CN101350242A - Method for sintering zinc oxide resistance sheet - Google Patents

Method for sintering zinc oxide resistance sheet Download PDF

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Publication number
CN101350242A
CN101350242A CNA2008101208139A CN200810120813A CN101350242A CN 101350242 A CN101350242 A CN 101350242A CN A2008101208139 A CNA2008101208139 A CN A2008101208139A CN 200810120813 A CN200810120813 A CN 200810120813A CN 101350242 A CN101350242 A CN 101350242A
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sintering
temperature
zinc oxide
oxide resistance
per hour
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CN101350242B (en
Inventor
高奇峰
汤建江
王海英
蒋烨
严斌杰
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NINGBO ZHENHAI GUOCHUANG HIGH-VOLTAGE ELECTRIC APPARATUS Co Ltd
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NINGBO ZHENHAI GUOCHUANG HIGH-VOLTAGE ELECTRIC APPARATUS Co Ltd
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Abstract

The invention relates to a sintering method of a zinc oxide resistance chip, the method of the invention is characterized by increasing the temperature to 850 DEG C from the indoor temperature with the speed of 100-250 DEG C per hour, then increasing the temperature to 1100-1300 DEG C from 30-80 DEG C and keeping the temperature for 2-10 hours, then carrying out the subsection cooling, namely cooling the temperature to 1050 DEG C from 70-100 DEG C and keeping the temperature for 1-2 hours, then cooling the temperature to 850 DEG C with the speed of 75-100 DEG C per hour and keeping the temperature for 1-2 hours, and then cooling the temperature to the indoor temperature with the speed of 75-120 DEG C per hour. The method of the invention is characterized in that the technique is reasonable, the yield of the zinc oxide resistance chip is high, the non-linear coefficient is high, the protection performance is good and the heat endurance is reliable.

Description

A kind of sintering method of zinc oxide resistance sheet
Technical field
The present invention relates to the sintering method of lightning arrester with zinc oxide resistance sheet, is the improvement to existing zinc oxide resistance sheet sintering method, the technical field that belongs to the piezo-resistance preparation and use.
Background technology
Zinc oxide resistance sheet is the core parts of zinc oxide arrester; it has excellent voltage one electric current nonlinear characteristic: when running into the surge voltage attack that exceeds the normal voltage manyfold; the resistance value of zinc oxide resistance sheet can instantaneously turn to low resistance by high resistance; make powerful momentary excess current flow into the earth, avoided protected electric equipment attacked by overvoltage through zinc oxide resistance sheet.As overvoltage protection element, desirable electrical characteristic is: the non linear coefficient height, response speed is fast, operation stability is high.
The preparation technology of zinc oxide resistance sheet and general electronic ceramic prepare basic identical, but because its special nonlinear characteristic, make its electric property higher to the dependence of technology, wherein sintering is one of technology of most critical in the manufacture process, the purpose of sintering is exactly the condition and the process of various physical-chemical reactions in the control voltage-sensitive ceramic base substrate, forms the chemical composition of expection and homogenizing and the densification that promotes microstructure.Under raw material, the prescription situation consistent with other technologies, sintering process plays decisive role to the electric property of zinc oxide resistance sheet.
Present domestic most of zinc oxide resistance sheet manufacturer all adopts traditional sintering method, adopt box or the tunnel type resistance furnace carries out sintering with electric energy heating to resistor disc, technology is generally: the highest sintering temperature is set in 1100 ℃~1300 ℃, sintering time is: 2~4 hours, linear temperature increase speed is per hour 80~120 ℃, and linear cooling rate is per hour 60~90 ℃.Utilize this sintering process, in the high-temperature region, heating-cooling speed is too fast.Be rapidly heated and make the physical-chemical reaction speed in the sintering process too fast, particularly, in the warm area that liquid phase forms, be unfavorable for that the gas steadily mobile and that decomposition is come out of component is overflowed more than 800 ℃, cause microstructure skewness, pore to increase, even produce micro-crack; In temperature-fall period, fast cooling causes the little crystal grain segregation of a large amount of ZnO that is in molten state evenly not to be segregated in making part ZnO abnormal grain growth on the big crystal grain, simultaneously, fast cooling makes the part crystal boundary have little time to undergo phase transition, and increases crystal grain defective and internal stress.The zinc oxide resistance sheet rate of finished products that adopts above-mentioned technology to obtain is low, and protective feature and poor heat stability are in case be struck by lightning; protection nargin is little, and is contained in lightning arrester after interior operation a period of time, and leakage current increases gradually; resistor disc is tending towards thermally labile, causes the useful life of zinc oxide resistance sheet short.
Summary of the invention
Technical problem to be solved by this invention is the sintering method that a kind of zinc oxide resistance sheet is provided at the prior art present situation, to improve rate of finished products, non linear coefficient, protective value and the thermal stability of zinc oxide resistance sheet.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the sintering method of zinc oxide resistance sheet of the present invention is on existing agglomerating plant and sintering process; by increasing cooling device; adjust sintering temperature curve, improve rate of finished products, non linear coefficient, protective value and the thermal stability of zinc oxide resistance sheet.
The sintering of zinc oxide resistance sheet of the present invention is to carry out in the push-plate type continuous tunnel furnace, and the characteristics of this sintering method are to adopt the multi-steps sintering of being made up of temperature-gradient method, soak and segmentation cooling.
Tool originally may further comprise the steps:
A, get the base substrate of binder removal pre-burning on the production line, put into the sintering alms bowl on the side behind the insulating barrier;
B, the sintering alms bowl that is placed with the pre-burning base substrate in the step (a) is put into push-plate type continuous tunnel furnace sintering, temperature-gradient method to 1100~1300 ℃.
C, under the described sintering temperature of step (b), kept 2-10 hour;
D, again temperature till the described sintering temperature segmentation of step (b) cool to room temperature.
Described temperature-gradient method is to heat up with two sections heating modes, and first section is to begin to be raised to 850 ℃ with 100~250 ℃ speed per hour from room temperature, and second section is to be warmed up to 1100 ℃~1300 ℃ of sintering temperatures with 30~85 ℃ heating rate from 850 ℃.
Described segmentation cooling is divided into five sections to be carried out, the phase I, after soak finishes, with per hour 70~100 ℃ be cooled to 1050 ℃; Second stage kept 1~2 hour at 1050 ℃; Phase III, with per hour 75~100 ℃ be cooled to 850 ℃, the quadravalence section kept 1~2 hour at 850 ℃, five-stage is with till 75~120 ℃ of cool to room temperature per hour.
Compared with prior art, the sintering method of zinc oxide resistance sheet of the present invention has the following advantages: shortened the low-temperature zone sintering time, improved operating efficiency; Control by segmentation, the high temperature section that slows down heating rate, impel that various physical-chemical reactions can steadily slowly carry out under the high temperature, help microstructure and evenly form, by slowing down the local cooling's speed after the insulation, the ZnO that helps molten state slowly separates out from liquid phase, reduce the defective of intragranular, crystal boundary, increase the insulating process of temperature descending section, help various phase transformations and take place, reduce internal stress, improve the electric property of resistor disc.
Technology of the present invention is reasonable, its rate of finished products height, and the non linear coefficient height of zinc oxide resistance sheet, protective feature is good, thermal stability is reliable.Zinc oxide resistance sheet with this method sintering, in ageing test, the leakage current of zinc oxide resistance sheet increases in time and descends, carry out ageing test according to international standard IEC 60099-4, power consumption is lasting downward trend, the ratio that stopped power consumption and initial power consumption in 1000 hours has improved the operational reliability of zinc oxide arrester less than 1.0, has prolonged its useful life.
Description of drawings
Fig. 1 is zinc oxide resistance sheet sintering curre figure of the present invention (T is a temperature among the figure, and t is the time).
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one: with insulating barrier on the presintered compact body side surface, be positioned over then in the sintering alms bowl and advance continuous tunnel furnace, with per hour 100 ℃ be warmed up to 850 ℃, again with per hour 30 ℃ be warmed up to 1100 ℃ and keep 2h, then with per hour 70 ℃ cool to 1050 ℃ and kept 2 hours, again with per hour 75 ℃ cool to 850 ℃ and kept 2 hours, at last with 75 ℃ of cool to room temperature per hour.Abrasive disc in a conventional manner cleans again, heat treatment, spraying aluminium electrode, test.By the zinc oxide resistance sheet rate of finished products height that this sintering method obtains, through the non linear coefficient height of this resistor disc of evidence, protective feature is good, and thermal stability is reliable.
Embodiment two: with insulating barrier on the presintered compact body side surface, be positioned over then in the sintering alms bowl and advance continuous tunnel furnace, with per hour 200 ℃ be warmed up to 850 ℃, again with per hour 50 ℃ be warmed up to 1200 ℃ and keep 5h, then with per hour 95 ℃ cool to 1050 ℃ and kept 2 hours, again with per hour 75 ℃ cool to 850 ℃ and kept 2 hours, with 100 ℃ of cool to room temperature per hour, sintering curre is seen Fig. 1 at last.Abrasive disc cleans in a conventional manner, heat treatment, spraying aluminium electrode, test.By the zinc oxide resistance sheet rate of finished products height that this sintering method obtains, through the non linear coefficient height of this resistor disc of evidence, protective feature is good, and thermal stability is reliable.
Embodiment three: with insulating barrier on the presintered compact body side surface, be positioned over then in the sintering alms bowl and advance continuous tunnel furnace, with per hour 250 ℃ be warmed up to 850 ℃, again with per hour 85 ℃ be warmed up to 1300 ℃ and keep 10h, then with per hour 100 ℃ cool to 1050 ℃ and kept 1 hour, again with per hour 100 ℃ cool to 850 ℃ and kept 1 hour, at last with 120 ℃ of cool to room temperature per hour.Abrasive disc in a conventional manner cleans again, heat treatment, spraying aluminium electrode, test.By the zinc oxide resistance sheet rate of finished products height that this sintering method obtains, through the non linear coefficient height of this resistor disc of evidence, protective feature is good, and thermal stability is reliable.
In above-mentioned three embodiment, wherein embodiment two is a preferred forms, and it is two execution modes relatively in addition, its rate of finished products of the zinc oxide resistance sheet that obtains, non linear coefficient, and protective feature, thermal stability more are better than other two execution mode.

Claims (4)

1, a kind of sintering method of zinc oxide resistance sheet is characterized in that: it adopts the multi-steps sintering of being made up of temperature-gradient method, soak and segmentation cooling.
2, the sintering method of zinc oxide resistance sheet according to claim 1 is characterized in that: described multi-steps sintering may further comprise the steps:
A, get the base substrate of binder removal pre-burning on the production line, put into the sintering alms bowl on the side behind the insulating barrier;
B, the sintering alms bowl that is placed with the pre-burning base substrate in the step (a) is put into push-plate type continuous tunnel furnace sintering, temperature-gradient method to 1100~1300 ℃;
C, under the described sintering temperature of step (b), kept 2-10 hour;
D, again temperature till the described sintering temperature segmentation of step (b) cool to room temperature.
3, the sintering method of zinc oxide resistance sheet according to claim 2, it is characterized in that: described temperature-gradient method is to heat up with two sections heating modes, first section is to begin to be raised to 850 ℃ with 100~250 ℃ speed per hour from room temperature, and second section is to be warmed up to 1100 ℃~1300 ℃ of sintering temperatures with 30~85 ℃ heating rate from 850 ℃.
4, according to the sintering method of claim 2 or 3 described zinc oxide resistance sheets, it is characterized in that: described segmentation cooling is divided into five sections to be carried out, the phase I, after soak finishes, with per hour 70~100 ℃ be cooled to 1050 ℃; Second stage kept 1~2 hour at 1050 ℃; Phase III, with per hour 75~100 ℃ be cooled to 850 ℃; The quadravalence section kept 1~2 hour at 850 ℃; Five-stage is with till 75~120 ℃ of cool to room temperature per hour.
CN2008101208139A 2008-09-05 2008-09-05 Method for sintering zinc oxide resistance sheet Expired - Fee Related CN101350242B (en)

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CN101350242B CN101350242B (en) 2011-04-13

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880157A (en) * 2010-06-24 2010-11-10 中国科学院宁波材料技术与工程研究所 Recipe and preparation method of high-voltage gradient zinc oxide resistance card
CN106380185A (en) * 2016-08-31 2017-02-08 安徽斯迈尔电子科技有限公司 Method for preparing compound film resistor substrate
CN116655368A (en) * 2023-05-26 2023-08-29 嘉兴瑞嘉电气股份有限公司 Preparation method of resistor disc capable of improving high-current impact resistance

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880157A (en) * 2010-06-24 2010-11-10 中国科学院宁波材料技术与工程研究所 Recipe and preparation method of high-voltage gradient zinc oxide resistance card
CN101880157B (en) * 2010-06-24 2012-07-04 中国科学院宁波材料技术与工程研究所 Recipe and preparation method of high-voltage gradient zinc oxide resistance card
CN106380185A (en) * 2016-08-31 2017-02-08 安徽斯迈尔电子科技有限公司 Method for preparing compound film resistor substrate
CN116655368A (en) * 2023-05-26 2023-08-29 嘉兴瑞嘉电气股份有限公司 Preparation method of resistor disc capable of improving high-current impact resistance
CN116655368B (en) * 2023-05-26 2023-12-08 嘉兴瑞嘉电气股份有限公司 Preparation method of resistor disc capable of improving high-current impact resistance

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