CN101423388B - Solid phase synthesis of PTC thermistor motor startup ceramic chip formula for one time and production process - Google Patents

Solid phase synthesis of PTC thermistor motor startup ceramic chip formula for one time and production process Download PDF

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CN101423388B
CN101423388B CN2008100689771A CN200810068977A CN101423388B CN 101423388 B CN101423388 B CN 101423388B CN 2008100689771 A CN2008100689771 A CN 2008100689771A CN 200810068977 A CN200810068977 A CN 200810068977A CN 101423388 B CN101423388 B CN 101423388B
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solid phase
ptc thermistor
phase synthesis
percent
ceramic chip
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CN101423388A (en
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王学杰
杨红平
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Guizhou Zhenhua Hongyun Electronics Co., Ltd.
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HONGYUN APPLIANCE FACTORY CHINA ZHENGHUA GROUP
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Abstract

The invention relates to a motor-on ceramic chip material formulation of a one-step solid phase synthesized PTC thermistor and a process for producing the same. A novel motor-on ceramic chip material formulation of the PTC thermistor is excogitated according to the characteristics of a motor-on thermistor by adopting a multi-donor doping principle, and the prior process for the domestic production of the motor-on chip of the PTC thermistor is improved according to the formula, wherein the formulation and the weight percentage are as follows: 88.28 to 94.85 percent of BaTiO3; 2.608 to 5.65 percent of CaCO3; 1.28 to 5.012 percent of TiO2; 0.68 to 0.84 percent of SiO2; 0.153 to 0.182 percent of [Y2O3, Nb2O3 and Sb2O3]; 0.008 to 0.012 percent of Li2CO3; and 0.165 to 0.192 percent of Mn(NO3)2. The production process is simplified from the prior more than 10 steps to a few steps. The material formulation uses a simple production process, can improve the product quality and the product qualification rate, save energy sources, and is an innovation to the prior formulation.

Description

Solid phase synthesis of PTC thermistor motor startup ceramic chip formula and production technology
Technical field: the present invention relates to a kind of ceramic material prescription, specifically solid phase synthesis of PTC thermistor motor startup ceramic chip formula and production technology.
Background technology: the PTC thermistor motor starting chip of producing at home at present nearly all is traditional prescription, in this type of prescription because SrCO 3, CaCO 3There is not pre-burning to decompose, if according to conventional experience pressed density 3.2～3.3g/Cm 3The interior crystal boundary space of porcelain basal body is bigger after the roasting, and pore is many, and constriction coefficient is bigger, even the porcelain primary surface has bubble to produce.
The conventional fabrication processes of PTC thermistor motor starting chip is a dewatered drying behind a ball milling; Must be 1100～1190 ℃ of pre-burning reactions; Then the pre-burning piece is pulverized, carried out secondary ball milling, granulation, dry-pressing, moulding, roasting and process PTC thermistor motor starting ceramic substrate.
The inventor proposes Y in " research of a solid phase synthesis CPTC of many donor dopings thermistor " (Guizhou University of Technology's journal natural science edition the 37th volume the 3rd phase 08.5.) literary composition 2O 3, Nb 2O 5Two donor dopings are used BaTiO 3The design of a solid phase synthesis CPTC of powder thermistor is for the present invention provides fundamental basis.
Summary of the invention: the object of the invention; Be to adopt the principle of a solid phase synthesis CPTC of many donor dopings thermal sensitive ceramics resistance; Characteristics according to motor starting PTC thermistor; Research and propose a kind of new PTC thermistor motor startup ceramic chip formula, and present domestic production PTC thermistor motor starting chip production technology is improved.
Prescription, proportioning and the processing technology of the new PTC thermistor motor startup ceramic chip that the present invention proposes is different fully with prescription, proportioning and process that the PTC thermistor horse of domestic production at present starts ceramic chip.The prescription and the quality per distribution ratio of domestic production PTC thermistor motor starting chip are at present:
1.BaCO 3 60～67％
2.CaCO 3 5～6％
3.TiO 2 26～32％
4.SiO 2 0.38～0.55％
5.SrCO 3 0.57～0.68％
6.Y 2O 3 0.189～0.265％
7.Mn(NO 3) 2 0.42～0.54％
Can know that from prescription carbonate content is high in the prescription, bakes to burn the article decomposes a large amount of gases of generation, and the bakes to burn the article decomposition is also incomplete in addition, roasting pressed density 3.2～3.3g/cm 3, can not meet the requirement of making PTC thermistor motor startup ceramic chip, must workpiece preheating block be pulverized; Carry out secondary ball milling granulation, dry-pressing formed and roasting; Process PTC thermistor motor startup ceramic chip, be called secondary ball milling or after baking technology, its technological process is followed successively by:
Batching → ball milling → dehydration → oven dry → granulation → precompressed → moulding → roasting → pulverizing → ball milling → granulation → dry-pressing → moulding → roasting
Nearly ten multisteps are rapid for operation
The present invention takes BaTiO according to many donor doping one defective material solid phase synthesis principles 3Powder control is with Y 2O 3+ Nb 2O 3+ Sb 2O 3Three alms givers are superfluous to mix, and combines to add Li 2CO 3Or K 2CO 3Acceptor impurity, the PTC thermistor motor startup ceramic chip prescription and the quality per distribution ratio of development are:
1.BaTiO 3 88.28～94.85％
2.CaCO 3 2.608～5.65％
3.TiO 2 1.28～5.012％
4.SiO 2 0.68～0.84％
5.[Y 2O 3+Nb 2O 3+Sb 2O 3] 0.153～0.182％
6.Li 2CO 3Or K 2CO 30.008～0.012%
7.Mn(NO 3) 2 0.165～0.192％
Optimization formula of the present invention and quality per distribution ratio do
1.BaTiO 3 88.28～94.85％
2.CaCO 3 2.608～5.65％
3.TiO 2 1.28～5.012％
4.SiO 2 0.68～0.84％
5.[Y 2O 3+Nb 2O 3+Sb 2O 3] 0.175
6.Li 2CO 3 0.010
7.Mn(NO 3) 2 0.183
The proportioning of each composition is a mass percent in the above-mentioned prescription, and total mass percent is 100%
Y 2O 3, Nb 2O 3And Sb 2O 3Mol ratio 7: 2: 1
The present invention's prescription is used BaTiO 3Replace BaCO 3And strict control BaTiO 3The quality of powder adopts the superfluous doping of three alms givers, and combines to add Li 2CO 3Or K 2CO 3Acceptor impurity, a ball milling roasting can pressed density reach 3.4～3.6g/cm 3Meet the requirement of PCT thermistor motor startup ceramic chip.
Technological process of the present invention is followed successively by:
Batching → ball milling → oven dry → granulation → dry-pressing → moulding → roasting, production technology of the present invention are called process for solid phase synthesis of a ball milling, compare with secondary ball milling or after baking technology, and processing step is simplified greatly.
The present invention is to BaTiO 3Powder quality control requires:
Free BaO<1.5; Specific area<2.0 particle size distribution D 50≤38mm; Barium titanium ratio: Ba/Ti=1; Impurity content control: Sr 2+≤15ppm, Ca 2+≤18ppm, Mg 2+≤4ppm, Fe 2+, 3+≤3ppm, Na +≤5ppm, k +≤6ppm, Al 3+≤5ppm, Si 4+≤9ppm.
Concrete operations are: raw material is weighed up in proportion, puts into the rolling ball milling jar, by material: ball: the weight ratio of water=1: 2: 2, ball milling 24h then discharging 120 ± 5 ℃ drying in oven, granulation, with high efficiency automatic make-up machine moulding; With 14 meters furnace superintendents, 11 groups of warm areas, 18 temperature control continuous tunnel furnaces; 1280～1340 ℃ of high-temperature region sintering temperatures; High temperature solid-state generated time 1.5～2 hours advances stove to the total time control 15～22 hours of coming out of the stove, and the chip after high temperature burns till is handled through Ohmic electrode and surface electrode.
Prescription of the present invention and technology have following characteristics:
(1) porcelain prescription of the present invention adopts Y 2O 3, Nb 2O 3And Sb 2O 5The superfluous doping of many alms givers also combines to add Li 2CO 3Or K 2CO 3The prescription and the technology of acceptor impurity powder one defective material solid phase synthesis of PTC thermistor motor starting chip, thus product cost reduced greatly, improved the output qualification rate.
(2) the concrete technical scheme of porcelain prescription is with BaTiO 3Powder is matrix, employing Y 2O 3, Nb 2O 3And Sb 2O 3Li is mixed, also combined to add to three alms givers surplus 2CO 3Or K 2CO 3Deng acceptor impurity one defective material solid phase synthesis, and control granulation grade uniformity, improve porcelain basal body green compact pressed density and be 3.4～3.6g～/cm 3, ceramic body shrinks system for counting not quite smooth surface, no bubble after the roasting like this.
(3) the concrete technical scheme of technology is; Directly make PTC thermistor motor starting ceramic substrate, (not needing the porcelain pre-burning in the technology, a direct solid phase synthesis) through ball milling, granulation, dry-pressing, moulding, roasting; Compare with prior manufacturing method and to have reduced precompressed, pre-burning, process procedures such as pulverizing, secondary ball milling again; Cut down the consumption of energy, reduce ambient impurities and bring formation pollution in the product into, thereby improve the quality of products.
Tool prescription of the present invention economical rationality, production technology is simple.Can also improve the quality of products, improve product percent of pass, owing to reduced technological process, practice thrift the energy, be a kind of innovation to conventional formulation.
Embodiment: embodiment 1
Formulation ratio (mass percent) weighing (weight portion)
1、BaTiO 3 88.28％ 203.32
2.、CaCO 3 5.65％ 13.013
3、TiO 2 5.012％ 11.543
4、SiO 2 0.69％ 1.589
5、Y 2O 3
+Nb 2O 3 + 0.175％ 0.403
+Sb 2O 3
6、Li 2CO 3 0.010％ 0.023
7、Mn(NO 3) 2 0.183％ 0.421
Σ230.31
Raw material is weighed up in proportion, put into the rolling ball milling jar, in material: ball: the ratio ball milling 24h of water=1: 2: 2, discharging granulation after 120 ± 5 ℃ drying in oven then is with high efficiency automatic make-up machine moulding; With 14 meters furnace superintendents, 11 groups of warm areas, 18 temperature control continuous tunnel furnaces, 1280～1340 ℃ of high-temperature region sintering temperatures, high temperature solid-state generated time 1.5～2 hours advances stove to the time control 15～22 hours of coming out of the stove.Chip after burning till is handled through Ohmic electrode and surface electrode, carries out electric performance test again.
The product examination result please read audit report book (1) P.7
Embodiment 2
Formulation ratio (mass percent) weighing (weight portion)
1、BaTiO 3 94.85％ 219.685
2.、CaCO 3 2.608％ 6.04
3、TiO 2 1.28％ 2.964
4、SiO 2 0.69％ 1.598
5、Y 2O 3
+Nb 2O 3 0.175％ 0.405
+Sb 2O 3
6、Li 2CO 3 0.010％ 0.0231
7、Mn(NO 3) 2 0.183％ 0.42
Σ231.61
Operation is with embodiment 1
The product examination result please read audit report book (2) P.8
Figure G2008100689771D00071

Claims (2)

1. a solid phase synthesis of PTC thermistor motor startup ceramic chip comprises and adopts many donor dopings defective material solid phase synthesis principle, it is characterized in that taking BaTiO 3Powder quality control, three alms givers are superfluous to mix, and combines to add Li 2CO 3Or K 2CO 3Acceptor impurity, its concrete quality per distribution ratio is:
1.BaTiO 3 88.28～94.85％
2.CaCO 3 2.608～5.65％
3.TiO 2 1.28～5.012％
4.SiO 2 0.68～0.84％
5.[Y 2O 3+Nb 2O 3+Sb 2O 3] 0.153～0.182％
6.Li 2CO 3Or K 2CO 30.008～0.012%
7.Mn(NO 3) 2 0.165～0.192％
Wherein, Y 2O 3, Nb 2O 3, Sb 2O 3Mol ratio 7: 2: 1,
Adopt one time ball-milling technology, a solid phase synthesis weighs up raw material in proportion; Put into the rolling ball milling jar; By material: ball: the weight ratio of water=1: 2: 2, ball milling 24h then discharging 120 ± 5 ℃ drying in oven, granulation, with high efficiency automatic make-up machine moulding; With 14 meters furnace superintendents, 11 groups of warm areas, 18 temperature control continuous tunnel furnaces; 1280～1340 ℃ of high-temperature region sintering temperatures; High temperature solid-state generated time 1.5～2 hours advances stove to the total time control 15～22 hours of coming out of the stove, and the chip after high temperature burns till is handled through Ohmic electrode and surface electrode.
2. a solid phase synthesis of PTC thermistor motor startup ceramic chip according to claim 1, its characteristic mass per distribution ratio is:
1.BaTiO 3 88.28～94.85％
2.CaCO 3 2.608～5.65％
3.TiO 2 1.28～5.012％
4.SiO 2 0.68～0.84％
5.[Y 2O 3+Nb 2O 3+Sb 2O 3] 0.175％
6.Li 2CO 3 0.010％
7.Mn(NO 3) 2 0.183％。
CN2008100689771A 2008-11-05 2008-11-05 Solid phase synthesis of PTC thermistor motor startup ceramic chip formula for one time and production process Expired - Fee Related CN101423388B (en)

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CN103408306A (en) * 2012-11-05 2013-11-27 海宁永力电子陶瓷有限公司 Process for producing high temperature and pressure resistant PTC (Positive Temperature Coefficient) thermistor ceramics
CN106554201A (en) * 2016-10-26 2017-04-05 安徽飞达电气科技有限公司 A kind of lead-free high-voltage ceramic capacitor material
CN107702815A (en) * 2017-09-25 2018-02-16 南京航伽电子科技有限公司 A kind of temperature transmitter suitable for the detection of wide warm area
CN113773072A (en) * 2021-09-06 2021-12-10 海宁金隆电子陶瓷有限公司 Processing technology of surface-mounted ceramic thermistor substrate

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1215485C (en) * 1999-05-20 2005-08-17 株式会社村田制作所 Barium titanate semiconductor ceramic powder and stacked semiconductor device

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1215485C (en) * 1999-05-20 2005-08-17 株式会社村田制作所 Barium titanate semiconductor ceramic powder and stacked semiconductor device

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JP特开平4－214070A 1992.08.05
王学杰,杨红平.多施主掺杂一次固相合成CPTC热敏电阻的研究.《贵州工业大学学报(自然科学版)》.2008,第37卷(第3期),第53页～第56页. *

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Owner name: GUIZHOU ZHENHUA HONGYUN ELECTRONIC CO., LTD.

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