CN102617135A - Thermal sensitive ceramic material and thermistor for overcurrent protection prepared by using thermal sensitive ceramic material and preparation method - Google Patents
Thermal sensitive ceramic material and thermistor for overcurrent protection prepared by using thermal sensitive ceramic material and preparation method Download PDFInfo
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- CN102617135A CN102617135A CN2012100805995A CN201210080599A CN102617135A CN 102617135 A CN102617135 A CN 102617135A CN 2012100805995 A CN2012100805995 A CN 2012100805995A CN 201210080599 A CN201210080599 A CN 201210080599A CN 102617135 A CN102617135 A CN 102617135A
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Abstract
The invention discloses a thermal sensitive ceramic material which comprises the following components in parts by mole: 69-71 parts of BaCO3, 13-15 parts of SrCO3, 6-8 parts of PbO, 8-10 parts of CaCO3, 101-102 parts of TiO2, 0.04-0.06 part of Y2O3, 0.03-0.04 part of Sb2O5, 0.05-0.06 part of Mn(NO3)2 as well as a sintered liquid phase additive. The invention also discloses a low-temperature-resistant high-voltage-resistant PTC (positive temperature coefficient) thermistor for overcurrent protection prepared by using the thermal sensitive ceramic material and a method for preparing the PTC thermistor. The method comprises the following steps: mixing the components according to the designed ratio, ball milling by a wet method, pre-sintering, ball milling by a secondary wet method, pelleting and tabletting, sintering and post processing, thereby preparing the PTC thermistor. The PTC thermistor resistance value can reach 800 Ohm-1200Ohm, and the product meet the bearing capability and self recovery capability under the conditions of extreme low temperature and extreme high temperature and high-voltage impact.
Description
Technical field
The invention belongs to the semiconductor ceramic material field, be specifically related to a kind of thermal sensitive ceramic material, and the low temperature resistant high pressure resistant overcurrent protection that is made by this thermal sensitive ceramic material is with thermistor and the method for making this thermistor.
Background technology
PTC (Positive Temperature Coefficient, posistor) is used in the environment of high-voltage, very low temperature, is very big tests to product performance.There is quite a few country in 1 year, to have quite a few time to be in the severe cold below-20 ℃ in the world, uses the high performance PTC of needs such as power equipment in outdoor environment, signal equipment that it is protected.
Specific requirement is following:
1, resistance 800 Ω～1200 Ω.
2, under-40 ℃ of conditions, satisfy 1000V/1A, logical 1 minute disconnected 5 minutes 20 times, product does not have damage, and change in resistance is less than 20%.
3, under 60 ℃ of conditions, satisfy 1000V/1A, logical 1 minute disconnected 5 minutes 20 times, product does not have damage, and change in resistance is less than 20%.
The low temperature resistant high pressure resistant overcurrent protection of market at present can't be satisfied above 3 kinds of requirements simultaneously with PTC.
Summary of the invention
The technical problem that the present invention mainly solves provides a kind of thermal sensitive ceramic material and uses PTC by the low temperature resistant high pressure resistant overcurrent protection that this thermal sensitive ceramic material makes.
The present invention also provides a kind of method of making this PTC.
The technical scheme that the present invention adopts is: a kind of thermal sensitive ceramic material comprises by its composition of mole umber: 69～71 parts of BaCO
3, 13～15 parts of SrCO
3, 6～8 parts of PbO, 8～10 parts of CaCO
3, 101～102 parts of TiO
2, 0.04～0.06 part of Y
2O
3, 0.03～0.04 part of Nb
2O
5, 0.05～0.06 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.
In preferred embodiment of the present invention, the composition of thermal sensitive ceramic material comprises by the mole umber: 70 parts of BaCO
3, 14 parts of SrCO
3, 7 parts of PbO, 9 parts of CaCO
3, 102 parts of TiO
2, 0.05 part of Y
2O
3, 0.04 part of Nb
2O
5, 0.05 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.
Comprise 1.2～1.5 parts of SiO by mole umber sintering liquid phase auxiliary agent
2With 0.5～0.5 part of Al
2O
3
In preferred embodiment of the present invention, sintering liquid phase auxiliary agent comprises 1.3 parts of SiO
2With 0.4 part of Al
2O
3
For solving the problems of the technologies described above, another technical scheme that the present invention adopts is: provide a kind of low temperature resistant high pressure resistant overcurrent protection to use PTC, made by thermal sensitive ceramic material.This thermal sensitive ceramic material comprises by its composition of mole umber: 69～71 parts of BaCO
3, 13～15 parts of SrCO
3, 6～8 parts of PbO, 8～10 parts of CaCO
3, 101～102 parts of TiO
2, 0.04～0.06 part of Y
2O
3, 0.03～0.04 part of Nb
2O
5, 0.05～0.06 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.With BaCO
3, SrCO
3, PbO, TiO
2, CaCO
3Deng the principal crystalline phase composition and execute the acceptor doping thing and sintering liquid phase auxiliary agent according to the design the ratio batch mixes after steps such as wet ball grinding, presintering, secondary wet process ball milling, granulation and compressing tablet, sintering, post-treatment make the PTC sheet.
Described wet ball grinding is with said mixture wet ball grinding 20～28 hours, and material: ball: the weight ratio of water is 0.5～1.5: 1～3: 1～2, and slurry is 100～150 ℃ of dryings;
Preferred wet ball grinding 24 hours, material: ball: the weight ratio of water is 1: 2: 1.5, slurry is dry down at 130 ℃;
Described presintering is with being under 1140～1160 ℃ through the mixture behind the above-mentioned wet ball grinding in temperature, is incubated 2～4 hours;
Preferably be incubated 3 hours down at 1150 ℃;
Described secondary wet process ball milling is that material: ball: the weight ratio of water is 0.5～1.5: 1～3 with the mixture of presintering wet ball grinding 20～28 hours once more: 1～2, and slurry is 100～150 ℃ of dryings;
Preferred wet ball grinding 24 hours, material: ball: the weight ratio of water is 1: 2: 1.5, slurry is dry down at 130 ℃;
Described granulation and compressing tablet are to add the PVA granulation, are pressed into φ 10.3*4.1mm then, and density is 3.3g/cm
3Disk;
Described sintering is to be under 1310～1330 ℃ in temperature, is incubated 50～70 minutes, and 1.5～2 ℃/minute cool to 800 ℃, cool to room temperature then naturally;
Preferred sintering temperature is 1320 ℃, is incubated 60 minutes, and 2 ℃/minute cool to 800 ℃;
Described post-treatment is sintering to be accomplished later PTC sheet carry out Yin Yin, obtain φ 9*3.5mm, the finished product of resistance 800 Ω～1200 Ω after welding, sealing.
The PTC finished product resistance that thermal sensitive ceramic material of the present invention makes can reach 800 Ω～1200 Ω; Under-40 ℃ and 60 ℃ of conditions; Satisfy 1000V/1A respectively, logical 1 minute disconnected 5 minutes 20 times, product does not have damage; Change in resistance is less than 20%, and product satisfies ability to bear and the self-recovery ability under impacting with high pressure under the condition of extreme low temperature and thermal extremes.
Embodiment
Set forth in detail in the face of preferred embodiment of the present invention down, thereby protection scope of the present invention is made more explicit defining so that advantage of the present invention and characteristic can be easier to it will be appreciated by those skilled in the art that.
Embodiment 1-3 is the thermal sensitive ceramic material compsn:
Embodiment 1
According to the molfraction meter, with the principal crystalline phase composition of following proportioning, execute the acceptor doping thing and sintering liquid phase auxiliary agent mixes:
The principal crystalline phase composition comprises 69 parts of BaCO
3, 13 parts of SrCO
3, 6 parts of PbO, 8 parts of CaCO
3, 101 parts of TiO
2
Execute the acceptor doping thing and comprise 0.04 part of Y
2O
3, 0.03 part of Nb
2O
5, 0.05 part of Mn (NO
3)
2
Sintering liquid phase auxiliary agent comprises 1.2 parts of SiO
2With 0.3 part of Al
2O
3
Embodiment 2
According to the molfraction meter, with the principal crystalline phase composition of following proportioning, execute the acceptor doping thing and sintering liquid phase auxiliary agent mixes:
The principal crystalline phase composition comprises 71 parts of BaCO
3, 15 parts of SrCO
3, 8 parts of PbO, 10 parts of CaCO
3, 101 parts of TiO
2
Execute the acceptor doping thing and comprise 0.06 part of Y
2O
3, 0.04 part of Nb
2O
5, 0.06 part of Mn (NO
3)
2
Sintering liquid phase auxiliary agent comprises 1.5 parts of SiO
2With 0.5 part of Al
2O
3
Embodiment 3
According to the molfraction meter, with the principal crystalline phase composition of following proportioning, execute the acceptor doping thing and sintering liquid phase auxiliary agent mixes:
The principal crystalline phase composition comprises 70 parts of BaCO
3, 14 parts of SrCO
3, 7 parts of PbO, 9 parts of CaCO
3, 102 parts of TiO
2
Execute the acceptor doping thing and comprise 0.05 part of Y
2O
3, 0.04 part of Nb
2O
5, 0.05 part of Mn (NO
3)
2
Sintering liquid phase auxiliary agent comprises 1.3 parts of SiO
2With 0.4 part of Al
2O
3
Embodiment 4-6 serve as reasons PTC that this thermal sensitive ceramic material mixture makes and the method for making PTC:
Embodiment 4
Each composition is prepared burden in embodiment 1, embodiment 2 or embodiment 3 arbitrary ratios, mix.
Wet ball grinding: with mixed raw material, ball, water with 0.5: 1: 1 weight ratio mixed mixed slurry, wet ball grinding 20 hours;
Presintering: with above-mentioned mixed slurry after 100 ℃ of dryings, 1140 ℃ of pre-burnings 4 hours;
The secondary wet process ball milling: material, ball, water are with mixed mixed slurry, the wet ball grinding 20 hours of getting of 0.5: 1: 1 weight ratio;
Granulation: the mixed slurry after above-mentioned the milling 100 ℃ of dryings, is added sticker PVA (Z 150PH) granulation then;
Compressing tablet: granulated pellet is pressed into φ 10.3*4.1mm, and density is 3.3g/cm
3Disk;
Sintering: disk 1310 ℃ of insulations 70 minutes, is cooled to 800 ℃ with 1.5 ℃/minute speed then, cool to room temperature more naturally;
Post-treatment: sintering is accomplished later PTC sheet and is carried out Yin Yin, obtains φ 9*3.5mm, the finished product of resistance 800 Ω～1200 Ω after welding, sealing.
Embodiment 5
Each composition is prepared burden in embodiment 1, embodiment 2 or embodiment 3 arbitrary ratios, mix.
Wet ball grinding: with mixed raw material, ball, water with 1.5: 3: 2 weight ratio mixed mixed slurry, wet ball grinding 28 hours;
Presintering: with above-mentioned mixed slurry after 150 ℃ of dryings, 1160 ℃ of pre-burnings 2 hours;
The secondary wet process ball milling: material, ball, water are with mixed mixed slurry, the wet ball grinding 28 hours of getting of 1.5: 3: 2 weight ratio;
Granulation: the mixed slurry after above-mentioned the milling 150 ℃ of dryings, is added sticker PVA (Z 150PH) granulation then;
Compressing tablet: granulated pellet is pressed into φ 10.3*4.1mm, and density is 3.3g/cm
3Disk;
Sintering: disk 1330 ℃ of insulations 50 minutes, is cooled to 800 ℃ with 2 ℃/minute speed then, cool to room temperature more naturally;
Post-treatment: sintering is accomplished later PTC sheet and is carried out Yin Yin, obtains φ 9*3.5mm, the finished product of resistance 800 Ω～1200 Ω after welding, sealing.
Embodiment 6
With the ratio batching of each composition, mix in embodiment 3.
Wet ball grinding: with mixed raw material, ball, water with 1: 2: 1.5 weight ratio mixed mixed slurry, wet ball grinding 24 hours;
Presintering: with above-mentioned mixed slurry after 130 ℃ of dryings, 1150 ℃ of pre-burnings 3 hours;
The secondary wet process ball milling: material, ball, water are with mixed mixed slurry, the wet ball grinding 24 hours of getting of 1: 2: 1.5 weight ratio;
Granulation: the mixed slurry after above-mentioned the milling 130 ℃ of dryings, is added sticker PVA (Z 150PH) granulation then;
Compressing tablet: granulated pellet is pressed into φ 10.3*4.1mm, and density is 3.3g/cm
3Disk;
Sintering: disk 1320 ℃ of insulations 60 minutes, is cooled to 800 ℃ with 2 ℃/minute speed then, cool to room temperature more naturally;
Post-treatment: sintering is accomplished later PTC sheet and is carried out Yin Yin, obtains φ 9*3.5mm, the finished product of resistance 800 Ω～1200 Ω after welding, sealing.
The PTC finished product resistance that thermal sensitive ceramic material of the present invention makes can reach 800 Ω～1200 Ω; Under-40 ℃ and 60 ℃ of conditions; Satisfy 1000V/1A respectively, logical 1 minute disconnected 5 minutes 20 times, product does not have damage; Change in resistance is less than 20%, and product satisfies ability to bear and the self-recovery ability under impacting with high pressure under the condition of extreme low temperature and thermal extremes.
Claims (7)
1. a thermal sensitive ceramic material is characterized in that, it comprises following component according to the molfraction meter: 69～71 parts of BaCO
3, 13～15 parts of SrCO
3, 6～8 parts of PbO, 8～10 parts of CaCO
3, 101～102 parts of TiO
2, 0.04～0.06 part of Y
2O
3, 0.03～0.04 part of Nb
2O
5, 0.05～0.06 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.
2. stupalith according to claim 1 is characterized in that, it comprises following component according to the molfraction meter: 70 parts of BaCO
3, 14 parts of SrCO
3, 7 parts of PbO, 9 parts of CaCO
3, 102 parts of TiO
2, 0.05 part of Y
2O
3, 0.04 part of Nb
2O
5, 0.05 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.
3. according to claim 1 or 2 described stupaliths, it is characterized in that: said sintering liquid phase auxiliary agent comprises 1.2～1.5 parts of SiO by the mole umber
2With 0.5～0.5 part of Al
2O
3
4. stupalith according to claim 3 is characterized in that: said sintering liquid phase auxiliary agent comprises 1.3 parts of SiO by the mole umber
2With 0.4 part of Al
2O
3
5. posistor is used in a low temperature resistant high pressure resistant overcurrent protection, it is characterized in that: said thermistor is made by the arbitrary described thermal sensitive ceramic material of claim 1～4.
6. a method of making the said thermistor of claim 5 is characterized in that, may further comprise the steps:
A) wet ball grinding: mixture is mixed in proportion, wet ball grinding 20～28 hours, material: ball: the weight ratio of water is 0.5～1.5: 1～3: 1～2, slurry is 100～150 ℃ of dryings;
B) presintering: is under 1140～1160 ℃ with the mixture behind the wet ball grinding in temperature, is incubated 2～4 hours;
C) secondary wet process ball milling: with the mixture of presintering wet ball grinding 20～28 hours once more, material: ball: the weight ratio of water is 0.5～1.5: 1～3: 1～2, and slurry is 100～150 ℃ of dryings;
D) granulation and compressing tablet: add the PVA granulation, be pressed into φ 10.3*4.1mm then, density is 3.3g/cm
3Disk;
E) sintering: in temperature is under 1310～1330 ℃, is incubated 50～70 minutes, and 1.5～2 ℃/minute cool to 800 ℃, cool to room temperature then naturally;
F) post-treatment: sintering is accomplished later PTC sheet carry out Yin Yin, obtain φ 9*3.5mm, the finished product of resistance 800 Ω～1200 Ω after welding, sealing.
7. according to the method for the said manufacturing thermistor of claim 6, it is characterized in that, may further comprise the steps:
A) wet ball grinding: mixture is mixed in proportion, wet ball grinding 24 hours, material: ball: the weight ratio of water is 1: 2: 1.5, and slurry is 130 ℃ of dryings;
B) presintering: is under 1150 ℃ with the mixture behind the wet ball grinding in temperature, is incubated 3 hours;
C) secondary wet process ball milling: with the mixture of presintering wet ball grinding 24 hours once more, material: ball: the weight ratio of water is 1: 2: 1.5, and slurry is 130 ℃ of dryings;
D) granulation and compressing tablet: add the PVA granulation, be pressed into φ 10.3*4.1mm then, density is 3.3g/cm
3Disk;
E) sintering: in temperature is under 1320 ℃, is incubated 60 minutes, and 2 ℃/minute cool to 800 ℃, cool to room temperature then naturally;
F) post-treatment: sintering is accomplished later PTC sheet carry out Yin Yin, obtain φ 9*3.5mm, the finished product of resistance 800 Ω～1200 Ω after welding, sealing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100805995A CN102617135A (en) | 2012-03-26 | 2012-03-26 | Thermal sensitive ceramic material and thermistor for overcurrent protection prepared by using thermal sensitive ceramic material and preparation method |
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|---|---|---|---|
| CN2012100805995A CN102617135A (en) | 2012-03-26 | 2012-03-26 | Thermal sensitive ceramic material and thermistor for overcurrent protection prepared by using thermal sensitive ceramic material and preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285337A (en) * | 2018-04-04 | 2018-07-17 | 宜兴市国强炉业有限公司 | A kind of cooling activeness and quietness corundum wear-resistant material and preparation method thereof |
| CN113548885A (en) * | 2020-04-24 | 2021-10-26 | 惠州市聚鼎电子有限公司 | Development method of low-temperature PPTC (polymeric positive temperature coefficient) of power battery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1137679A (en) * | 1995-06-02 | 1996-12-11 | 上海大地通信电子有限公司 | Production process for positive temp. coefficient ceramic thermal resistor |
| CN101357844A (en) * | 2008-09-02 | 2009-02-04 | 周金平 | PTC thermal sensitive ceramic material and method for preparing the same |
| CN101805178A (en) * | 2010-01-22 | 2010-08-18 | 华中科技大学 | High-energy ball milling preparation method of barium titanate-based semiconductor ceramics |
-
2012
- 2012-03-26 CN CN2012100805995A patent/CN102617135A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1137679A (en) * | 1995-06-02 | 1996-12-11 | 上海大地通信电子有限公司 | Production process for positive temp. coefficient ceramic thermal resistor |
| CN101357844A (en) * | 2008-09-02 | 2009-02-04 | 周金平 | PTC thermal sensitive ceramic material and method for preparing the same |
| CN101805178A (en) * | 2010-01-22 | 2010-08-18 | 华中科技大学 | High-energy ball milling preparation method of barium titanate-based semiconductor ceramics |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285337A (en) * | 2018-04-04 | 2018-07-17 | 宜兴市国强炉业有限公司 | A kind of cooling activeness and quietness corundum wear-resistant material and preparation method thereof |
| CN113548885A (en) * | 2020-04-24 | 2021-10-26 | 惠州市聚鼎电子有限公司 | Development method of low-temperature PPTC (polymeric positive temperature coefficient) of power battery |
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Application publication date: 20120801 |