CN102617136A - Thermosensitive ceramic material and electromobile thermosensitive resistor made of thermosensitive ceramic material and manufacturing method of thermosensitive resistor - Google Patents
Thermosensitive ceramic material and electromobile thermosensitive resistor made of thermosensitive ceramic material and manufacturing method of thermosensitive resistor Download PDFInfo
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- CN102617136A CN102617136A CN2012100806517A CN201210080651A CN102617136A CN 102617136 A CN102617136 A CN 102617136A CN 2012100806517 A CN2012100806517 A CN 2012100806517A CN 201210080651 A CN201210080651 A CN 201210080651A CN 102617136 A CN102617136 A CN 102617136A
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Abstract
The invention discloses a thermosensitive ceramic material which comprises the following components in molar parts: 57-61 parts of BaCO3, 1.5-2 parts of SrCO3, 12-13 parts of Pb3O4, 1.5-2 parts of CaCO3, 101-102 parts of TiO2, 0.07-0.09 part of Y2O3, 0.07-0.09 part of SbO3 and 0.04-0.05 part of Mn(NO3)2 and sintering liquid-phase assistant. The invention also discloses an electromobile PTC (positive temperature coefficient) thermosensitive resistor made of the thermosensitive ceramic material and used for heating and a manufacturing method of the PTC thermosensitive resistor. The manufacturing method comprises the following steps of: mixing the above components according to the proportion, carrying out wet ball milling, presintering, secondary wet ball milling, pelleting and tabletting, sintering and then processing into a PTC thermosensitive resistor. The PTC thermosensitive resistor has the advantages of high-voltage resistance, moisture resistance, etchant gas resistance, has small current surge in a heating process and can completely meet the use requirement of an electromobile.
Description
Technical field
The invention belongs to the semiconductor ceramic material field, be specifically related to a kind of thermal sensitive ceramic material, and heat with thermistor and the method for making this thermistor by the electromobile that this thermal sensitive ceramic material makes.
Background technology
World level is led in China's electromobile research; Realized the industrial pattern that electromobile is more complete; In key component technology,, obtained major progress like aspects such as automobile fuel battery engine, store batteries; Form supporting industrial chain, might become the country that takes the lead in realizing the extensive commercial application of power truck in the world.
Along with the development of ev industry, the electromobile accessory is also proposed the requirement of technical renovation.The inner Working environment of electromobile is complicated, requires to be used in the ability that electric heater unit in the electromobile can have high pressure resistant, humidity, corrosion-resistant gas, requires the electric heater unit rush current more little good more simultaneously, with the protection automobile circuit.PTC (Positive Temperature Coefficient, posistor) is the significant components in the electric heater unit, the quality of decision electric heater unit.
Specific requirement is following:
1, PTC sheet proof voltage wants high, for PTC heating piece (24mm*15mm*3.0mm, the T of traditional specification
S255 ℃, resistance 1～3.5K Ω), proof voltage should be more than 1200V.
2, the PTC sheet has very high liftdrag, and the warm area scope at 110 ℃ can guarantee reasonable temperature capacity.
3, R
Min/ R
25 ℃Value can guarantee smaller rush current greater than 0.5.
4, reasonable corrosion resistance nature is arranged.
The electromobile of market heating at present can't be satisfied above 4 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 electromobile heating that is used for 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: 57～61 parts of BaCO
3, 1.5～2 parts of SrCO
3, 12～13 parts of Pb
3O
4, 1.5～2 parts of CaCO
3, 101～102 parts of TiO
2, 0.07～0.09 part of Y
2O
3, 0.07～0.09 part of Sb
2O
3, 0.04～0.05 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: 57.5 parts of BaCO
3, 1.5 parts of SrCO
3, 13 parts of Pb
3O
4, 2 parts of CaCO
3, 102 parts of TiO
2, 0.08 part of Y
2O
3, 0.07 part of Sb
2O
3, 0.05 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.
Comprise 1.2～1.4 parts of SiO by mole umber sintering liquid phase auxiliary agent
2With 1.5～1.8 parts of Al
2O
3
In preferred embodiment of the present invention, sintering liquid phase auxiliary agent comprises 1.2 parts of SiO
2With 1.5 parts of Al
2O
3
For solving the problems of the technologies described above, another technical scheme that the present invention adopts is: a kind of high voltage withstanding PTC is provided, is made by thermal sensitive ceramic material.This thermal sensitive ceramic material comprises by its composition of mole umber: 57～61 parts of BaCO
3, 1.5～2 parts of SrCO
3, 12～13 parts of Pb
3O
4, 1.5～2 parts of CaCO
3, 101～102 parts of TiO
2, 0.07～0.09 part of Y
2O
3, 0.07～0.09 part of Sb
2O
3, 0.04～0.05 part of Mn (NO
3)
2And sintering liquid phase auxiliary agent.With BaCO
3, SrCO
3, Pb
3O
4, 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 1090～1100 ℃ through the mixture behind the above-mentioned wet ball grinding in temperature, is incubated 2.5～3.5 hours;
Preferably be incubated 3 hours down at 1090 ℃;
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 27.95mm*17.42mm*3.8mm then, and density is 3.5g/cm
3Square sheet;
Described sintering is to be under 1300～1320 ℃ in temperature, is incubated 0.5～1.5 hour, and 1.5～2 ℃/minute cool to 800 ℃, cool to room temperature then naturally;
Preferred sintering temperature is 1310 ℃, is incubated 1 hour, and 1.5 ℃/minute cool to 800 ℃;
Described post-treatment is sintering to be accomplished later PTC sheet carry out the planar thickness grinding, dries 1.5～2.5 hours for 100～150 ℃, and vacuum sputtering aluminium electrode is processed 24mm*15mm*3.0mm, T
S255 ℃, resistance 1～3.5K Ω product;
Preferred 130 ℃ of oven dry 2 hours.
The PTC finished product that thermal sensitive ceramic material of the present invention makes is withstand voltage can to reach 1200V, has 10
4Liftdrag, R
Min/ R
25 ℃Value is greater than 0.5, and withstand voltage properties is higher than 400V/mm, and electrode uses the mode of vacuum sputtering to make the aluminium electrode, can guarantee reasonable corrosion resistance nature, and this PTC sheet can fully satisfy the electromobile request for utilization.
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 57 parts of BaCO
3, 1.8 parts of SrCO
3, 12 parts of Pb
3O
4, 1.5 parts of CaCO
3, 101 parts of TiO
2
Execute the acceptor doping thing and comprise 0.07 part of Y
2O
3, 0.07 part of Sb
2O
3, 0.04 part of Mn (NO
3)
2
Sintering liquid phase auxiliary agent comprises 1.2 parts of SiO
2With 1.6 parts 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 61 parts of BaCO
3, 2 parts of SrCO
3, 12.5 parts of Pb
3O
4, 1.8 parts of CaCO
3, 101.5 parts of TiO
2
Execute the acceptor doping thing and comprise 0.09 part of Y
2O
3, 0.08 part of Sb
2O
3, 0.05 part of Mn (NO
3)
2
Sintering liquid phase auxiliary agent comprises 1.4 parts of SiO
2With 1.8 parts 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 57.5 parts of BaCO
3, 1.5 parts of SrCO
3, 13 parts of Pb
3O
4, 2 parts of CaCO
3, 102 parts of TiO
2
Execute the acceptor doping thing and comprise 0.08 part of Y
2O
3, 0.07 part of Sb
2O
3, 0.05 part of Mn (NO
3)
2
Sintering liquid phase auxiliary agent comprises 1.2 parts of SiO
2With 1.5 parts 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, 1090 ℃ of pre-burnings 3.5 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 27.95mm*17.42mm*3.8mm, and density is 3.5g/cm
3Square sheet;
Sintering: square sheet 1300 ℃ of insulations 1.5 hours, 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 the planar thickness grinding, dries 2.5 hours for 100 ℃, and vacuum sputtering aluminium electrode is processed 24mm*15mm*3.0mm, T
S255 ℃, resistance 1～3.5K Ω product.
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, 1100 ℃ of pre-burnings 2.5 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 27.95mm*17.42mm*3.8mm, and density is 3.5g/cm
3Square sheet;
Sintering: square sheet 1320 ℃ of insulations 0.5 hour, 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 the planar thickness grinding, dries 1.5 hours for 150 ℃, and vacuum sputtering aluminium electrode is processed 24mm*15mm*3.0mm, T
S255 ℃, resistance 1～3.5K Ω product.
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, 1090 ℃ 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 27.95mm*17.42mm*3.8mm, and density is 3.5g/cm
3Square sheet;
Sintering: square sheet 1310 ℃ of insulations 1 hour, 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 the planar thickness grinding, dries 2 hours for 130 ℃, and vacuum sputtering aluminium electrode is processed 24mm*15mm*3.0mm, T
S255 ℃, resistance 1～3.5K Ω product.The PTC finished product that thermal sensitive ceramic material of the present invention makes is withstand voltage can to reach 1200V, has 10
4Liftdrag, R
Min/ R
25 ℃Value is greater than 0.5, and withstand voltage properties is higher than 400V/mm, and electrode uses the mode of vacuum sputtering to make the aluminium electrode, can guarantee reasonable corrosion resistance nature, and this PTC sheet can fully satisfy the electromobile request for utilization.
Claims (7)
1. a thermal sensitive ceramic material is characterized in that, it comprises following component according to the molfraction meter: 57～61 parts of BaCO
3, 1.5～2 parts of SrCO
3, 12～13 parts of Pb
3O
4, 1.5～2 parts of CaCO
3, 101～102 parts of TiO
2, 0.07～0.09 part of Y
2O
3, 0.07～0.09 part of Sb
2O
3, 0.04～0.05 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: 57.5 parts of BaCO
3, 1.5 parts of SrCO
3, 13 parts of Pb
3O
4, 2 parts of CaCO
3, 102 parts of TiO
2, 0.08 part of Y
2O
3, 0.07 part of Sb
2O
3, 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 1.2～1.4 parts of SiO by the mole umber
2With 1.5～1.8 parts of Al
2O
3
4. stupalith according to claim 3 is characterized in that: said sintering liquid phase auxiliary agent comprises 1.2 parts of SiO by the mole umber
2With 1.5 parts of Al
2O
3
5. posistor is used in an electromobile heating, and 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 1090～1100 ℃ with the mixture behind the wet ball grinding in temperature, is incubated 2.5～3.5 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 27.95mm*17.42mm*3.8mm then, density is 3.5g/cm
3Square sheet;
E) sintering: in temperature is under 1300～1320 ℃, is incubated 0.5～1.5 hour, 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 the planar thickness grinding, dried 1.5～2.5 hours for 100～150 ℃, vacuum sputtering aluminium electrode is processed 24mm*15mm*3.0mm, T
S255 ℃, resistance 1～3.5K Ω product.
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 1090 ℃ 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 27.95mm*17.42mm*3.8mm then, density is 3.5g/cm
3Square sheet;
E) sintering: in temperature is under 1310 ℃, is incubated 1 hour, and 1.5 ℃/minute cool to 800 ℃, cool to room temperature then naturally;
F) post-treatment: sintering is accomplished later PTC sheet carry out the planar thickness grinding, dried 2 hours for 130 ℃, vacuum sputtering aluminium electrode is processed 24mm*15mm*3.0mm, T
S255 ℃, resistance 1～3.5K Ω product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100806517A CN102617136A (en) | 2012-03-26 | 2012-03-26 | Thermosensitive ceramic material and electromobile thermosensitive resistor made of thermosensitive ceramic material and manufacturing method of thermosensitive resistor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100806517A CN102617136A (en) | 2012-03-26 | 2012-03-26 | Thermosensitive ceramic material and electromobile thermosensitive resistor made of thermosensitive ceramic material and manufacturing method of thermosensitive resistor |
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|---|---|
| CN102617136A true CN102617136A (en) | 2012-08-01 |
Family
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|---|---|---|---|
| CN2012100806517A Pending CN102617136A (en) | 2012-03-26 | 2012-03-26 | Thermosensitive ceramic material and electromobile thermosensitive resistor made of thermosensitive ceramic material and manufacturing method of thermosensitive resistor |
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Citations (5)
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|---|---|---|---|---|
| CN101429020A (en) * | 2008-11-26 | 2009-05-13 | 丹东国通电子元件有限公司 | Method for producing positive temperature coefficient thermistor for surge suppressor |
| CN101447264A (en) * | 2008-12-24 | 2009-06-03 | 丹东科亮电子有限公司 | Manufacturing method of PTC thermistance and PTC thermistance thereof |
| CN101894641A (en) * | 2010-06-23 | 2010-11-24 | 深圳市三宝创业科技有限公司 | Method for improving thermosensitive resistor production efficiency |
| CN101891464A (en) * | 2010-06-29 | 2010-11-24 | 章慧 | High temperature thermistor and manufacturing method thereof |
| CN102040378A (en) * | 2010-08-23 | 2011-05-04 | 仙桃市展朋新材料有限公司 | Lead-series low-resistivity heat-sensitive resistor and manufacturing method thereof |
-
2012
- 2012-03-26 CN CN2012100806517A patent/CN102617136A/en active Pending
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|---|---|---|---|---|
| CN101429020A (en) * | 2008-11-26 | 2009-05-13 | 丹东国通电子元件有限公司 | Method for producing positive temperature coefficient thermistor for surge suppressor |
| CN101447264A (en) * | 2008-12-24 | 2009-06-03 | 丹东科亮电子有限公司 | Manufacturing method of PTC thermistance and PTC thermistance thereof |
| CN101894641A (en) * | 2010-06-23 | 2010-11-24 | 深圳市三宝创业科技有限公司 | Method for improving thermosensitive resistor production efficiency |
| CN101891464A (en) * | 2010-06-29 | 2010-11-24 | 章慧 | High temperature thermistor and manufacturing method thereof |
| CN102040378A (en) * | 2010-08-23 | 2011-05-04 | 仙桃市展朋新材料有限公司 | Lead-series low-resistivity heat-sensitive resistor and manufacturing method thereof |
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|---|
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Application publication date: 20120801 |