CN1546425A - Graphite, phenolic resin, (Ba1-x-y, Srx, Pby) TiO3 based PTC thermistor and method for preparing the same - Google Patents

Graphite, phenolic resin, (Ba1-x-y, Srx, Pby) TiO3 based PTC thermistor and method for preparing the same Download PDF

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Publication number
CN1546425A
CN1546425A CNA2003101071519A CN200310107151A CN1546425A CN 1546425 A CN1546425 A CN 1546425A CN A2003101071519 A CNA2003101071519 A CN A2003101071519A CN 200310107151 A CN200310107151 A CN 200310107151A CN 1546425 A CN1546425 A CN 1546425A
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tio
graphite
ptc thermistor
resol
ball milling
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CN100462328C (en
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曲远方
杨光
马卫兵
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a graphite / phenol resin / (Ba-[1-x-y], Sr-[x], Pb-[y]TiO3 based PTC thermo-sensitive resistor and its making process, wherein its raw material and ingredients are (percentage by weight), Ba[1-x-y], Sr-[x], Pb[y]TiO3 based ceramic powder 62-78%, where x=0.005-0.35, y=0.002-0.56, graphite 14-28%, 5% phenolic resins containing PVA curing agent 8-18.6%. The invention also discloses the process for preparing the thermo-sensitive resistor.

Description

Graphite/resol/(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC thermistor and preparation method
Technical field
The present invention relates to a kind of graphite/resol/(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC thermistor and preparation method belong to the technology of preparing of ceramic material and components and parts thereof.
Background technology
By at BaTiO 3Add micro-acceptor impurity (Mn, Fe or Cr etc.) in the base PTC stupalith, can effectively increase PTC effect (Huybrechts B, Ishizaki K, Takata M.Proposed phenomenological PTCR model andaccompanying phenomenological PTCR chart[J] .J Am Ceram Soc, 1994,77 (1), 286~288.), owing in prescription, add the recipient element of trace simultaneously, the room temperature resistivity of ptc material can be increased; If restriction recipient element consumption then can have influence on the PTC performance of material.BaTiO 3The resistance lowering of matrix PTC material is a main trend [Gene H, Haertling K.Ferroelectric ceramics:History and Technology[J] the .J Am Ceram Soc of current development, 1999,82 (4): 797~818.] and, present BaTiO 3The room temperature resistivity of base PTC stupalith is higher, this having a strong impact on PTC stupalith and device under the low voltage condition from promotion and application [the I-Nan Lin aspect temperature control heating and the overcurrent protection; Hormg-YiChan; Kuo-Shung Liu.Microwave sintering of PTCR ceramics and their electrical properties[J] .Ferroelectrics Proceedings of the Tenth IEEE International Symposium on Applications ofFerroelectrics.18-21 Aug 1996.Page (s): 987~990 vol 2.].
Summary of the invention
The object of the present invention is to provide a kind of graphite/resol/(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC thermistor and preparation method.This PTC thermistor not only has better liftdrag performance, and has good low-resistivity performance at normal temperatures.
The present invention is realized having the PTC thermistor of low-resistivity performance under good liftdrag and the normal temperature by following technical proposals, it is characterized in that its material composition and weight percent content are:
(Ba 1-x-y, Sr x, Pb y) TiO 3Based ceramic powder: 62~78%, x=0.005~0.35 wherein, y=0.002~0.56;
Graphite: 14~28%;
Contain the PVA solidifying agent and be 5% resol: 8~18.6%.
Above-mentioned (Ba 1-x-y, Sr x, Pb y) TiO 3The component of based ceramic powder and weight percent content are:
(Ba 1-x-y,Sr x,Pb y)TiO 3:65.47~75.01%;
Sb 2O 3:5.81~7.26%;
Nb 2O 5:9.12~10.84%;
MnO 2:0.96~1.58%;
Al 2O 3:3.08~3.86%;
SiO 2:4.06~4.65%;
TiO 2:1.96~2.48%。
The preparation method of the PTC thermistor of said components and content comprises (Ba 1-x-y, Sr x, Pb y) TiO 3The preparation of based ceramic powder, batching, ball milling, granulation, compression moulding and prepare electrode process on formed body is characterized in that the (Ba with 62~78% 80~100 order numbers 1-x-y, Sr x, Pb y) TiO 3Base pottery oven dry powder is with after 14~28% graphite mixes 1~24h with ball milling, add lentamente 8~18.6% contain PVA solidifying agent resol, still mixing 40~150min with ball milling, mix whole mistake 200 mesh sieves in back, put into mould then with after the compression moulding of 40~100Mpa pressure, the upper and lower surface on the formed body with 40~100Mpa compacting on metal electrode, or Electroless Plating Ni electrode, or sputter Ni or Al electrode, obtain the PTC thermistor.
The outstanding advantage of compound PTC thermistor of the present invention is under the prerequisite that guarantees better liftdrag, compare with former PTC ceramic thermal resistance, the graphite that causes low room temperature resistivity of having avoided traditional PTC ceramic high temperature to burn till is oxidized, and the room temperature resistivity of compound PTC thermistor obviously reduces.
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 0.0127MnO 2, 0.0341Al 2O 3, 0.0462SiO 2And 0.0208TiO 2Carrying out weigh batching, is the medium wet-milling 6h that will prepare burden with the deionized water, and mix and granulation with the PVA solution of 5% (mass percent) ball milling material oven dry back, is pressed into the disk of φ 12mm * 3mm then, and moulding pressure is 30MPa.Green compact are incubated 20min down at 1250 ℃ then and burn till through binder removal, make the PTC pottery and burn till material; Or expect to place alumina crucible to be incubated 20min down the oven dry of ball milling material and burn till, make the PTC pottery and burn till material at 1250 ℃.Then this PTC pottery is burnt till material and carry out crossing 80 mesh sieves after the mechanical disintegration, the taking-up oven dry is stand-by behind the ball milling 30min again.Prepare burden and carry out ball milling mixing 3h by graphite add-on 20.1% (weight percent) and PTC pottery ball milling oven dry material 64.2% (weight percent), slowly add the resol that 15.7% (weight percent) is mixed with solidifying agent then.Said mixture is carried out mixing and ball milling 60min again, treat all by behind 200 mesh sieves, this compound is put into fixed mould, be pressed into the disk of φ 12mm * 3mm with the pressure of 40Mpa, upper and lower surface compacting aluminium electrode at the disk sample, moulding pressure is 56.6Mpa, at room temperature solidifies 24 h then and makes compound PTC thermistor sample.The room temperature resistivity of this compound PTC thermistor sample is 59.35 Ω cm, and liftdrag is 2.158 * 10 3The room temperature resistivity of the PTC stupalith before compound is 331.1 Ω cm, and liftdrag is 3.82 * 10 3

Claims (3)

1, a kind of graphite/resol/(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC thermistor, it is characterized in that: its material composition and weight percent content are:
(Ba 1-x-y, Sr x, Pb y) TiO 3Based ceramic powder: 62~78%, x=0.005~0.35 wherein, y=0.002~0.56;
Graphite: 14~28%;
Contain the PVA solidifying agent and be 5% resol: 8~18.6%.
2, by the described graphite/resol of claim 1/(Ba 1-x-y, Sr x, Pb y) TiO 3Base PTC thermistor is characterized in that: (Ba 1-x-y, Sr x, Pb y) TiO 3The component of based ceramic powder and weight percent content are:
(Ba 1-x-y,Sr x,Pb y)TiO 3:65.47~75.01%;
Sb 2O 3:5.81~7.26%;
Nb 2O 5:9.12~10.84%;
MnO 2:0.96~1.58%;
Al 2O 3:3.08~3.86%;
SiO 2:4.06~4.65%;
TiO 2:1.96~2.48%。
3, a kind of preparation is by the described graphite/resol of claim 1/(Ba 1-x-y, Sr x, Pb y) TiO 3The method of base PTC thermistor, this method comprises (Ba 1-x-y, Sr x, Pb y) TiO 3The preparation of based ceramic powder, batching, ball milling, choosing grain, compression moulding reach and prepare electrode process on formed bodys, it is characterized in that: (the Ba of 80~100 order numbers with 62~78% 1-x-y, Sr x, Pb y) TiO 3Base pottery oven dry powder is with after 14~28% graphite mixes 1~24h with ball milling, add lentamente 8~18.6% contain PVA solidifying agent resol, still mix 40~150min with ball milling, mix whole mistake 200 mesh sieves in back, put into grinding tool then with after the compression moulding of 40~100Mpa pressure, the upper and lower surface on the formed body with 40~100Mpa compacting on metal electrode, or Electroless Plating Ni electrode, or sputter Ni or Al electrode, obtain compound PTC thermistor.
CNB2003101071519A 2003-12-02 2003-12-02 Graphite, phenolic resin, (Ba1-x-y, Srx, Pby) TiO3 based PTC thermistor and method for preparing the same Expired - Fee Related CN100462328C (en)

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CNB2003101071519A CN100462328C (en) 2003-12-02 2003-12-02 Graphite, phenolic resin, (Ba1-x-y, Srx, Pby) TiO3 based PTC thermistor and method for preparing the same

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1300049C (en) * 2005-09-15 2007-02-14 武汉理工大学 Copolymerized nylon and piezo-electric ceramic composite material and preparation
US8237539B2 (en) 2010-10-07 2012-08-07 Hewlett-Packard Development Company, L.P. Thermistor
CN102701731A (en) * 2012-06-21 2012-10-03 西北大学 Novel thermosensitive ceramic material used for temperature detector
CN103396599A (en) * 2013-08-23 2013-11-20 哈尔滨理工大学 Polymer-base PTC (Positive Temperature Coefficient) composite material for self temperature limiting heat tape
CN114678177A (en) * 2022-03-30 2022-06-28 天津瑞肯新型材料科技有限公司 Composite positive temperature coefficient thermistor material and preparation method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3727396A1 (en) * 1987-08-17 1989-03-02 Philips Patentverwaltung METHOD FOR PRODUCING CERAMIC POWDERS WITH PEROWSKIT STRUCTURE
CN1030873C (en) * 1993-12-04 1996-01-31 清华大学 Thermo-sensitive resistor with multi-layer piled sheet structure
WO1997006537A2 (en) * 1995-08-07 1997-02-20 Philips Electronics N.V. Multiplet ptc resistor

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1300049C (en) * 2005-09-15 2007-02-14 武汉理工大学 Copolymerized nylon and piezo-electric ceramic composite material and preparation
US8237539B2 (en) 2010-10-07 2012-08-07 Hewlett-Packard Development Company, L.P. Thermistor
CN102701731A (en) * 2012-06-21 2012-10-03 西北大学 Novel thermosensitive ceramic material used for temperature detector
CN103396599A (en) * 2013-08-23 2013-11-20 哈尔滨理工大学 Polymer-base PTC (Positive Temperature Coefficient) composite material for self temperature limiting heat tape
CN103396599B (en) * 2013-08-23 2015-11-04 哈尔滨理工大学 Self-limiting heating cable polymer matrix PTC matrix material and preparation method thereof
CN114678177A (en) * 2022-03-30 2022-06-28 天津瑞肯新型材料科技有限公司 Composite positive temperature coefficient thermistor material and preparation method thereof

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