control is at 0.0001MPa ~ 0.08MPa.
The preparation method of said a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material is characterized in that: the described vacuum tightness optimization range of step (5) is at 0.005 ~ 0.06MPa.
Beneficial effect of the present invention is:
The present invention is at existing conventional MnNiFeO
4Titanium, copper, tin, cobalt, zine ion through suitably being added on variable valence under the high temperature negative pressure state on the basis of series ceramic material obtain low-resistivity, high B-value negative temperature coefficient thermal sensitive ceramic material through the negative pressure sintering processing; The material that is obtained is 3-75 Ω m 25 ℃ resistivity, and the B value of 25-85 ℃ of warm area is 3600-4500K.
Embodiment
Embodiment 1: name consists of (MnNiFe)
1-x/3Ti
xO
4Preparation, resistivity and the B value of the thermal sensitive ceramic material of (x=0.0,0.12,0.24) low-resistivity high B-value negative temperature coefficient.
1.Quality prescription: with MnO
2, Ni
2O
3, Fe
2O
3, TiO
2Be starting raw material, get the prescription of the admixtion of three kinds of thermal sensitive ceramic materials.
MnNiFeO
4Prescription: MnO
2: Ni
2O
3: Fe
2O
3=
34.85%:33.15%：32.01%；
(MnNiFe)
0.96Ti
0.12O
4Prescription: MnO
2: Ni
2O
3: Fe
2O
3: TiO
2=
33.51%:31.87%：30.77%：3.85%；
(MnNiFe)
0.92Ti
0.24O
4Prescription: MnO
2: Ni
2O
3: Fe
2O
3: TiO
2=
31.34%:31.11%：30.04%：7.51%；
2.Ball milling: with material: water: ball=1:0.8:1.8 ratio wet ball grinding 10 hours, cross 400 mesh sieves after, dry for use;
3.Twice calcining: calcining temperature is 850 ℃ for the first time, soaking time 6 hours, and take out the cooling back, and to expect: ball=1:1.4 dry ball milling is crossed 400 mesh sieves and is treated calcining for the second time after 6 hours; For the second time calcining temperature is 950 ℃, soaking time 6 hours, and take out the cooling back, with material: ball=1:1.4 dry ball milling 6 hours, cross behind 400 mesh sieves for use;
4.Granulation: press the 5wt% of powder quality ratio, adding concentration is the 10wt%PVA aqueous solution, and 180 mesh sieves are crossed in manual granulation;
5.Moulding: with the uniaxial tension moulding, forming pressure is 300MPa, processes the sheet appearance of Φ 13mm * (1.5 ~ 2.5) mm;
6.Burn till: sheet appearance base substrate is put into the tubular type vacuum oven, and vacuum degree control is 0.01MPa, and sintering temperature curve is following:
Room temperature-600 ℃, 1.5 ℃/min of temperature rise rate;
600 ℃-600 ℃, insulation 60min;
600 ℃-900 ℃, 2 ℃/min of temperature rise rate;
900 ℃-900 ℃, insulation 60min
900 ℃---1280 ℃, 5 ℃/min of temperature rise rate;
1280 ℃---1280 ℃, insulation 300min;
1280 ℃---room temperature is cooled to room temperature with stove;
The apparent density of burning the back ceramics is (5.2 ~ 5.5) g/cm
3
7.Silver ink firing: adopting reduction temperature is the two sides of 850 ℃ silver slurry coating ceramics, and the silver ink firing soaking time is 40min.
8.Electric performance test: place 25 ± 0.1 ℃ and 85 ± 0.1 ℃ of constant temperature oil baths to measure its resistance values in sample, calculated resistance rate, B value as follows:
MnNiFeO
425 ℃ of resistivity of sample and B
25/85Value
(MnNiFe)
0.96Ti
0.12O
425 ℃ of resistivity of sample and B
25/85Value
(MnNiFe)
0.92Ti
0.24O
425 ℃ of resistivity of sample and B
25/85Value
Embodiment 2: different vacuum tightnesss (0.0001MPa, 0.005MPa, 0.06MPa, 0.08MPa) are sintering down, and name consists of (MnNiFe)
0.96Ti
0.12O
4Resistivity and B value.
1. the quality prescription of present embodiment thermal sensitive ceramic material admixtion: MnO
2: Ni
2O
3: Fe
2O
3: TiO
2=
33.51%:31.87%：30.77%：3.85%；
2. by implementing the identical technology of 2-8 among the embodiment 1, only change resistivity and the B Value Data such as the following table of vacuum tightness (0.001MPa, 0.005MPa, 0.06MPa, 0.08MPa) sintered sample.
Embodiment 3: a kind of name consists of (MnNiFe)
0.96Cu
0.12O
4Preparation and resistivity and B value.
1.The prescription of present embodiment thermal sensitive ceramic material admixtion: MnO2:Ni
2O
3: Fe
2O
3: CuO=
33.51%:?31.88%：30.78%：3.83%。
2.Press the identical technology of 2-8 among the embodiment 1, the vacuum sintering temperature changes 1270 ℃ into, and vacuum tightness changes 0.05MPa into, and all the other are all identical.
Sample test result such as following table:
Embodiment 4: a kind of name consists of (MnNiFe)
0.92Sn
0.24O
4Preparation, resistivity and B value.
1. the prescription of present embodiment thermal sensitive ceramic material admixtion: MnO
2: Ni
2O
3: Fe
2O
3: SnO
2=
30.10%:?28.64%：27.65%：13.61%。
2. press the identical technology of 2-8 among the embodiment 1, vacuum tightness changes 0.05MPa into, and all the other are all identical.
Sample test result such as following table:
Embodiment 5: a kind of name consists of (MnNiFe)
0.92Co
0.24O
4Preparation, resistivity and B value.
1. the prescription of present embodiment thermal sensitive ceramic material admixtion: MnO
2: Ni
2O
3: Fe
2O
3: Co
2O
3=
33.00%:?30.08%：29.05%：7.87%。
2. press the identical technology of 2-8 among the embodiment 1, the vacuum sintering temperature changes 1300 into
oC, vacuum tightness is 0.05MPa, all the other are all identical.
Sample test result such as following table:
Embodiment 6: a kind of name consists of (MnNiFe)
0.96Zn
0.12O
4Preparation and resistivity and B value.
1.The prescription of present embodiment thermal sensitive ceramic material admixtion: MnO
2: Ni
2O
3: Fe
2O
3: ZnO=
33.48%:?31.85%：30.75%：3.92%。
2.Press the identical technology of 2-8 among the embodiment 1, the vacuum sintering temperature changes 1270 ℃ into, and vacuum tightness is 0.04MPa, and all the other are all identical.
Sample test result such as following table:
Claims (6)
1. low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material is characterized in that: the nominal chemical constitution of this thermal sensitive ceramic material is (MnNiFe)
1-x/3M
xO
4, M represents titanium, copper, tin, cobalt, zinc.
2. a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material according to claim 1, it is characterized in that: the span of described x is 0 ~ 0.24.
3. a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material according to claim 1, it is characterized in that: the optimization range of described x is 0.06 ~ 0.15.
4. the preparation method of a low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material as claimed in claim 1; It is characterized in that: it is that the metering by chemical constitution is that starting raw material is mixed with admixtion than to form cationic, oxidized thing; With its ball milling to certain fineness; Through twice calcining, add under certain condition of negative pressure, to fire behind certain organic binder bond granulating and forming and form.
5. according to the preparation method of the said a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material of claim 4, it is characterized in that:
(1) be that starting raw material is mixed with admixtion to form cationic, oxidized thing, under water ball milling to 400 mesh sieve, the powder oven dry behind the ball milling is for use;
(2) warp of the powder behind the gained ball milling is sintered into phase twice, and calcining temperature is 800 ~ 900 ℃ for the first time, soaking time 4 ~ 10 hours; Calcining temperature is 950 ~ 1050 ℃ for the second time, soaking time 4 ~ 10 hours; Calcine after under dry ball milling to 400 mesh sieve at every turn;
(3) ceramic powder after being sintered into is mutually carried out granulation, using solid content is that the aqueous solution of 3 ~ 10wt%PVA or CMC is granulating agent, and the granulating agent consumption is 1 ~ 6wt%;
(4) dry-pressing formed after the granulation, pressure is 250MPa ~ 350MPa;
(5) sintering processing of dry-pressing formed back base substrate adopts the air negative pressure mode, and vacuum degree control is at 0.0001MPa ~ 0.08MPa.
6. according to the preparation method of the said a kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material of claim 5, it is characterized in that: the described vacuum tightness optimization range of step (5) is at 0.005 ~ 0.06MPa.
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| CN104193306A (en) * | 2014-08-20 | 2014-12-10 | 华南理工大学 | Thermal sensitive ceramic material with low resistivity, high B value and negative temperature coefficient and preparation method thereof |
| CN105552322A (en) * | 2015-12-13 | 2016-05-04 | 浙江美达瑞新材料科技有限公司 | Quaternary ionic composite-modified positive pole material for lithium-ion battery and preparation method of quaternary ion composite-modified positive pole material |
| CN106211388A (en) * | 2016-07-05 | 2016-12-07 | 安徽吉安特种线缆制造有限公司 | A kind of self limiting temperature cable material of good weatherability |
| CN106699158A (en) * | 2017-01-18 | 2017-05-24 | 广州新莱福磁电有限公司 | Method for manufacturing high-precision NTC thermistor chip |
| CN108288529A (en) * | 2018-01-19 | 2018-07-17 | 安徽建筑大学 | A kind of preparation method for bearing low ageing rate negative temperature coefficient thermistor ceramic material |
| CN109133901A (en) * | 2018-10-29 | 2019-01-04 | 惠州嘉科实业有限公司 | Thermistor containing iron series and preparation method thereof |
| CN112390640A (en) * | 2020-11-13 | 2021-02-23 | 深圳顺络电子股份有限公司 | NTC thermistor and manufacturing 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 |
| CN116283231A (en) * | 2023-01-30 | 2023-06-23 | 广东风华高新科技股份有限公司 | NTC thermistor material and preparation method thereof |
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| CN104193306B (en) * | 2014-08-20 | 2015-12-30 | 华南理工大学 | A kind of low-resistivity high B-value negative temperature coefficient thermal sensitive ceramic material and preparation method thereof |
| CN104193306A (en) * | 2014-08-20 | 2014-12-10 | 华南理工大学 | Thermal sensitive ceramic material with low resistivity, high B value and negative temperature coefficient and preparation method thereof |
| CN105552322B (en) * | 2015-12-13 | 2018-07-03 | 浙江美达瑞新材料科技有限公司 | Composite modified anode material for lithium-ion batteries of quaternary ion and preparation method thereof |
| CN105552322A (en) * | 2015-12-13 | 2016-05-04 | 浙江美达瑞新材料科技有限公司 | Quaternary ionic composite-modified positive pole material for lithium-ion battery and preparation method of quaternary ion composite-modified positive pole material |
| CN106211388A (en) * | 2016-07-05 | 2016-12-07 | 安徽吉安特种线缆制造有限公司 | A kind of self limiting temperature cable material of good weatherability |
| CN106699158B (en) * | 2017-01-18 | 2019-12-03 | 广州新莱福磁电有限公司 | A kind of manufacturing method of high-precision NTC thermistor chip |
| CN106699158A (en) * | 2017-01-18 | 2017-05-24 | 广州新莱福磁电有限公司 | Method for manufacturing high-precision NTC thermistor chip |
| CN108288529A (en) * | 2018-01-19 | 2018-07-17 | 安徽建筑大学 | A kind of preparation method for bearing low ageing rate negative temperature coefficient thermistor ceramic material |
| CN108288529B (en) * | 2018-01-19 | 2019-07-26 | 安徽建筑大学 | Bear the preparation method of low ageing rate negative temperature coefficient thermistor ceramic material |
| CN109133901A (en) * | 2018-10-29 | 2019-01-04 | 惠州嘉科实业有限公司 | Thermistor containing iron series and preparation method thereof |
| CN112390640A (en) * | 2020-11-13 | 2021-02-23 | 深圳顺络电子股份有限公司 | NTC thermistor and manufacturing 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 |
| CN116283231A (en) * | 2023-01-30 | 2023-06-23 | 广东风华高新科技股份有限公司 | NTC thermistor material and preparation method thereof |
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