CN1632886A - Ni/graphite (Ba-[1-x-y],Sr-[x],Pb-[y])TiO-[3] base composite PTC thermistor and preparing method - Google Patents

Ni/graphite (Ba-[1-x-y],Sr-[x],Pb-[y])TiO-[3] base composite PTC thermistor and preparing method Download PDF

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Publication number
CN1632886A
CN1632886A CN 200410094023 CN200410094023A CN1632886A CN 1632886 A CN1632886 A CN 1632886A CN 200410094023 CN200410094023 CN 200410094023 CN 200410094023 A CN200410094023 A CN 200410094023A CN 1632886 A CN1632886 A CN 1632886A
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Prior art keywords
tio
graphite
positive temperature
temperature coefficient
powder
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曲远方
杜娟
方春行
马卫兵
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Tianjin University
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Tianjin University
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Abstract

This invention discloses a compound positive temperature parameters of heat sensitive resistance based on Ba#-[1-x-y], Sr#-[x], Pb#-[y])TiO#-[3] and its process method. The process comprises the following steps: to make the positive temperature heat sensitive ceramics powder based on Ba#-[1-x-y], Sr#-[x], Pb#-[y])TiO#-[3]; to mix the processed ceramics powder with Ni powder and lead powder and to join the PVA solution particles to process crude compact by pressure shaping through dry ball grinding; to sinter the crude compact into ceramics sample under temperature of 1200~1280DEG C; To make the upper and down surfaces of the sample contact the silver or aluminum electrode to make the compound temperature heat sensitive resistance.

Description

Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3Based composite positive temperature coefficient thermistor and preparation method
Technical field
The present invention relates to a kind of Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3Based composite positive temperature coefficient thermistor and preparation method belong to the technology of preparing of ceramic material and components and parts thereof.
Background technology
Add metal or other low-resistance phase material at present and can reduce BaTiO 3The room temperature resistivity of based composite positive temperature coefficient thermistor material, but process conditions complexity, and the PTC poor-performing of the composite material that makes [Ze ming He, Jan Ma, QuYuanfang, Wang chengang.A structural model of Cr/ (Ba, Pb) TiO 3Positive temperaturecoefficient composites[J] .Journal of materials science:Materials in Electronics.2000,11 (3): 235-238; Li Xiaolei, Qu Yuanfang, Xu Tingxian. burn till and Technology for Heating Processing to Ni/PTC ceramic composite Effect on Performance [J]. silicate circular, 2001.3:50 ~ 54].BaTiO 3The resistance lowering of matrix PTC material is a main trend of current development, reduces BaTiO 3The room temperature resistivity of matrix PTC material has become one of important topic of this research field [Gene H, Haertling K.Ferroelectric ceramics:History and Technology[J] .J Am CeramSoc, 1999,82 (4): 797 ~ 818.].Present BaTiO 3The room temperature resistivity of base PTC ceramic material is higher, this seriously limited PTC ceramic material and device under the low-voltage condition from the promotion and application [I-NanLin aspect temperature control heating and the overcurrent protection; Horng-Yi Chan; Kuo-Shung Liu.Microwave sintering of PTCR ceramics and theirelectrical properties[J] .Ferroelectrics Proceedings of the Tenth IEEE InternationalSymposium on Applications of Ferroelectrics.18-21 Aug 1996.Page (s): 987～990 vol2.; S.Urek, M.Drofenik.PTC behavior of highly donor doped BaTiO 3[J] .Journal ofthe European Ceramic Society.1999,19:913 ~ 916].
Summary of the invention
The purpose of this invention is to provide a kind of Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3Based composite positive temperature coefficient thermistor and preparation method, this PTC thermistor not only has better lift-drag ratio performance, also has low room temperature resistivity performance, and its preparation method is simple.
The present invention is realized by following technical proposals, a kind of Ni/ graphite/(Ba with low-resistivity performance under good lift-drag ratio and the normal temperature 1-x-y, Sr x, Pb y) TiO 3Based composite positive temperature coefficient thermistor is characterized in that, its material composition and molar content are:
(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC ceramic powder: (62.0～98.9) %, x=0.00～0.35 wherein, y=0.00～0.56;
Metal Ni powder: (0.01～22) %;
Graphite powder: (0～16) %;
This Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3The room temperature resistivity of based composite positive temperature coefficient thermistor material is 4.37～8.28 Ω cm, and lift-drag ratio is 5.86 * 10 2～1.23 * 10 3
Above-mentioned (Ba 1-x-y, Sr x, Pb y) TiO 3The component and the quality percentage composition of base PTC thermistor ceramic powder are:
(Ba 1-x-y，Sr x，Pb y)TiO 3：(99.9236～99.9298)％；
Sb 2O 3：(0.01～0.0726)％；
Nb 2O 5：(0.014～0.1084)％；
MnO 2：(0.014～0.0158)％；
Al 2O 3：(0.012～0386)％；
SiO 2：(0.01～0.0465)％；
TiO 2：(0.01～0.0248)％；
Above-mentioned Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3The preparation method of based composite positive temperature coefficient thermistor is characterized in that comprising following process:
1, is mixed with (Ba with following component and quality percentage composition 1-x-y, Sr x, Pb y) TiO 3The base positive temperature coefficient thermal resistor ceramic powder,
(Ba 1-x-y，Sr x，Pb y)TiO 3：(99.9236～99.9298)％；
Sb 2O 3：(0.01～0.0726)％；
Nb 2O 5：(0.014～0.1084)％；
MnO 2：(0.014～0.0158)％；
Al 2O 3：(0.012～0.0386)％；
SiO 2：(0.01～0.0465)％；
TiO 2：(0.01～0.0248)％；
2, (the Ba of 80～100 order numbers that step 1 is prepared 1-x-y, Sr x, Pb y) TiO 3The base positive temperature coefficient thermal resistor ceramic powder, by mole percentage composition (62.0～a 98.9) %, metal Ni powder batching by mole percentage composition (0.01～22) % and graphite powder molar content (0～16) %, mix 4～24h through dry ball milling, add the PVA solution granulation of mass content 5% then, make green compact with 200～300MPa moulding.
3, green compact are through binder removal or without binder removal, at Al 2O 3Button burns in the crucible, by Al 2O 3The local reduction atmosphere that the graphite of placing in the crucible causes is incubated 10～40min Low fire ceramic sample down in 1200～1280 ℃.Sample is made Ni/ graphite/BaTiO through upper and lower surface burning infiltration ohmic contact silver electrode or aluminium electrode 3Based composite positive temperature coefficient thermistor.
Advantage of the present invention: preparation process is simple, and prepared composite material room temperature resistivity is 4.37～8.28 Ω cm, and lift-drag ratio is 5.86 * 10 2～1.23 * 10 3, and do not add the former (Ba of metal Ni powder and graphite powder 1-x-y, Sr x, Pb y) TiO 3The room temperature resistivity of base positive temperature coefficient thermal resistor ceramic material is 331.1 Ω cm, and lift-drag ratio is 3.82 * 10 3Ni/ graphite of the present invention/(Ba 1-x-y, Sr x, Pb y) TiO 3The based composite positive temperature coefficient thermistor performance obviously is better than existing (Ba 1-x-y, Sr x, Pb y) TiO 3Based positive temperature coefficient thermistor material.
Embodiment
Embodiment: be (Ba by prescription 0.9, Sr 0.08, Pb 0.02) TiO 3+ 0.0641Sb 2O 3+ 0.1062Nb 2O 5With other a small amount of admixture 0.1270MnO 2, 0.0341Al 2O 3, 0.0462SiO 2And 0.0208TiO 2Carry out weigh batching, mix and granulation with the PVA solution of 5% (mass percent) after ball milling 6h oven dry, be pressed into the disk of φ 12mm * 3mm then, moulding pressure is 300MPa.Green compact are incubated 20min down at 1250 ℃ then and burn till through binder removal, make the present invention (Ba 0.9, Sr 0.08, Pb 0.02) TiO 3The base positive temperature coefficient thermal resistor pottery burns till material; Or expect to place alumina crucible to be incubated 20min down above-mentioned ball milling material oven dry and burn till, make (Ba at 1250 ℃ 0.9, Sr 0.08, Pb 0.02) TiO 3The base positive temperature coefficient thermal resistor pottery burns till material.Then should (Ba 0.9, Sr 0.08, Pb 0.02) TiO 3The base positive temperature coefficient thermal resistor pottery burns till material to carry out crossing 80 mesh sieves after the mechanical crushing, and the taking-up oven dry is stand-by behind the ball milling 30min again.Add 0.10% metal nickel powder and 0.005% graphite powder in the oven dry material, mix through dry ball milling 24h, add the PVA solution granulation of 5wt% then, be shaped to the disk of φ 10mm * 2mm, moulding pressure is 250MPa.Green compact are without binder removal, at Al 2O 3Button burns in the crucible, by Al 2O 3The local reduction atmosphere that the graphite of placing in the crucible causes is incubated 20min Low fire ceramic sample down in 1260 ℃.The upper and lower surface burning infiltration ohmic contact silver electrode of sample warp.The room temperature resistivity of this composite positive temperature coefficient thermistor ceramic material is 8.28 Ω cm, and lift-drag ratio is 1.23 * 10 3

Claims (3)

1, a kind of Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3Based composite positive temperature coefficient thermistor is characterized in that, its material composition and molar content are:
(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC ceramic powder: (62.0～98.9) %, x=0.00～0.35 wherein, y=0.00～0.56;
Metal Ni powder: (0.01～22) %;
Graphite powder: (0～16) %;
This Ni/ graphite/(Ba 1-x-y, Sr x, Pb y) TiO 3The room temperature resistivity of based composite positive temperature coefficient thermistor material is 4.37～8.28 Ω cm, and lift-drag ratio is 5.86 * 10 2～1.23 * 10 3
2, by the described Ni/ graphite of claim 1/(Ba 1-x-y, Sr x, Pb y) TiO 3Based composite positive temperature coefficient thermistor is characterized in that: (Ba 1-x-y, Sr x, Pb y) TiO 3The component and the quality percentage composition of base PTC thermistor ceramic powder are:
(Ba 1-x-y，Sr x，Pb y)TiO 3：(99.9236～99.9298)％；
Sb 2O 3：(0.01～0.0726)％；
Nb 2O 5：(0.014～0.1084)％；
MnO 2：(0.014～0.0158)％；
Al 2O 3：(0.012～0386)％；
SiO 2：(0.01～0.0465)％；
TiO 2：(0.01～0.0248)％。
3, the described Ni/ graphite of a kind of preparation claim 1/(Ba 1-x-y, Sr x, Pb y) TiO 3The method of based composite positive temperature coefficient thermistor is characterized in that comprising following process:
1) is mixed with (Ba with following component and quality percentage composition 1-x-y, Sr x, Pb y) TiO 3The base positive temperature coefficient thermal resistor ceramic powder,
(Ba 1-x-y，Sr x，Pb y)TiO 3：(99.9236～99.9298)％；
Sb 2O 3：(0.01～0.0726)％；
Nb 2O 6：(0.014～0.1084)％；
MnO 2：(0.014～0.0158)％；
Al 2O 3：(0.012～0.0386)％；
SiO 2：(0.01～0.0465)％；
TiO 2：(0.01～0.0248)％；
2) (the Ba of 80～100 order numbers that step 1) is prepared 1-x-y, Sr x, Pb y) TiO 3The base positive temperature coefficient thermal resistor ceramic powder, press the batching of mole percentage composition (0～16) % by mole percentage composition (0.01～22) % and graphite powder by mole percentage composition (62.0～98.9) %, metal Ni powder, mix 4～24h through dry ball milling, add the PVA solution granulation of mass content 5% then, make green compact with 200～300MPa moulding;
3) green compact are through binder removal or without binder removal, at Al 2O 3Button burns in the crucible, by Al 2O 3The local reduction atmosphere that the graphite of placing in the crucible causes, insulation 10～40min Low fire ceramic sample under 1200～1280 ℃, sample is made Ni/ graphite/BaTiO through upper and lower surface burning infiltration ohmic contact silver electrode or aluminium electrode 3Based composite positive temperature coefficient thermistor.
CN 200410094023 2004-12-27 2004-12-27 Ni/graphite (Ba-[1-x-y],Sr-[x],Pb-[y])TiO-[3] base composite PTC thermistor and preparing method Pending CN1632886A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101671177B (en) * 2009-09-24 2012-07-04 东莞市龙基电子有限公司 Preparation method of positive temperature coefficient ceramics by dry-method ball milling
WO2017198233A1 (en) * 2016-05-20 2017-11-23 济南圣泉集团股份有限公司 Ptc inorganic composite material, and manufacturing method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101671177B (en) * 2009-09-24 2012-07-04 东莞市龙基电子有限公司 Preparation method of positive temperature coefficient ceramics by dry-method ball milling
WO2017198233A1 (en) * 2016-05-20 2017-11-23 济南圣泉集团股份有限公司 Ptc inorganic composite material, and manufacturing method and application thereof

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