CN102976747A - Lithium niobate doped barium titanate based positive temperature coefficient resistance material and preparation method thereof - Google Patents
Lithium niobate doped barium titanate based positive temperature coefficient resistance material and preparation method thereof Download PDFInfo
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- CN102976747A CN102976747A CN2012105496339A CN201210549633A CN102976747A CN 102976747 A CN102976747 A CN 102976747A CN 2012105496339 A CN2012105496339 A CN 2012105496339A CN 201210549633 A CN201210549633 A CN 201210549633A CN 102976747 A CN102976747 A CN 102976747A
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Abstract
The invention discloses a lithium niobate doped barium titanate based positive temperature coefficient resistance material and a preparation method thereof. The chemical composition general formula of the barium titanate based positive temperature coefficient resistance material is as follows: Ba[1-x]LixTi[1-x]NbxO3, wherein x is more than 0 and not more than 0.08, and x is a molar fraction. The preparation method comprises the following steps: (1) weighing and preparing original BaCO3, TiO2, Li2CO3 and Nb2O5 powders with the purity of above 99.9% according to Ba[1-x]LixTi[1-x]NbxO3, wherein x is more than 0 and not more than 0.08 and x is the molar fraction; and (2) performing ball milling on the prepared ball material in the step (1) for 4 hours, pre-burning at the temperature of 1000-1100 DEG C for 2 hours, further performing ball milling for 3 hours, granulating, tabletting, dispensing glue, calcining at the temperature of 1150-1250 DEG C for 3 hours and loading an electrode to prepare the lithium niobate doped barium titanate based positive temperature coefficient resistance material. The barium titanate based positive temperature coefficient resistance material disclosed by the invention can achieve the practical level from the two aspects of ingredients and process and is suitable for industrial large-scale production; and the prepared resistance material is lead-free, thereby avoiding the harm to physical health of people and the environmental pollution.
Description
Technical field
The present invention relates to barium titanate-based positive temperature coefficient resistance material of a kind of doped lithium columbate and preparation method thereof, belong to the thermo-sensitive material field.
Background technology
PTC pottery (positive temperature coefficient thermal sensitive ceramic) has the advantages that resistivity raises and increases with temperature.It is rapidly one of electronic material of development in recent years.Posistor can be divided into switching mode and offset-type two large classes, and its characteristic and application is also different.Switching mode positive temperature coefficient thermo-sensitive material is mainly used in the protection etc. of the rectifier cell of motor, transformer, bearing, high-power silicon, and it also is applied to the aspects such as current limliting, current stabilization, voltage stabilizing and velocity measurement as the hear rate element.Offset-type positive temperature coefficient thermo-sensitive material can be used as the temperature compensation of transistor.
The barium titanate-based positive temperature coefficient thermo-sensitive material is a kind of Ferro-Electric Semiconductor material, is rapidly one of electronic material of development in recent years.But the Curie temperature of barium titanate only has 120 ℃, and the PTC thermo-sensitive material of Curie temperature above 120 ℃ all is leaded in the market.Improving barium titanate positive temperature coefficient transition temperature both at home and abroad mainly is to realize by adding lead element.Although this kind method and technology is ripe and obtained preferably effect, lead has very strong toxicity.Products containing lead is from being prepared into use and even all having very strong harm to last recycling use.Begun in 2006 in the world to completely forbid to use plumbous piezo component has been arranged.In recent years, along with the demand of environment protection and human kind sustainable development, research novel lead-free PTC resistive material is extremely urgent.Nowadays unleaded positive temperature coefficient thermo-sensitive material mainly is macromolecular material, but because the hot mastication of macromolecular material has limited its use range greatly.So seeking unleaded high-curie temperature positive temperature coefficient thermo-sensitive material tool has very important significance.There are a lot of Chinese patents to report environment-friendly type positive temperature coefficient thermo-sensitive material, such as (Ba
xSr
yCa
z) Ti
uO
3, wherein, x:0.6~0.9, y:0~0.3, z:0.02~0.2, u:0.98~1.02; : (Bi
1/2K
1/2-a/2Na
A/2) Ce
1-bDbO
3, a=0~1 wherein, b=0.0005~0.005 etc., but Curie temperature not high (being lower than 160 ℃).Tang Xingui etc. have reported BaTiO
3-Bi
0.5Na
0.5TiO
3-Bi
0.5K
0.5TiO
3Be the positive temperature coefficient thermo-sensitive material, its Integrated using sol-gel method, solid reaction process, discharge plasma sintering method prepares by one or more metal oxides that mix, but the highest Curie temperature also is no more than 250 ℃.We only utilize conventional solid-state method take barium carbonate, titanium dioxide, Quilonum Retard, Niobium Pentxoxide as raw material, the positive temperature coefficient thermo-sensitive material of preparation high-curie temperature.
Summary of the invention
The objective of the invention is provides barium titanate-based positive temperature coefficient resistance material of a kind of doped lithium columbate and preparation method thereof in order to improve the low problem of barium titanate-based positive temperature coefficient resistance material Curie temperature.
The chemical constitution general formula of the barium titanate-based positive temperature coefficient resistance material of the doped lithium columbate that the present invention relates to is: Ba
1-xLi
xTi
1-xNb
xO
3, wherein: 0<x≤0.08; X is molar fraction.
Preparation method's concrete steps of the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate are:
(1) with purity is BaCO more than 99.9%
3, TiO
2, Li
2CO
3And Nb
2O
5Starting powder press Ba
1-xLi
xTi
1-xNb
xO
3Form weigh batching, wherein: 0<x≤0.08; X is molar fraction.
(2) pellet that step (1) prepared mill 4 hours, 1000~1100 ℃ of pre-burnings 2 hours, ball milling is 3 hours again, granulation, compressing tablet, binder removal, 1150~1250 ℃ of calcinings 3 hours, top electrode namely makes the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate.
The barium titanate-based positive temperature coefficient resistance material of the doped lithium columbate of the present invention's preparation has the following advantages: composition is unleaded, can not work the mischief to environment with to human body; Mixed behind the Lithium niobium trioxide, even trace doped, also can greatly improve the Curie temperature of component.
Embodiment
Embodiment 1:
Be 99.9% BaCO with purity
3, TiO
2, Li
2CO
3And Nb
2O
5Starting powder, press x=0.02, i.e. Ba
0.98Li
0.02Ti
0.98Nb
0.02O
3Weigh batching; The material that then will prepare is with planetary mills ball milling 4 hours, 1100 ℃ of pre-burnings 2 hours, and ball milling is 3 hours again, granulation, compressing tablet, binder removal, 1250 ℃ of calcinings 3 hours, top electrode is prepared the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate; Prepared product is carried out performance test, its Curie temperature T
c200 ℃ of ≈, resistivity is 10 Ω m, temperature factor is 8%/℃, maximum resistance rate/lowest resistivity (liftdrag) is greater than 9 * 10
3
Embodiment 2:
Be 99.9% BaCO with purity
3, TiO
2, Li
2CO
3And Nb
2O
5Starting powder, press x=0.04, i.e. Ba
0.96Li
0.04Ti
0.96Nb
0.04O
3Weigh batching; With the material for preparing with planetary mills ball milling 4 hours, 1060 ℃ of pre-burnings 2 hours, ball milling is 3 hours again, granulation, compressing tablet, binder removal, 1200 ℃ of calcinings 3 hours, top electrode is prepared the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate; Prepared product is carried out performance test, its Curie temperature T
c240 ℃ of ≈, resistivity is 8 Ω m, temperature factor is 12%/℃, maximum resistance rate/lowest resistivity (liftdrag) is greater than 10
4
Embodiment 3:
Be 99.9% BaCO with purity
3, TiO
2, Li
2CO
3And Nb
2O
5Starting powder, press x=0.06, i.e. Ba
0.94Li
0.06Ti
0.94Nb
0.06O
3Weigh batching; With the material for preparing with planetary mills ball milling 4 hours, 1040 ℃ of pre-burnings 2 hours, ball milling is 3 hours again, granulation, compressing tablet, binder removal, 1180 ℃ of calcinings 3 hours, top electrode is prepared the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate; Prepared product is carried out performance test, its Curie temperature T
c300 ℃ of ≈, resistivity is 6 Ω m, temperature factor is 16%/℃, maximum resistance rate/lowest resistivity (liftdrag) is greater than 6 * 10
3
Embodiment 4:
Be 99.9% BaCO with purity
3, TiO
2, Li
2CO
3And Nb
2O
5Starting powder, press x=0.08, i.e. Ba
0.92Li
0.08Ti
0.92Nb
0.08O
3Weigh batching; With the material for preparing with planetary mills ball milling 4 hours, 1000 ℃ of pre-burnings 2 hours, ball milling is 3 hours again, granulation, compressing tablet, binder removal, 1150 ℃ of calcinings 3 hours, top electrode is prepared the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate; Prepared product is carried out performance test, its Curie temperature T
c350 ℃ of ≈, resistivity is 12 Ω m, temperature factor is 12%/℃, maximum resistance rate/lowest resistivity (liftdrag) is greater than 1.4 * 10
4
Claims (2)
1. the barium titanate-based positive temperature coefficient resistance material of a doped lithium columbate is characterized in that the chemical constitution general formula of described resistive material is: Ba
1-xLi
xTi
1-xNb
xO
3, wherein: 0<x≤0.08, x is molar fraction.
2. the preparation method of the barium titanate-based positive temperature coefficient resistance material of described doped lithium columbate according to claim 1 is characterized in that concrete steps are:
(1) with purity is BaCO more than 99.9%
3, TiO
2, Li
2CO
3And Nb
2O
5Starting powder press Ba
1-xLi
xTi
1-xNb
xO
3Form weigh batching, wherein: 0<x≤0.08; X is molar fraction;
(2) pellet that step (1) prepared mill 4 hours, 1000~1100 ℃ of pre-burnings 2 hours, ball milling is 3 hours again, granulation, compressing tablet, binder removal, 1150~1250 ℃ of calcinings 3 hours, top electrode namely makes the barium titanate-based positive temperature coefficient resistance material of doped lithium columbate.
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Cited By (8)
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---|---|---|---|---|
CN105036742A (en) * | 2015-09-10 | 2015-11-11 | 桂林理工大学 | High-curie-point positive-temperature-coefficient resistance material Ba3Li3Bi2Nb5O20 and preparation method thereof |
CN105236970A (en) * | 2015-09-28 | 2016-01-13 | 桂林理工大学 | High Curie point positive temperature coefficient resistor material Ba5LiTiNb3O15and preparation method thereof |
CN105272237A (en) * | 2015-09-28 | 2016-01-27 | 桂林理工大学 | High-Curie point positive temperature coefficient resistor material Li3BaTiNbO7 and preparation method thereof |
CN105272236A (en) * | 2015-09-20 | 2016-01-27 | 桂林理工大学 | High Curie point positive temperature coefficient resistance material Ba2Li3Bi2Nb5O19 and preparation method |
CN108863080A (en) * | 2018-08-10 | 2018-11-23 | 江西正强电瓷电器有限公司 | The preparation method of the porcelain insulator glaze of positive temperature coefficient |
CN111704461A (en) * | 2020-05-22 | 2020-09-25 | 江苏波速传感器有限公司 | Formula and preparation method of high Curie point low temperature co-fired piezoelectric ceramic |
CN113582685A (en) * | 2021-08-05 | 2021-11-02 | 湖南省美程陶瓷科技有限公司 | Lead-free piezoelectric ceramic material for breathing machine and preparation method thereof |
CN113651612A (en) * | 2021-08-13 | 2021-11-16 | 湖州南木纳米科技有限公司 | Barium titanate PTC thermal sensitive ceramic material and application thereof in lithium battery |
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Cited By (10)
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CN105036742A (en) * | 2015-09-10 | 2015-11-11 | 桂林理工大学 | High-curie-point positive-temperature-coefficient resistance material Ba3Li3Bi2Nb5O20 and preparation method thereof |
CN105272236A (en) * | 2015-09-20 | 2016-01-27 | 桂林理工大学 | High Curie point positive temperature coefficient resistance material Ba2Li3Bi2Nb5O19 and preparation method |
CN105236970A (en) * | 2015-09-28 | 2016-01-13 | 桂林理工大学 | High Curie point positive temperature coefficient resistor material Ba5LiTiNb3O15and preparation method thereof |
CN105272237A (en) * | 2015-09-28 | 2016-01-27 | 桂林理工大学 | High-Curie point positive temperature coefficient resistor material Li3BaTiNbO7 and preparation method thereof |
CN108863080A (en) * | 2018-08-10 | 2018-11-23 | 江西正强电瓷电器有限公司 | The preparation method of the porcelain insulator glaze of positive temperature coefficient |
CN108863080B (en) * | 2018-08-10 | 2021-04-16 | 江西正强电瓷电器有限公司 | Preparation method of porcelain insulator glaze with positive temperature coefficient |
CN111704461A (en) * | 2020-05-22 | 2020-09-25 | 江苏波速传感器有限公司 | Formula and preparation method of high Curie point low temperature co-fired piezoelectric ceramic |
CN113582685A (en) * | 2021-08-05 | 2021-11-02 | 湖南省美程陶瓷科技有限公司 | Lead-free piezoelectric ceramic material for breathing machine and preparation method thereof |
CN113582685B (en) * | 2021-08-05 | 2022-07-15 | 湖南省美程陶瓷科技有限公司 | Lead-free piezoelectric ceramic material for breathing machine and preparation method thereof |
CN113651612A (en) * | 2021-08-13 | 2021-11-16 | 湖州南木纳米科技有限公司 | Barium titanate PTC thermal sensitive ceramic material and application thereof in lithium battery |
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Application publication date: 20130320 |