CN102745984B - High-curie-point lead-free PTC (Positive Temperature Coefficient) ceramic material and preparation method thereof - Google Patents

High-curie-point lead-free PTC (Positive Temperature Coefficient) ceramic material and preparation method thereof Download PDF

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CN102745984B
CN102745984B CN201210261384.3A CN201210261384A CN102745984B CN 102745984 B CN102745984 B CN 102745984B CN 201210261384 A CN201210261384 A CN 201210261384A CN 102745984 B CN102745984 B CN 102745984B
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CN102745984A (en
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蒲永平
袁启斌
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Yancheng Qinglong Jinbang water Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention provides a high-curie-point lead-free PTC (Positive Temperature Coefficient) ceramic material and a preparation method of the ceramic material. The ceramic material mainly comprises Ba1-x(K0.5Bi0.5)xTiO3, wherein x is more than or equal to 0.05 and smaller than or equal to 0.3. The high-curie-point PTC ceramic material provided by the invention does not contain lead, so damages of resistor devices to the human bodies and the environment in manufacturing and using processes are avoided; the processes of oxidation and then reduction are adopted, so semi-conduction of the material is achieved without donor doping; and PTC heat-sensitive materials with different curie points can be prepared through controlling the doping quantities of KBT (KBiTiO).

Description

A kind of high-Curie-point lead-free PTC ceramic material and preparation method thereof
Technical field
The present invention relates to a kind of semi-conducting material, particularly a kind ofly meet K unleaded, low-resistance 0.5bi 0.5tiO 3(KBT) high-concentration dopant BaTiO 3(BT) high-Curie-point lead-free PTC thermistor ceramic material and preparation method thereof.
Background technology
BaTiO 3base positive temperature coefficient resistance (positive temperature coefficient resistance is called for short PTCR) ceramic material is a kind of Ferro-Electric Semiconductor material, is development in recent years one of novel electron material rapidly.Because PTCR ceramic material has " switch " function automatically such as temperature sensitive, current limliting, time delay, the every field such as telecommunications, Aero-Space, auto industry, household electrical appliance have been widely used in.
Yet current piezoelectricity and ferroelectric material that can be practical be mainly to using Pb as the mobile agent of Curie point, realize with the lattice position of Pb displacement Ba.This series products is because its good stability, repeatability and higher Curie point are widely used.But containing Pb oxide, inevitably because of a variety of causes, flow into living environment and natural environment, thereby human body and natural environment are worked the mischief.Because current various countries are to the improving constantly of environmental requirement, PTCR material unleaded become a kind of inexorable trend.Environmentally friendly PTCR thermal sensitive ceramic material has far-reaching social effect and economic implications.
One of system of various countries researcher most study is BT-KBT at present, but focuses mostly in KBT(K 0.5bi 0.5tiO 3) to BT(BaTiO 3) low concentration doping (being generally no more than 5%).
Summary of the invention
The object of the present invention is to provide a kind of high-Curie-point lead-free PTC ceramic material and preparation method thereof.
For achieving the above object, the present invention has adopted following technical scheme.
A high-Curie-point lead-free PTC ceramic material, this ceramic material comprises following component:
Ba 1-x(K 0.5Bi 0.5) xTiO 3
, 0.05≤x≤0.3 wherein.
The preparation method of above-mentioned high-Curie-point lead-free PTC ceramic material, comprises the following steps:
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 350-500r/min respectively in mixture A and mixture B, after ball milling, at 80-100 ℃, dry;
2), after step 1), mixture A is incubated at 900-950 ℃ to the synthetic K of 2-3h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 2-3h at 1100-1150 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and M are according to the mixture C of preparing burden to obtain of formula below:
Ba 1-x(K 0.5Bi 0.5) xTiO 3+yM
0.05≤x≤0.3 wherein, 0≤y≤0.05, y gets 0 o'clock, sintering temperature can be higher, and M is the minor compound additive as sintering agent, glassy phase and reinforcing material temperature coefficient, to adding after deionized water ball milling 4h under the rotating speed of 350-500r/min in mixture C, after ball milling, at 80-100 ℃, dry, then granulation, moulding obtain idiosome;
4) by idiosome in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen, be incubated 1-2h at 800-1100 ℃, obtain high-Curie-point lead-free PTC ceramic material.
Described M is one or several the mixture containing in the oxide of Si, Al, Ti or Mn.
In the described argon gas that is mixed with trace oxygen, the volume fraction of oxygen is 0.5-4%.
The high-Curie-point lead-free PTC ceramic material that the present invention prepares can reach following parameter request: Tc=150-230 ℃ through resistance material Characteristics Detection; R 25≤ 3.5k Ω; Lg (R max/ R min)>=3.0.Characteristics Detection adopts In-Ga alloy as electrode, records room temperature resistance and the resistance-temperature curve of components and parts.In actual production, can select other electrode materials (as aluminium electrode, nickel electrode etc.).
The preparation method of high-Curie-point lead-free PTC ceramic material of the present invention has the following advantages: 1. adopt conventional solid-state method to prepare powder, particle without reuniting, fillibility is good, cost is low, output is large, preparation technology is simple, easy control of reaction conditions.2. by KBT, the high concentration of BT (5% ~ 30%) is adulterated to realize the raising of Curie point.3. sample carries out sintering in argon gas atmosphere, realizes resistance lowering, the semiconducting of sample in the situation that not carrying out donor doping.4. the sample after reduction is at Ar and O 2mist in, reoxidize.By controlling the ratio of each component in mist, execute oxygen temperature, execute the conditions such as oxygen time, to control the lift-drag ratio of material.5. the high-Curie-point PTC ceramic material that prepared by the present invention is not leaded, has avoided resistance element, in manufacture and use procedure, human body and environment are produced to harm.The technique that adopts reduction to reoxidize, has realized the semiconducting of material in the situation that not carrying out donor doping.And can pass through the control to KBT doping, to realize the preparation of the PTC thermo-sensitive material of different Curie points.6. the preparation method of high-Curie-point lead-free PTC ceramic material of the present invention can obtain high-purity phase composition, stable performance, high-Curie-point PTC thermistor that reliability is high, in the formula of principal component, the doping scope of KBT is wide, in actual application, can adjust accordingly according to production technology, flexibility is large.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 400r/min respectively in mixture A and mixture B, after ball milling, filter and remove ballstone, then at 80 ℃, dry;
2), after step 1), mixture A is incubated at 925 ℃ to the synthetic K of 2h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 3h at 1100 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and SiO 2according to formula Ba 1-x(K 0.5bi 0.5) xtiO 3+ ySiO 2prepare burden and obtain mixture C, x=0.05 wherein, y=0.05, to adding after a certain amount of deionized water ball milling 4h under the rotating speed of 400r/min in mixture C, after ball milling, filter and remove ballstone, then at 80 ℃, through 6 hours, dry, after oven dry, add a certain amount of PVA granulation, moulding to obtain idiosome, idiosome is wafer type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) by idiosome in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen (volume fraction of oxygen is 2%), be incubated 1h at 900 ℃ and reoxidize, so that grain boundary oxidation and form crystal boundary potential barrier and obtain high-Curie-point lead-free PTC ceramic material;
6) two sides of lead-free PTC ceramic material is polished, be coated with In-Ga alloy as electrode;
7) after step 6), will obtain PTC ceramic material and carry out resistance temperature curve measurement, the performance of resulting ceramic material: Tc(Curie point)=150 ℃; R 25=3.5k Ω; Lg (R max/ R min)=3.25.
Embodiment 2
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 350r/min respectively in mixture A and mixture B, after ball milling, filter and remove ballstone, then at 90 ℃, dry;
2), after step 1), mixture A is incubated at 930 ℃ to the synthetic K of 3h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 2h at 1130 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and SiO 2according to formula Ba 1-x(K 0.5bi 0.5) xtiO 3+ ySiO 2prepare burden and obtain mixture C, x=0.07 wherein, y=0.05, to adding after a certain amount of deionized water ball milling 4h under the rotating speed of 350r/min in mixture C, after ball milling, filter and remove ballstone, then at 100 ℃, through 4 hours, dry, after oven dry, add a certain amount of PVA granulation, moulding to obtain idiosome, idiosome is wafer type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) by idiosome in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen (volume fraction of oxygen is 3%), be incubated 1h at 1000 ℃ and reoxidize, so that grain boundary oxidation and form crystal boundary potential barrier and obtain high-Curie-point lead-free PTC ceramic material;
6) two sides of lead-free PTC ceramic material is polished, be coated with In-Ga alloy as electrode;
7) after step 6), will obtain PTC ceramic material and carry out resistance temperature curve measurement, the performance of resulting ceramic material: Tc=170 ℃; R 25=2.5k Ω; Lg (R max/ R min)=3.10.
Embodiment 3
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 500r/min respectively in mixture A and mixture B, after ball milling, filter and remove ballstone, then at 100 ℃, dry;
2), after step 1), mixture A is incubated at 950 ℃ to the synthetic K of 2h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 3h at 1150 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and SiO 2according to formula Ba 1-x(K 0.5bi 0.5) xtiO 3+ ySiO 2prepare burden and obtain mixture C, x=0.10 wherein, y=0.05, to adding after a certain amount of deionized water ball milling 4h under the rotating speed of 500r/min in mixture C, after ball milling, filter and remove ballstone, then at 90 ℃, through 5 hours, dry, after oven dry, add a certain amount of PVA granulation, moulding to obtain idiosome, idiosome is wafer type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) by idiosome in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen (volume fraction of oxygen is 4%), be incubated 1h at 1100 ℃ and reoxidize, so that grain boundary oxidation and form crystal boundary potential barrier and obtain high-Curie-point lead-free PTC ceramic material;
6) two sides of lead-free PTC ceramic material is polished, be coated with In-Ga alloy as electrode;
7) after step 6), will obtain PTC ceramic material and carry out resistance temperature curve measurement, the performance of resulting ceramic material: Tc=178 ℃; R 25=2.9k Ω; Lg (R max/ R min)=3.15.
Embodiment 4
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 450r/min respectively in mixture A and mixture B, after ball milling, filter and remove ballstone, then at 90 ℃, dry;
2), after step 1), mixture A is incubated at 900 ℃ to the synthetic K of 3h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 2h at 1120 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and SiO 2according to formula Ba 1-x(K 0.5bi 0.5) xtiO 3+ ySiO 2prepare burden and obtain mixture C, x=0.13 wherein, y=0.05, to adding after a certain amount of deionized water ball milling 4h under the rotating speed of 450r/min in mixture C, after ball milling, filter and remove ballstone, then at 90 ℃, through 5 hours, dry, after oven dry, add a certain amount of PVA granulation, moulding to obtain idiosome, idiosome is wafer type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) by idiosome in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen (volume fraction of oxygen is 0.5%), be incubated 2h at 800 ℃ and reoxidize, so that grain boundary oxidation and form crystal boundary potential barrier and obtain high-Curie-point lead-free PTC ceramic material;
6) two sides of lead-free PTC ceramic material is polished, be coated with In-Ga alloy as electrode;
7) after step 6), will obtain PTC ceramic material and carry out resistance temperature curve measurement, the performance of resulting ceramic material: Tc=201 ℃; R 25=2.8k Ω; Lg (R max/ R min)=3.30.
Embodiment 5
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 450r/min respectively in mixture A and mixture B, after ball milling, filter and remove ballstone, then at 90 ℃, dry;
2), after step 1), mixture A is incubated at 900 ℃ to the synthetic K of 3h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 2h at 1140 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and SiO 2according to formula Ba 1-x(K 0.5bi 0.5) xtiO 3+ ySiO 2prepare burden and obtain mixture C, x=0.25 wherein, y=0.02, to adding after a certain amount of deionized water ball milling 4h under the rotating speed of 450r/min in mixture C, after ball milling, filter and remove ballstone, then at 90 ℃, through 5 hours, dry, after oven dry, add a certain amount of PVA granulation, moulding to obtain idiosome, idiosome is wafer type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) by idiosome in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen (volume fraction of oxygen is 0.5%), be incubated 2h at 800 ℃ and reoxidize, so that grain boundary oxidation and form crystal boundary potential barrier and obtain high-Curie-point lead-free PTC ceramic material;
6) two sides of lead-free PTC ceramic material is polished, be coated with In-Ga alloy as electrode;
7) after step 6), will obtain PTC ceramic material and carry out resistance temperature curve measurement, the performance of resulting ceramic material: Tc=211 ℃; R 25=2.9k Ω; Lg (R max/ R min)=3.20.
In embodiment 1-5, in ball milling, the usage ratio of deionized water, ballstone is:
Material: ball: water=1:(1 ~ 1.4): (0.8 ~ 1.2) this ratio can change as one sees fit, very faint on the impact of final result.

Claims (1)

1. a preparation method for high-Curie-point lead-free PTC ceramic material, is characterized in that: comprise the following steps:
1) first by K 2cO 3, Bi 2o 3and TiO 2according to K 2cO 3: Bi 2o 3: TiO 2the mixed in molar ratio of=1:1:4 obtains mixture A, then by BaCO 3and TiO 2according to the mixed in molar ratio of 1:1, obtain mixture B, to adding after deionized water ball milling 4h under the rotating speed of 350-500r/min respectively in mixture A and mixture B, after ball milling, at 80-100 ℃, dry;
2), after step 1), mixture A is incubated at 900-950 ℃ to the synthetic K of 2-3h 0.5bi 0.5tiO 3powder is incubated mixture B the synthetic BaTiO of 2-3h at 1100-1150 ℃ 3powder;
3) by K 0.5bi 0.5tiO 3powder, BaTiO 3powder and M are according to the mixture C of preparing burden to obtain of formula below:
Ba 1-x(K 0.5Bi 0.5) xTiO 3+yM
0.05≤x≤0.3 wherein, 0≤y≤0.05, described M is one or several the mixture containing in the oxide of Si, Al, Ti or Mn, to adding after deionized water ball milling 4h under the rotating speed of 350-500r/min in mixture C, after ball milling, at 80-100 ℃, dry, then granulation, moulding obtain base substrate;
4) by base substrate in passing into the atmosphere furnace of argon gas in 1300 ℃ of insulation 2h, obtain the ceramics sample of semiconducting;
5) by the ceramics sample of semiconducting in being mixed with the argon gas of trace oxygen, be incubated 1-2h at 800-1100 ℃, obtain high-Curie-point lead-free PTC ceramic material, described in be mixed with oxygen in the argon gas of trace oxygen volume fraction be 0.5-4%.
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CN1814570A (en) * 2005-02-01 2006-08-09 四川大学 Bi.Na.K.Li Ag titanate series lead-free piezoelectric ceramics
CN101213155A (en) * 2005-04-28 2008-07-02 日立金属株式会社 Semiconductor porcelain composition and method of producing the same
CN101276659A (en) * 2007-03-26 2008-10-01 太阳诱电株式会社 Dielectric ceramics and multi-layer ceramic capacitor
CN102177105A (en) * 2008-10-16 2011-09-07 韩国Ceramic技术院 Lead free ceramic composition for PTC thermistor and PTC ceramic thermistor thereby

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CN85100513A (en) * 1985-04-01 1986-08-13 中国科学院上海硅酸盐研究所 Bi-Na-Ba-TiO 3 series piezoelectric ceramic material for ultrasonic devices
CN1814570A (en) * 2005-02-01 2006-08-09 四川大学 Bi.Na.K.Li Ag titanate series lead-free piezoelectric ceramics
CN101213155A (en) * 2005-04-28 2008-07-02 日立金属株式会社 Semiconductor porcelain composition and method of producing the same
CN101276659A (en) * 2007-03-26 2008-10-01 太阳诱电株式会社 Dielectric ceramics and multi-layer ceramic capacitor
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Correct: Yancheng Qingdun Jinbang Water Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8)

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