CN102745987A - High-curie-point lead-free PTC (Positive Temperature Coefficient) thermal sensitive ceramic material and preparation method thereof - Google Patents

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

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CN102745987A
CN102745987A CN2012102614901A CN201210261490A CN102745987A CN 102745987 A CN102745987 A CN 102745987A CN 2012102614901 A CN2012102614901 A CN 2012102614901A CN 201210261490 A CN201210261490 A CN 201210261490A CN 102745987 A CN102745987 A CN 102745987A
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ceramic material
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CN102745987B (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) thermal sensitive ceramic material and a preparation method of the ceramic material. The main component of the material is ba1-x(Na0.5Bi0.5)xTiO3+yNa2TiO3+zM, wherein x is more than or equal to 0.08 and less than or equal to 0.3, y is more than or equal to 0.01 and less than or equal to 0.10, z is more than or equal to 0.001 and less than or equal to 0.005, and M is a semiconducting element. The high-curie-point PTC thermal sensitive ceramic material provided by the invention does not contain lead, and the damages to the human bodies and the environment of resistor devices in the manufacturing and using processes are avoided; a doping process of trace semiconducting elements is adopted, so the semiconducting problem of the PTC thermal sensitive material at the room temperature is solved; and the PTC thermal sensitive materials with different curie points can be prepared through controlling the doping quantities of NBT (NaBiTiO) and NT (NaTiO).

Description

A kind of high curie point lead-free PTC thermal sensitive ceramic material and preparation method thereof
Technical field
The present invention relates to a kind of semiconductor material, particularly a kind ofly meet Na unleaded, low-resistance 2Ti 6O 13(NT)-Na 0.5Bi 0.5TiO 3(NBT)-BaTiO 3(BT) system's 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) stupalith is a kind of Ferro-Electric Semiconductor material, is development in recent years one of novel electron material rapidly.Because the PTCR stupalith has " switch " function automatically such as temperature sensitive, current limliting, time-delay, has been widely used in every field such as telecommunications, aerospace, automotive industry, household electrical appliance.
Yet, but the piezoelectricity of current practicability and ferroelectric material mainly are with the mobile agent of Pb as Curie temperature, realize with the crystallographic site of Pb displacement Ba.This series products is because its satisfactory stability property, repeatability and higher Curie temperature have obtained application widely.But contain the Pb oxide compound inevitably because a variety of causes flows into living environment and physical environment, thereby human body and physical 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.
It is that bismuth-containing compound substitutes the mobile agent of Pb as Curie temperature that present various countries researchist studies maximum systems; And NBT is one of mobile agent of the maximum bismuth-containing Curie temperature of research, but does not also have a kind of ptc material of NBT-BT system of effective raising Curie temperature at present.
Summary of the invention
The object of the present invention is to provide a kind of high curie point lead-free PTC thermal sensitive ceramic material and preparation method thereof.
For achieving the above object, the present invention has adopted following technical scheme.
A kind of high curie point lead-free PTC thermal sensitive ceramic material, this stupalith comprises following component:
Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM, 0.08≤x≤0.3,0.01≤y≤0.10,0.001≤z≤0.005 wherein, M is the oxide compound of semiconductor element.
The preparation method of above-mentioned high curie point lead-free PTC stupalith may further comprise the steps:
1) at first with Na 2CO 3, Bi 2O 3And TiO 2According to Na 2CO 3: Bi 2O 3: TiO 2=1: 1: 4 mixed in molar ratio gets mixture A, then with BaCO 3And TiO 2Get mixture B according to 1: 1 mixed in molar ratio, again with Na 2CO 3, TiO 2With NaCl according to Na 2CO 3: TiO 2: NaCl=1: 6: 2 mixed in molar ratio gets mixture C, in mixture A, mixture B and mixture C, adds behind the deionized water ball milling 4h under the rotating speed of 350-500r/min respectively, behind the ball milling 80-100 ℃ of oven dry down;
2), mixture A is incubated the synthetic Na of 2-3h down at 800-850 ℃ through after the step 1) 0.5Bi 0.5TiO 3Powder is incubated the synthetic BaTiO of 2-3h with mixture B down at 1100-1150 ℃ 3Powder is incubated 8-12h with mixture C down at 950-1100 ℃, insulation postcooling to room temperature, and the NaCl that rinses out then in the product obtains Na 2Ti 6O 13Powder;
3) with Na 0.5Bi 0.5TiO 3Powder, BaTiO 3Powder, Na 2Ti 6O 13Powder and M according to following prescription prepare burden mixture D:
Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM, wherein 0.08≤x≤0.3,0.01≤y≤0.10; 0.001≤z≤0.005, M is the oxide compound of semiconductor element, in mixture D, adds behind the deionized water ball milling 4h under the rotating speed of 350-500r/min; 80-100 ℃ of oven dry down, granulation then, moulding get idiosome behind the ball milling;
4) idiosome is carried out sintering in box-type furnace; During sintering;, room temperature is incubated 0.5h after being warmed up to 500 ℃ with the speed of 3 ℃/min; And then be incubated 1-3h after being warmed up to 1250-1320 ℃ with the speed of 3 ℃/min, again with the speed cool to room temperature of 3 ℃/min, promptly obtain high curie point lead-free PTC thermal sensitive ceramic material.
Said M is one or several the mixture that contains in the oxide compound of trivalent or pentavalent rare earth trace semiconductor element.
Said trivalent or pentavalent rare earth trace semiconductor element are La, Nb, Sb or Dy.
The high curie point lead-free PTC thermal sensitive ceramic material that the present invention prepares can reach following parameter request: Tc (Curie temperature)=165-250 ℃ through the resistive material Characteristics Detection; R 25≤2.5k Ω; Lg (R Max/ R Min)>=3.0; Characteristics Detection adopts the In-Ga alloy as electrode, records the room temperature resistance and the resistance-temperature curve of components and parts.Can select other electrode materialss (like aluminium electrode, nickel electrode etc.) in the actual production for use.
The preparation method of high curie point lead-free PTC thermal sensitive ceramic material according to the invention has the following advantages: 1. adopt conventional solid-state method to prepare powder, particle does not have reunion, fillibility is good, cost is low, output is big, preparation technology is simple, easy control of reaction conditions.2. through NBT the high density (8% ~ 30%) of BT is mixed to realize the raising of Curie temperature.3. through the introducing of NT, utilize the formed liquid phase acceleration of sintering of Ti among the NT on the one hand, avoid the introducing of sintering aid; Utilize the high temperature iron of NT electrical on the other hand, Curie temperature is further improved.4. the high curie point PTC thermal sensitive ceramic material of the present invention's preparation is not leaded, has avoided resistance element in manufacturing and use, human body and environment to be produced harm.Adopt the doping process of micro-semiconductor element, solved PTC thermo-sensitive material semiconductor problem at room temperature.And can be through to the control of dopings such as NBT, NT, with the preparation of the PTC thermo-sensitive material of realizing different Curie temperatures.The preparation method of high curie point lead-free PTC thermal sensitive ceramic material 5. according to the invention can obtain high-purity phase composite, stable performance, safety highland high curie point PTC thermistor; The doping scope of NBT is wide in the prescription of principal constituent; Can adjust accordingly according to production technique in the actual application, handiness is big.
Description of drawings
Fig. 1 is the resistance-temperature characteristics curve of the stupalith for preparing of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further.
Embodiment 1
1) at first with Na 2CO 3, Bi 2O 3And TiO 2According to Na 2CO 3: Bi 2O 3: TiO 2=1: 1: 4 mixed in molar ratio gets mixture A, then with BaCO 3And TiO 2Get mixture B according to 1: 1 mixed in molar ratio, again with Na 2CO 3, TiO 2With NaCl according to Na 2CO 3: TiO 2: NaCl=1: 6: 2 mixed in molar ratio gets mixture C, in mixture A, mixture B and mixture C, adds behind the deionized water ball milling 4h under the rotating speed of 400r/min respectively, and the ball milling after-filtration is removed ballstone, then 90 ℃ of oven dry down;
2), mixture A is incubated the synthetic Na of 2h down at 825 ℃ through after the step 1) 0.5Bi 0.5TiO 3Powder is incubated the synthetic BaTiO of 3h with mixture B down at 1125 ℃ 3Powder is incubated 8h with mixture C down at 1000 ℃, insulation postcooling to room temperature, and the NaCl that rinses out then in the product obtains Na 2Ti 6O 13Powder;
3) with Na 0.5Bi 0.5TiO 3Powder, BaTiO 3Powder, Na 2Ti 6O 13Powder and M are according to prescription Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM prepare burden mixture D, x=0.08 wherein, y=0.02, z=0.002, M are Nb 2O 5In mixture D, add behind the deionized water ball milling 4h under the rotating speed of 400r/min, the ball milling after-filtration is removed ballstone, then 90 ℃ down through 5h dry powder; A certain amount of PVA granulation of adding, moulding get idiosome in powder; Idiosome is the disk type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) idiosome is carried out sintering in box-type furnace; During sintering;, room temperature is incubated 0.5h after being warmed up to 500 ℃ with the speed of 3 ℃/min; And then be incubated 1h after being warmed up to 1300 ℃ with the speed of 3 ℃/min, again with the speed cool to room temperature of 3 ℃/min, promptly obtain high curie point lead-free PTC thermal sensitive ceramic material.
5) two sides with the lead-free PTC thermal sensitive ceramic material polishes, and is coated with the In-Ga alloy as electrode;
6) the lead-free PTC thermal sensitive ceramic material be will obtain after the step 5) and resistance temperature curve measurement, the performance of resulting stupalith: Tc=172 ℃ carried out; R 25=2.35k Ω; Lg (R Max/ R Min)=3.25 (shown in (a) among Fig. 1).
Embodiment 2
1) at first with Na 2CO 3, Bi 2O 3And TiO 2According to Na 2CO 3: Bi 2O 3: TiO 2=1: 1: 4 mixed in molar ratio gets mixture A, then with BaCO 3And TiO 2Get mixture B according to 1: 1 mixed in molar ratio, again with Na 2CO 3, TiO 2With NaCl according to Na 2CO 3: TiO 2: NaCl=1: 6: 2 mixed in molar ratio gets mixture C, in mixture A, mixture B and mixture C, adds behind the deionized water ball milling 4h under the rotating speed of 450r/min respectively, and the ball milling after-filtration is removed ballstone, then 95 ℃ of oven dry down;
2), mixture A is incubated the synthetic Na of 3h down at 830 ℃ through after the step 1) 0.5Bi 0.5TiO 3Powder is incubated the synthetic BaTiO of 2h with mixture B down at 1100 ℃ 3Powder is incubated 10h with mixture C down at 1100 ℃, insulation postcooling to room temperature, and the NaCl that rinses out then in the product obtains Na 2Ti 6O 13Powder;
3) with Na 0.5Bi 0.5TiO 3Powder, BaTiO 3Powder, Na 2Ti 6O 13Powder and M are according to prescription Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM prepare burden mixture D, x=0.10 wherein, y=0.02, z=0.003, M are Nb 2O 5In mixture D, add behind the deionized water ball milling 4h under the rotating speed of 450r/min, the ball milling after-filtration is removed ballstone, then 100 ℃ down through 4h dry powder; A certain amount of PVA granulation of adding, moulding get idiosome in powder; Idiosome is the disk type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) idiosome is carried out sintering in box-type furnace; During sintering;, room temperature is incubated 0.5h after being warmed up to 500 ℃ with the speed of 3 ℃/min; And then be incubated 2h after being warmed up to 1280 ℃ with the speed of 3 ℃/min, again with the speed cool to room temperature of 3 ℃/min, promptly obtain high curie point lead-free PTC thermal sensitive ceramic material.
5) two sides with the lead-free PTC thermal sensitive ceramic material polishes, and is coated with the In-Ga alloy as electrode;
6) the lead-free PTC thermal sensitive ceramic material be will obtain after the step 5) and resistance temperature curve measurement, the performance of resulting stupalith: Tc=187 ℃ carried out; R 25=2.2k Ω; Lg (R Max/ R Min)=3.0 (shown in (b) among Fig. 1).
Embodiment 3
1) at first with Na 2CO 3, Bi 2O 3And TiO 2According to Na 2CO 3: Bi 2O 3: TiO 2=1: 1: 4 mixed in molar ratio gets mixture A, then with BaCO 3And TiO 2Get mixture B according to 1: 1 mixed in molar ratio, again with Na 2CO 3, TiO 2With NaCl according to Na 2CO 3: TiO 2: NaCl=1: 6: 2 mixed in molar ratio gets mixture C, in mixture A, mixture B and mixture C, adds behind the deionized water ball milling 4h under the rotating speed of 350r/min respectively, and the ball milling after-filtration is removed ballstone, then 100 ℃ of oven dry down;
2), mixture A is incubated the synthetic Na of 3h down at 800 ℃ through after the step 1) 0.5Bi 0.5TiO 3Powder is incubated the synthetic BaTiO of 2h with mixture B down at 1150 ℃ 3Powder is incubated 11h with mixture C down at 950 ℃, insulation postcooling to room temperature, and the NaCl that rinses out then in the product obtains Na 2Ti 6O 13Powder;
3) with Na 0.5Bi 0.5TiO 3Powder, BaTiO 3Powder, Na 2Ti 6O 13Powder and M are according to prescription Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM prepare burden mixture D, x=0.15 wherein, y=0.03, z=0.003, M are La 2O 3In mixture D, add behind the deionized water ball milling 4h under the rotating speed of 350r/min, the ball milling after-filtration is removed ballstone, then 80 ℃ down through 6h dry powder; A certain amount of PVA granulation of adding, moulding get idiosome in powder; Idiosome is the disk type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) idiosome is carried out sintering in box-type furnace; During sintering;, room temperature is incubated 0.5h after being warmed up to 500 ℃ with the speed of 3 ℃/min; And then be incubated 3h after being warmed up to 1320 ℃ with the speed of 3 ℃/min, again with the speed cool to room temperature of 3 ℃/min, promptly obtain high curie point lead-free PTC thermal sensitive ceramic material.
5) two sides with the lead-free PTC thermal sensitive ceramic material polishes, and is coated with the In-Ga alloy as electrode;
6) the lead-free PTC thermal sensitive ceramic material be will obtain after the step 5) and resistance temperature curve measurement, the performance of resulting stupalith: Tc=204 ℃ carried out; R 25=1.67k Ω; Lg (R Max/ R Min)=3.15 (shown in (c) among Fig. 1).
Embodiment 4
1) at first with Na 2CO 3, Bi 2O 3And TiO 2According to Na 2CO 3: Bi 2O 3: TiO 2=1: 1: 4 mixed in molar ratio gets mixture A, then with BaCO 3And TiO 2Get mixture B according to 1: 1 mixed in molar ratio, again with Na 2CO 3, TiO 2With NaCl according to Na 2CO 3: TiO 2: NaCl=1: 6: 2 mixed in molar ratio gets mixture C, in mixture A, mixture B and mixture C, adds behind the deionized water ball milling 4h under the rotating speed of 500r/min respectively, and the ball milling after-filtration is removed ballstone, then 80 ℃ of oven dry down;
2), mixture A is incubated the synthetic Na of 3h down at 850 ℃ through after the step 1) 0.5Bi 0.5TiO 3Powder is incubated the synthetic BaTiO of 3h with mixture B down at 1120 ℃ 3Powder is incubated 12h with mixture C down at 980 ℃, insulation postcooling to room temperature, and the NaCl that rinses out then in the product obtains Na 2Ti 6O 13Powder;
3) with Na 0.5Bi 0.5TiO 3Powder, BaTiO 3Powder, Na 2Ti 6O 13Powder and M are according to prescription Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM prepare burden mixture D, x=0.25 wherein, y=0.05, z=0.003, M are La 2O 3In mixture D, add behind the deionized water ball milling 4h under the rotating speed of 500r/min, the ball milling after-filtration is removed ballstone, then 95 ℃ down through 5h dry powder; A certain amount of PVA granulation of adding, moulding get idiosome in powder; Idiosome is the disk type, and the diameter of disk is 12mm, and thickness is 3.5-4.0mm;
4) idiosome is carried out sintering in box-type furnace; During sintering;, room temperature is incubated 0.5h after being warmed up to 500 ℃ with the speed of 3 ℃/min; And then be incubated 1h after being warmed up to 1250 ℃ with the speed of 3 ℃/min, again with the speed cool to room temperature of 3 ℃/min, promptly obtain high curie point lead-free PTC thermal sensitive ceramic material.
5) two sides with the lead-free PTC thermal sensitive ceramic material polishes, and is coated with the In-Ga alloy as electrode;
6) the lead-free PTC thermal sensitive ceramic material be will obtain after the step 5) and resistance temperature curve measurement, the performance of resulting stupalith: Tc=223 ℃ carried out; R 25=2.4k Ω; Lg (R Max/ R Min)=3.80 (shown in (d) among Fig. 1).
Among the embodiment 1-4, the usage ratio of deionized water, ballstone is in the ball milling:
Material: ball: water=1: (1 ~ 1.4): (0.8 ~ 1.2) this ratio can change as one sees fit, and is very faint to final result's influence.

Claims (4)

1. high curie point lead-free PTC thermal sensitive ceramic material, it is characterized in that: this stupalith comprises following component:
Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM, 0.08≤x≤0.3,0.01≤y≤0.10,0.001≤z≤0.005 wherein, M is the oxide compound of semiconductor element.
2. one kind prepares high curie point lead-free PTC method of ceramic material according to claim 1, it is characterized in that: may further comprise the steps:
1) at first with Na 2CO 3, Bi 2O 3And TiO 2According to Na 2CO 3: Bi 2O 3: TiO 2=1: 1: 4 mixed in molar ratio gets mixture A, then with BaCO 3And TiO 2Get mixture B according to 1: 1 mixed in molar ratio, again with Na 2CO 3, TiO 2With NaCl according to Na 2CO 3: TiO 2: NaCl=1: 6: 2 mixed in molar ratio gets mixture C, in mixture A, mixture B and mixture C, adds behind the deionized water ball milling 4h under the rotating speed of 350-500r/min respectively, behind the ball milling 80-100 ℃ of oven dry down;
2), mixture A is incubated the synthetic Na of 2-3h down at 800-850 ℃ through after the step 1) 0.5Bi 0.5TiO 3Powder is incubated the synthetic BaTiO of 2-3h with mixture B down at 1100-1150 ℃ 3Powder is incubated 8-12h with mixture C down at 950-1100 ℃, insulation postcooling to room temperature, and the NaCl that rinses out then in the product obtains Na 2Ti 6O 13Powder;
3) with Na 0.5Bi 0.5TiO 3Powder, BaTiO 3Powder, Na 2Ti 6O 13Powder and M according to following prescription prepare burden mixture D:
Ba 1-x(Na 0.5Bi 0.5) xTiO 3+ yNa 2Ti 6O 13+ zM, wherein 0.08≤x≤0.3,0.01≤y≤0.10; 0.001≤z≤0.005, M is the oxide compound of semiconductor element, in mixture D, adds behind the deionized water ball milling 4h under the rotating speed of 350-500r/min; 80-100 ℃ of oven dry down, granulation then, moulding get idiosome behind the ball milling;
4) idiosome is carried out sintering in box-type furnace; During sintering;, room temperature is incubated 0.5h after being warmed up to 500 ℃ with the speed of 3 ℃/min; And then be incubated 1-3h after being warmed up to 1250-1320 ℃ with the speed of 3 ℃/min, again with the speed cool to room temperature of 3 ℃/min, promptly obtain high curie point lead-free PTC thermal sensitive ceramic material.
3. according to the said a kind of preparation high curie point lead-free PTC method of ceramic material of claim 2, it is characterized in that: said M is one or several the mixture that contains in the oxide compound of trivalent or pentavalent rare earth trace semiconductor element.
4. according to the said a kind of preparation high curie point lead-free PTC method of ceramic material of claim 3, it is characterized in that: said trivalent or pentavalent rare earth trace semiconductor element are La, Nb, Sb or Dy.
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CN109152130A (en) * 2018-08-06 2019-01-04 深圳大图科创技术开发有限公司 It is connected with the LED illumination lamp of temperature sensor

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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)

False: Yancheng Qingyi Jinbang Water Affairs Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8)

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