CN109534809A - A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted - Google Patents
A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted Download PDFInfo
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- CN109534809A CN109534809A CN201910057966.1A CN201910057966A CN109534809A CN 109534809 A CN109534809 A CN 109534809A CN 201910057966 A CN201910057966 A CN 201910057966A CN 109534809 A CN109534809 A CN 109534809A
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- electric field
- barium titanate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped 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 titanium oxides or titanates
- C04B35/462—Shaped 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 titanium oxides or titanates based on titanates
- C04B35/465—Shaped 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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped 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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Abstract
The present invention relates to a kind of methods of low temperature Fast Sintering barium titanate ceramics by electric field-assisted, and barium titanate ceramics are warming up to certain temperature with certain heating rate, then add a suitable voltage, ceramic idiosome quick densifying at a lower temperature can be realized.During the sintering process, electric energy generates Joule heat, while the transmission process of electric field excitation solid particle in ceramic idiosome internal consumption, and improving Particle diffusion migration rate so that ceramic particle is shunk rapidly largely reduces sintering temperature, shortens the sintering period.Fine and close and tiny crystal grain barium titanate ceramics can be obtained using the method for this electric field-assisted, to improve the breakdown of PTC ceramics, the PTC ceramics worn for production high strike provides novel process.
Description
Technical field
The invention belongs to barium titanate PTC ceramics technical field of material, and in particular to a kind of electric field-assisted low temperature is quick
The method for being sintered barium titanate PTC ceramics.
Background technique
Thermistor is one kind of sensitive components, can be divided into posive temperature coefficient thermistor according to temperature coefficient difference
Device (PTC) and negative tempperature coefficient thermistor (NTC).The typical feature of thermistor be it is temperature sensitive, at a temperature of different
Show different resistance values.Positive temperature coefficient thermistor (PTC) resistance when temperature is higher is bigger.
Currently, for barium titanate-based PTC ceramics sintering processing be conventional sintering, idiosome after molding 1300 DEG C ~
2 hours are kept the temperature at 1340 DEG C is sintered.Its sintering period is long, sintering temperature is high.Furthermore ceramic post sintering consumes a large amount of energy, simultaneously
A large amount of room temperature air is generated, it is very unfavorable to environment.Therefore, develop a kind of quick sintering processing of low temperature to reduce energy consumption,
Sintering rate is improved, it is very necessary to reduce energy consumption.Ceramic post sintering is the process persistently densified simultaneously, is burnt in tradition
During knot, the sintering period is longer, and ceramic crystalline grain size is bigger, and abnormal grain growth is more obvious, usual barium titanate ceramics crystal grain
It is 10 ~ 20 μm, excessive crystallite dimension makes the breakdown performance decline of ceramics.For barium titanate PTC ceramics, using
Certain dieletric strength is needed in journey.The sintering process of ceramics how is controlled, sintering temperature is reduced, shortens sintering time, it is real
Existing low temperature Fast Sintering obtains the high-overpressure resistance barium titanate PTC ceramics of high-compactness, this seems especially in electronic ceramics application field
It is important.
Summary of the invention
Deficiency in view of the above technology, the present invention propose a kind of electric field-assisted low temperature Fast Sintering barium titanate PTC ceramics
Method, the method for use are electric field-assisted sintering, can choose corresponding different electric field strength for the sintering of different temperatures.
The technical issues of solution is how to realize low temperature Fast Sintering barium titanate PTC ceramics and make it have higher-density and smaller crystalline substance
Particle size, to improve the pressure-resistant performance of barium titanate ceramics.
A kind of method of electric field-assisted low temperature Fast Sintering barium titanate PTC ceramics, steps are as follows:
Step 1: barium titanate ceramics raw embryo is heated to critical-temperature；The critical-temperature is proper in the case where applying respective electric field intensity
Occurs the temperature of Fast Sintering well；
Step 2: critical electric field is applied to ceramic idiosome and forms a carrying current, and duration t (30 s≤t≤
300 s), and the sintering of ceramics is completed in time t；The critical electric field is the electric field strength that Fast Sintering can occur for ceramics；
The carrying current refers to the electric current that ceramic body can densify completely；
The critical-temperature T are as follows: 1025 DEG C≤T≤1075 DEG C.
The critical electric field strength E are as follows: the V/cm of 120 V/cm≤E≤160.
The limiting current density J are as follows: 30 mA/mm2≤J≤90 mA/mm2。
A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted proposed by the present invention, barium titanate is made pottery
Porcelain idiosome is warming up to certain temperature with certain heating rate, then adds a suitable electric field, ceramic low-temp may be implemented
Fast Sintering.Different electric field strengths can be applied depending on the temperature.Electric energy generates joule in ceramic body internal consumption
Heat, while the transmission process of electric field excitation solid particle, improve Particle diffusion migration rate, so that ceramic particle is shunk rapidly,
Sintering temperature is largely reduced, the sintering period is shortened.The low temperature Fast Sintering mode of this electric field-assisted can obtain
The tiny barium titanate ceramics of high-compactness crystal grain are obtained, to improve the breakdown performance of ceramics.
Detailed description of the invention
Fig. 1 varies with temperature curve for the sintering power under different sintering temperatures not same electric field.
Fig. 2 is the scanned photograph of barium titanate PTC ceramics prepared by different soaking times.
Specific embodiment
Now in conjunction with embodiment, attached drawing, the present invention will be further described:
Embodiment 1
1) ceramic body is heated to 1075 DEG C with the heating rate of 10 DEG C/min；
2) voltage for being 120V/cm plus electric field strength to the barium titanate idiosome for being warming up to 1075 DEG C, after several seconds, power supply is supplied
Constant current state is jumped into from constant pressure state to state, adjusting current density is 80 mA/mm2, removed after keeping 30 s in this state
Electric field, stove start to be down to room temperature with the rate of 5 DEG C/min to get the barium titanate PTC ceramics for being 94% to consistency.
Embodiment 2
1) ceramic body is heated to 1055 DEG C with the heating rate of 10 DEG C/min；
2) voltage for being 140V/cm plus electric field strength to the barium titanate idiosome for being warming up to 1055 DEG C, after several seconds, power supply is supplied
Constant current state is jumped into from constant pressure state to state, adjusting current density is 80 mA/mm2, removed after keeping 30 s in this state
Electric field, stove start to be down to room temperature with the rate of 5 DEG C/min to get the barium titanate PTC ceramics for being 96% to consistency.
Embodiment 3
1) ceramic body is heated to 1025 DEG C with the heating rate of 10 DEG C/min；
2) voltage for being 160V/cm plus electric field strength to the barium titanate idiosome for being warming up to 1025 DEG C, after several seconds, power supply is supplied
Constant current state is jumped into from constant pressure state to state, adjusting current density is 80 mA/mm2, removed after keeping 30 s in this state
Electric field, stove start to be down to room temperature with the rate of 5 DEG C/min to get the barium titanate PTC ceramics for being 95% to consistency.
Embodiment 4
1) ceramic body is heated to 1055 DEG C with the heating rate of 10 DEG C/min；
2) voltage for being 140V/cm plus electric field strength to the barium titanate idiosome for being warming up to 1055 DEG C, after several seconds, power supply is supplied
Constant current state is jumped into from constant pressure state to state, adjusting current density is 80 mA/mm2, removed after keeping 60 s in this state
Electric field, stove start to be down to room temperature with the rate of 5 DEG C/min to get the barium titanate PTC ceramics for being 95% to consistency.
Embodiment 5
1) ceramic body is heated to 1055 DEG C with the heating rate of 10 DEG C/min；
2) voltage for being 140V/cm plus electric field strength to the barium titanate green body for being warming up to 1055 DEG C, after several seconds, power supply is supplied
Constant current state is jumped into from constant pressure state to state, adjusting current density is 80 mA/mm2, 300 s is kept to drop back in this state
Electric field is removed, stove starts to be down to room temperature with the rate of 5 DEG C/min to get the barium titanate PTC ceramics for being 95% to consistency.
Claims (4)
1. a kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted, which comprises the steps of:
Step 1: barium titanate ceramics raw embryo is heated to critical-temperature；The critical-temperature is proper in the case where applying respective electric field intensity
Occurs the temperature of Fast Sintering well；
Step 2: critical electric field is applied to ceramic idiosome and forms a carrying current, and duration t, 30s≤t≤
300 s complete the sintering of ceramics in time t；The critical electric field is the electric field strength that Fast Sintering can occur for ceramics；Institute
It states carrying current and refers to the electric current that ceramic body can densify completely.
2. a kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted according to claim 1, feature
It is: the critical-temperature T are as follows: 1025 DEG C≤T≤1075 DEG C.
3. a kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted according to claim 1, feature
It is: the critical electric field strength E are as follows: the V/cm of 120 V/cm≤E≤160.
4. a kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted according to claim 1, feature
It is: the limiting current density J are as follows: 30 mA/mm2≤J≤90 mA/mm2。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
Citations (4)
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|---|---|---|---|---|
| KR970042426A (en) * | 1995-12-02 | 1997-07-24 | 손영목 | Manufacturing Method of Semiconducting BaTiO₃ Ceramics by Low Temperature Sintering |
| CN105645987A (en) * | 2016-01-20 | 2016-06-08 | 西北工业大学 | Method for electric-field-assisted low-temperature fast sintering of porous ceramics |
| CN106630974A (en) * | 2016-11-25 | 2017-05-10 | 中国工程物理研究院材料研究所 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
| CN108383522A (en) * | 2018-03-29 | 2018-08-10 | 长安大学 | A kind of low temperature Fast Sintering prepares the method and piezoelectric ceramics of PZT piezoelectric ceramics |
-
2019
- 2019-01-22 CN CN201910057966.1A patent/CN109534809A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR970042426A (en) * | 1995-12-02 | 1997-07-24 | 손영목 | Manufacturing Method of Semiconducting BaTiO₃ Ceramics by Low Temperature Sintering |
| CN105645987A (en) * | 2016-01-20 | 2016-06-08 | 西北工业大学 | Method for electric-field-assisted low-temperature fast sintering of porous ceramics |
| CN106630974A (en) * | 2016-11-25 | 2017-05-10 | 中国工程物理研究院材料研究所 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
| CN108383522A (en) * | 2018-03-29 | 2018-08-10 | 长安大学 | A kind of low temperature Fast Sintering prepares the method and piezoelectric ceramics of PZT piezoelectric ceramics |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
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