CN102173819B - Preparation method of electric vacuum ceramic tube shell - Google Patents
Preparation method of electric vacuum ceramic tube shell Download PDFInfo
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- CN102173819B CN102173819B CN 201110041219 CN201110041219A CN102173819B CN 102173819 B CN102173819 B CN 102173819B CN 201110041219 CN201110041219 CN 201110041219 CN 201110041219 A CN201110041219 A CN 201110041219A CN 102173819 B CN102173819 B CN 102173819B
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Abstract
The invention relates to a preparation method of an electric vacuum ceramic tube shell. By the method, the problems of energy waste, environmental pollution and high reject ratio caused by discharging wax at a high temperature by a hot pressed casting method in the prior art, and the problems of large equipment investment, low working efficiency and resource waste caused by an isostatic pressing forming method are solved. The preparation method comprises six procedures of preparing materials, performing ball milling, mixing wax, forming, discharging wax at a low temperature and sintering at a high temperature and is characterized in that: in the low-temperature wax-discharging procedure, the wax-discharging temperature is controlled to be 100 to 200 DEG C, the time is controlled to be 12 to 16 hours, and a layer of hard wax film shell is formed on the surface of a green body after the wax is discharged; and in the high-temperature sintering process, the green body with one layer of the hard wax film shell is directly placed into a kiln to be subjected to high-temperature sinter molding, the sintering temperature is between 1,650 and 1,700 DEG C, and the sintering period is 25 to 35 hours. The preparation method has the advantages of energy conservation, environment friendliness, good quality and high finished product rate, meets the technical requirements on using of a high-quality electric vacuum ceramic tube and contributes to popularization and application.
Description
Technical field
The invention belongs to a kind of special cermacis valve tube preparation method technical field, particularly a kind of preparation method of the electrovacuum ceramic tube envelope of in power industry, using.
Background technology
Electrovacuum ceramic tube envelope is the key part that is applied in the power switch in the high, medium and low voltage electrovacuum switching cabinet.Prior art mainly contains hot die-casting molding method and isostatic pressing method to the preparation method of electrovacuum ceramic tube envelope.The hot die-casting molding method is that China's production Product of Ceramic Vacuum Tubes is used a kind of method the earliest, because hot die-casting molding law technology ripening degree height, that adopt at present also mainly is the hot die-casting molding preparation method, it is the mobile and plastic characteristics of utilizing paraffin, heating paraffin is melted, powder added inject metal die after making slip in the wax slurry, the cooling back is frozen into certain shape in mould, and then the molded blank pipe imbedded in the saggar that sorbent material is housed, in kiln, carry out once-firing, and this time carrying out de-waxing in the sintering process, whole de-waxing process adopts 900 ℃～1100 ℃ high temperature.Above-mentioned preparation method has two fatal problems, the one, binder burnout temperature is higher, waste energy, simultaneously also owing to the burning-point of binder burnout temperature greater than wax, make the wax burning, cause environmental pollution, the 2nd, owing in technological processs such as de-waxing, injection molding, there is air to get involved easily, organic discharge during de-waxing, be easy to make goods to produce inhomogeneous pore, directly influence homogeneity and the electric property of goods, therefore intensity also reduce, the shell scrap rate height that therefore this method is produced is difficult to adapt to the technical requirements that the high quality electrovacuum ceramic tube envelope uses.
In order to guarantee high-quality shell, the isostatic pressing method becomes a kind of technology of new rise.The isostatic pressing method is to utilize the characteristics of liquid medium incompressibility and even transitivity to finish, and general flow is batching, wet-milling, mist projection granulating, isostatic pressing, blank processing, burns till, and makes finished product through post-treatment again.The advantage of isostatic pressing base is isotropy, high conformity, the intensity height, but facility investment is big, work efficiency is low, and the Mold Making cycle is long, worker's die clamper is many, need to leave the amount of finish of blank processing in this external isostatic pressing process and burn till after the amount of finish of post-treatment, so take material, the waste resource.
Number of patent application provides a kind of production method of electrovacuum ceramic tube envelope for 200810139749.9 patent application, the roll forming technology that this method proposes, be not complementary with original production unit, if the preparation method who adopts this patent application to propose, need carry out a large amount of facility investments, and its method is also very easily introduced impurity in shell inside and shell surface in pugging roll extrusion process, cause the reduction of product performance.
Number of patent application provides a kind of preparation method of tubular zirconium-oxide for 200810121058.6 patent application, the preparation method of this tubular zirconium-oxide comprises the ceramic size preparation, injection molding, the low temperature de-waxing, isostatic cool pressing and high temperature sintering, but, preparation method according to above-mentioned tubular zirconium-oxide, the temperature control of described low temperature de-waxing is at 600～900 ℃, blank needs to reach 48 hours low-temperature heat processing in low temperature de-waxing process, with tackiness agents such as discharge paraffin resins, will guarantee also that simultaneously blank does not become porcelain or becomes porcelain rate＜5%, blank also will carry out isostatic cool pressing behind the low temperature de-waxing handles, and then carries out high temperature sintering, to guarantee the quality of pipe, so, above-mentioned preparation method, complex process, the low temperature de-waxing time is longer, cause the waste of the energy, and the waste gas that produces in de-waxing process volatilization, environmental pollution caused.In addition, aforesaid method carries out isostatic cool pressing behind de-waxing handles, and difficulty is very big in actual production, is easy to produce breaking of base substrate, causes waste product.
Number of patent application provides a kind of functional porous ceramic plate preparation technology for 200610035401.6 patent application, this preparation method adopts hot die-casting molding and shuttle kiln or pushed bat kiln to burn till, firing temperature is at 1280 ℃～1330 ℃, firing period 18～36 hours, its processing step be batch mixing, ball milling, with powder add form in the wax slurry slurry that flows, with wax starch injection moulding mould molding, the demoulding, with the base substrate de-waxing of making, install to shuttle kiln then or pushed bat kiln burns till, the temperature of described de-waxing adopts the mode of adorning naked burning of revealing below 300 ℃ when burning till.At first, the theme of this application for a patent for invention is porous ceramic plate preparation technology, according to its specification sheets analysis as can be known, this technology is to need in the traditional technology that the porous ceramic plate base substrate imbedded aluminum oxide powder and put into that wax and other organism are difficult to drain in the saggar in order to overcome, and the de-waxing process cycle long cause energy dissipation and burn till after get lodged in the problem that the aluminum oxide powder in the hole is difficult to clean out, de-waxing is to carry out in special wax expelling furnace, binder burnout temperature is below 300 ℃, adopt when burning till and reveal the mode of adorning naked burning, firing temperature is at 1280 ℃～1330 ℃.The temperature of above-mentioned de-waxing below 300 ℃ is being an inapt temperature, can not reach the de-waxing effect what temperature was lower than that paraffin flow to need below 80 ℃, and above-mentioned temperature that has provided de-waxing be below 300 ℃, and the time of low temperature de-waxing does not provide; Owing to adopt the mode of adorning naked burning of revealing when burning till, thereby the wax in the base substrate is all discharged, outside billet surface certainly will being exposed to like this, can suck airborne impurity, under the effect of 1280 ℃～1330 ℃ of firing temperatures, impurity and the ceramic material compound impurity that easy formation can't be drained that combines, as the porous ceramic plate that is applied in the infrared burner parts, do not influence the quality of its use, but at height, in, the electrovacuum ceramic tube envelope of the key part of the power switch of using in the low tension vacuum switch cabinet, this problem does not allow to produce, suck airborne impurity if be exposed to outer billet surface, also can cause shell to become waste product.
Summary of the invention
Technical problem to be solved by this invention is to overcome problem and the defective that prior art exists, utilize and have mobile and plastic characteristics after heating paraffin is melted in the hot die-casting molding method, through test, adjustment and the control of processing parameter, realize energy-saving and environmental protection and reduce cost and improve the purpose of yield rate and product performance.
Preparation method of the present invention comprises batching, ball milling, and wax, moulding, low temperature de-waxing and high temperature burn till six procedures, described burden process is to be 93.5% aluminium sesquioxide with containing weight percent, the silicon-dioxide of 3.2% calcium carbonate 1.%, 2% kaolin and surplus are that talcous raw material mixes, described ball milling operation is to adopt ball mill batching to be worn into 2～10 microns powder, described and wax operation is earlier according to 12%～16% ratio of the powder weight paraffin of weighing, temperature heat fused paraffin with 80～150 ℃, make wax water, powder stirred in the wax water make slip, described molding procedure is with slip injection moulding mould, become the shape and size of base substrate requirement by die casting, the demoulding is standby then, described low temperature de-waxing operation is that the base substrate after the moulding is added in the saggar, around base substrate, fill with sorbent material, the saggar that base substrate will be housed is then put in the kiln and is carried out the low temperature de-waxing, binder burnout temperature control is at 100～200 ℃, time, control was at 8～16 hours, billet surface behind the de-waxing forms the hard cere shell of one deck, described high temperature firing process is that the base substrate that has the hard cere shell of one deck is directly put into high temperature sintering moulding in the kiln, firing temperature is at 1650～1700 ℃, and firing period was at 25～35 hours.
In the described low temperature de-waxing operation, when the base substrate wall thickness was 2～5mm, binder burnout temperature was controlled at 110 ℃～120 ℃, and the de-waxing soaking time was controlled at 8～10 hours.
In the described low temperature de-waxing operation, when the base substrate wall thickness was 6～10mm, binder burnout temperature was controlled at 150 ℃～160 ℃, and the de-waxing soaking time was controlled at 12～13 hours.
In the described low temperature de-waxing operation, at the base substrate wall thickness be＞during 10mm, binder burnout temperature is controlled at 180 ℃～200 ℃, and the de-waxing soaking time was controlled at 15～16 hours.
Compared with prior art, the beneficial effect that produces of the present invention is:
(1) low temperature binder burnout temperature control of the present invention is at 100～200 ℃, time, control was at 8～16 hours, compare high temperature de-waxing (1000 ℃ of binder burnout temperatures or higher in the prior art, the 40 hours de-waxing time or longer) or low temperature de-waxing (300 ℃ or 600～900 ℃ of binder burnout temperatures, 21 hours de-waxing time or 48 hours), binder burnout temperature is low, the de-waxing time is short, therefore more energy-conservation, evidence only is 10%～15% of former high temperature de-waxing operation power consumption at the power consumption of de-waxing operation.
(2) the present invention is owing to adopt 100～200 ℃ of low temperature de-waxing technologies, and temperature control is below the paraffin burning-point in the de-waxing process, and paraffin does not burn, thereby has solved the root that causes environmental pollution.
(3) behind the low temperature de-waxing of the present invention; owing at shell base substrate outside surface the hard protection that resembles burnt yellow or black cere shell of one deck is arranged; make airborne impurity can't enter the shell base substrate; thereby surface quality and the internal soundness of shell base substrate have been guaranteed; after the high temperature sintering moulding; electrovacuum ceramic tube envelope is assorted few, has improved the yield rate of product.
(4) behind the low temperature de-waxing of the present invention, electrovacuum ceramic tube envelope base substrate outside surface form one deck hard resemble burnt yellow or black cere shell, adhesion sorbent material, base substrate does not need repaired biscuit, can directly enter the high temperature sintering link, owing to cancelled the repaired biscuit operation, efficient is higher.
(5) the present invention utilizes and has mobile and plastic characteristics in the hot die-casting molding method after the paraffin slip heating and melting, do not need to carry out a large amount of facility investments, test, adjustment and control through processing parameter, just can produce the high quality vacuum ceramic cartridge, satisfy the technical requirements that high quality electrovacuum ceramics pipe uses, be more convenient for applying.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
The said preparation method of the present invention comprises that batching, ball milling and wax, moulding, low temperature de-waxing and high temperature burn till six procedures,
Described burden process be with contain the silicon-dioxide that weight percent is 93.5% aluminium sesquioxide, 3.2% calcium carbonate 1.%, 2% kaolin and surplus is that talcous raw material mixes,
Described ball milling operation is to adopt ball mill that above-mentioned batching is worn into 2～10 microns powder,
Described and wax operation is earlier according to 12%～16% ratio of the powder weight paraffin of weighing, and with 80～150 ℃ temperature heat fused paraffin, makes wax water, powder is stirred in the wax water make slip
Described molding procedure is with slip injection moulding mould, becomes the shape and size of base substrate requirement by die casting, and the demoulding is standby then,
Described low temperature de-waxing operation is that the base substrate after the moulding is added in the saggar, around base substrate, fill with sorbent material, the saggar that base substrate will be housed is then put in the kiln, when the base substrate wall thickness was 2～5mm, binder burnout temperature was controlled at 110 ℃～120 ℃, and soaking time was controlled at 8～10 hours, can in base substrate, discharge paraffin outside the base substrate, take out the base substrate behind the de-waxing this moment from saggar, as seen the base substrate outside surface form one deck hard resemble burnt orange cere shell
Described high temperature firing process is, will have the hard electrovacuum ceramic tube envelope base substrate that resembles burnt orange cere shell of one deck and directly advance in the pushed bat kiln, and the high temperature sintering moulding, firing temperature is at 1650～1700 ℃, and firing period was at 25～35 hours.
Embodiment 2
Identical with six procedures of embodiment 1, difference is, in the described low temperature de-waxing operation, when base substrate thickness is 6～10mm, binder burnout temperature control is at 150 ℃～160 ℃, and soaking time was controlled at 12～13 hours, can discharge paraffin outside the base substrate in base substrate, take out the base substrate behind the de-waxing this moment from saggar, as seen the base substrate outside surface form one deck hard resemble burnt orange cere shell.
Embodiment 3
Identical with six procedures of embodiment 1, difference is, in the described low temperature de-waxing operation, at base substrate thickness be＞during 10mm, binder burnout temperature control is at 180 ℃～200 ℃, and soaking time was controlled at 15～16 hours, can discharge paraffin outside the base substrate in base substrate, take out the base substrate behind the de-waxing this moment from saggar, as seen the base substrate outside surface form one deck hard resemble burnt orange or black cere shell.
Claims (4)
1. the preparation method of an electrovacuum ceramics pipe, comprise batching, ball milling, and wax, moulding, low temperature de-waxing and high temperature burn till six procedures, described burden process is to be 93.5% aluminium sesquioxide with containing weight percent, the silicon-dioxide of 3.5% calcium carbonate 1.37%, 2% kaolin and surplus are that talcous raw material mixes, described ball milling operation is to adopt ball mill batching to be worn into 2～10 microns powder, described and wax operation is earlier according to 12%～16% ratio of the powder weight paraffin of weighing, temperature heat fused paraffin with 80～150 ℃, make the wax slurry, powder stirred in the wax slurry make slip, described molding procedure is with slip injection moulding mould, become the shape and size of base substrate requirement by die casting, the demoulding is standby then, it is characterized in that, described low temperature de-waxing operation is that the base substrate after the moulding is added in the saggar, around base substrate, fill with sorbent material, the saggar that base substrate will be housed is then put in the kiln and is carried out the low temperature de-waxing, binder burnout temperature control is at 100～200 ℃, the control of de-waxing soaking time was at 8～16 hours, billet surface behind the de-waxing forms the hard cere shell of one deck, described high temperature firing process is that the base substrate that has the hard cere shell of one deck is directly put into high temperature sintering moulding in the kiln, firing temperature is at 1650～1700 ℃, and firing period was at 25～35 hours.
2. according to the preparation method of the described a kind of electrovacuum ceramics pipe of claim 1, it is characterized in that in the described low temperature de-waxing operation, when the base substrate wall thickness was 2～5mm, binder burnout temperature was controlled at 110 ℃～120 ℃, the de-waxing soaking time was controlled at 8～10 hours.
3. according to the preparation method of the described a kind of electrovacuum ceramics pipe of claim 1, it is characterized in that: in described low temperature de-waxing operation, when base substrate thickness was 6～10mm, binder burnout temperature was controlled at 150 ℃～160 ℃, and the de-waxing soaking time was controlled at 12～13 hours.
4. according to the preparation method of the described a kind of electrovacuum ceramics pipe of claim 1, it is characterized in that, in the described low temperature de-waxing operation, at base substrate thickness be＞during 10mm, binder burnout temperature is controlled at 180 ℃～200 ℃, and the de-waxing soaking time was controlled at 15～16 hours.
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| CN103073271A (en) * | 2011-11-18 | 2013-05-01 | 常熟市创新陶瓷有限公司 | High-abrasion-resistance high-temperature-resistance ceramic |
| CN102407291B (en) * | 2011-12-06 | 2013-06-05 | 辽宁速航特铸材料有限公司 | Method for manufacturing ceramic cores through two-stage burying sintering |
| CN103011781B (en) * | 2012-12-26 | 2015-01-28 | 成都旭光电子股份有限公司 | Ceramic for electrical vacuum device and preparation method thereof |
| CN103224387A (en) * | 2013-05-02 | 2013-07-31 | 湖南泰鑫瓷业有限公司 | AL2O3-Fe base ceramic composite material and production method thereof |
| CN106187070A (en) * | 2015-05-09 | 2016-12-07 | 新化县湘港兴科陶瓷发展有限公司 | A kind of production technology of earthenware |
| CN106621846B (en) * | 2017-01-13 | 2019-05-10 | 江西博鑫精陶环保科技有限公司 | A kind of full ceramic filter membrane component of hollow plate and its process of preparing |
| CN107599151B (en) * | 2017-10-23 | 2022-12-30 | 浙江新光阳照明股份有限公司 | Production line for ceramic tubes |
| CN111662074A (en) * | 2020-06-23 | 2020-09-15 | 宜兴市奥米那陶瓷有限公司 | Process for preparing forming raw materials of thin-wall and slender products of alumina ceramics difficult to form |
| CN111916303A (en) * | 2020-09-04 | 2020-11-10 | 浙江瑞光真空电气有限公司 | Vacuum switch tube for circuit breaker and manufacturing method of shell of vacuum switch tube |
| CN113213895A (en) * | 2021-06-08 | 2021-08-06 | 宜兴市兴洲特种陶瓷厂(普通合伙) | Novel electric heating high-temperature-resistant ceramic tube and manufacturing method thereof |
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| CN1297862A (en) * | 2000-12-05 | 2001-06-06 | 龚建新 | Hot-pressing injection-molded alumina ceramic product and manufacturing method thereof |
| CN1182073C (en) * | 2002-09-30 | 2004-12-29 | 闻本良 | Injection formation technology for silicon carbide |
| CN101348372A (en) * | 2008-09-03 | 2009-01-21 | 山东硅苑新材料科技股份有限公司 | Production method of electrovacuum ceramic tube envelope |
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Address after: On the south side of the 121213 Jinzhou city of Liaoning Province Linghai Shuang Yang Zhen Zi Jing Cun Da Jin line Patentee after: LIAONING YINGGUAN HIGH-TECH CERAMIC CO., LTD. Address before: On the south side of the 121213 Jinzhou city of Liaoning Province Linghai Shuang Yang Zhen Zi Jing Cun Da Jin line Patentee before: Liaoning Yingguan Hi-Tech Ceramic Co., Ltd. |