CN103582193A - Instant ceramic heating tube and processing technology thereof - Google Patents

Instant ceramic heating tube and processing technology thereof Download PDF

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Publication number
CN103582193A
CN103582193A CN201210280046.4A CN201210280046A CN103582193A CN 103582193 A CN103582193 A CN 103582193A CN 201210280046 A CN201210280046 A CN 201210280046A CN 103582193 A CN103582193 A CN 103582193A
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Prior art keywords
ceramic
ceramic rod
aluminium oxide
rod
resistive film
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CN201210280046.4A
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Chinese (zh)
Inventor
刘文刚
晏育权
刘贤香
吴研
刘辉
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HUNAN XINHUA COUNTY QIRUI ELECTRONIC APPLIANCES Co Ltd
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HUNAN XINHUA COUNTY QIRUI ELECTRONIC APPLIANCES Co Ltd
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Priority to CN201210280046.4A priority Critical patent/CN103582193A/en
Publication of CN103582193A publication Critical patent/CN103582193A/en
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Abstract

The invention provides an instant ceramic heating tube comprising a ceramic rod and a resistive film. According to the resistive film, an aluminum oxide green tape serves as a substrate, and a tungsten metal heating circuit film is printed on the substrate. An external electrode is lead out through brazing of the tungsten metal heating circuit film. The aluminum oxide green type wraps the ceramic rod. The aluminum oxide green tape and the ceramic rod are fired together and form a whole. A preparation method of the instant ceramic heating tube comprises the steps that firstly, the ceramic rod and the resistive film are prepared, the ceramic rod is coated with the resistive film, hot-pressing and co-firing are conducted, and the instant ceramic heating tube is formed. The instant ceramic heating tube is simple and compact in structure, high in temperature rising speed, even in heating, resistant to corrosion, environmentally friendly, and capable of saving energy.

Description

A kind of Instant heating type ceramic heating pipe and processing technology
Technical field
The present invention relates to a kind of ceramic heater, be specifically related to a kind of Instant heating type ceramic heating pipe and processing technology thereof.
Background technology
At present, the complex structures such as the ordinary copper heating tube of existing use, retaining heater, combustion heater, volume is large, and programming rate is slow, and security performance is low, and energy consumption is large, and environmental-protecting performance is poor.Ceramic heater is the heater that a kind of High Efficiency Thermal is evenly distributed, and can guarantee that hot-face temperature is even, has eliminated focus and the cold spot of equipment, and has the advantages such as long-life, good heat insulating, strong, corrosion-resistant, the diamagnetic field of mechanical performance.Therefore be necessary to design a kind of Instant heating type ceramic heater, the current in the earthenware of flowing through are heated, supply with heating tube water heater and use.
Summary of the invention
Technical problem solved by the invention is to provide a kind of Instant heating type ceramic heating pipe and processing technology, thereby solves the problem in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A ceramic heating pipe, comprises ceramic rod and resistive film, and described resistive film is usingd aluminium oxide ceramic chips as substrate, and on substrate, prints tungsten metal heating circuit film, and external electrode is drawn in the soldering of described tungsten metal heating circuit film; Described aluminium oxide ceramic chips is coated on the outside of described ceramic rod, and burns altogether and form integral body with described ceramic rod.
As a kind of improvement, on described ceramic rod, be provided with ceramic flange.
A processing technology for Instant heating type ceramic heating pipe, comprises the steps.
S1. ceramic rod preparation
Described ceramic rod comprises the raw material of following weight portion:
Alpha-alumina 93.5
Suzhou soil 1.55
Calcium carbonate and SiO 2mixture 2.65
Yittrium oxide 0.3
Zirconia 2
The wax that adds 11.3 weight portions after above raw material mixing and ball milling is hot-forming at the temperature of 60 ℃, biscuiting is described ceramic rod at 1350 ℃.
Obviously, when prepared by described ceramic rod, also need to use other processing step, overall flow is: raw material processing-baking-batching-ball milling-add wax stir-to make the biscuiting-inspection of semifinished product of gatch-moulding-blank check-de-waxing.
S2. resistive film preparation
The aluminium oxide ceramic chips of resistive film comprises the raw material of following weight portion:
Alpha-alumina 93-96
Suzhou soil 1-2
Calcium carbonate 1-3
Adhesive 2-3
First in above-mentioned raw materials powder, add the porcelain of the deionized water of 15 weight portions, the zirconium dioxide of 12 weight portions and 7.5 weight portions to carry out mix grinding for the first time, obtain slurry, after slurry ball milling 6h, cross 270 mesh sieves, in the slurry of 10-20 ℃ of refrigeration, add again dimethylbenzene/n-butanol intermixture of 10 weight portions to carry out for the second time ball milling 18 hours, and add defrother to carry out vacuum stirring 30 minutes, de-bubble, technique flow casting molding is made aluminium oxide ceramic chips routinely.
Described adhesive comprises polyvinyl alcohol.
Described defrother comprises tributyl phosphate.
Described porcelain is commercially available, and for example the porcelain that porcelain Co., Ltd produces is upgraded in Jiyuan City.
Overall flow is: the configuration-barreling-refrigeration-ball milling-froth in vacuum-flow casting molding-section-check of adhesive configuration-slurry.
Take aluminium oxide ceramic chips as substrate, print tungsten metal heating circuit film thereon.
S3. ceramic rod is combined with resistive film
The aluminium oxide ceramic chips substrate resistance film making is coated on to the outside of described ceramic rod, hot pressing, then at 1500 ℃ of temperature, burns altogether, both are integrally combined.
Obviously, the present invention also needs through follow-up check, ceramic flange is installed, the soldering of tungsten metal heating circuit film is drawn to the steps such as external electrode, test and packing warehouse-in, because above-mentioned steps all adopts common process, at this, does not repeat.
In the present invention, the crystalline phase of described ceramic rod becomes corundum, mullite, ZrO 2crystal grain.
As a kind of improvement, control the crystalline phase growth in described ceramic rod, in described ceramic rod, the crystalline phase part by weight of corundum and described mullite is 3:1, and the crystalline phase weight of described corundum is no more than 55% of ceramic rod weight, the crystalline phase weight of described mullite is no less than 10% of ceramic rod weight, described ZrO 2the crystalline phase weight of crystal grain is the 1-10% of ceramic rod weight, thereby ceramic rod has good sintering character and thermal coefficient of expansion.
In the present invention, the mixed solvent dimethylbenzene/n-butanol of 10 weight portions that adulterate in the preparation of aluminium oxide ceramic chips, the wettability of slurry is best, and the suspendability of slurry and rheological property are best.
In ceramic rod provided by the invention, the crystallite dimension 1-2 μ m of corundum, mullite is needle-like, fails to grow up in 10 μ m.Corundum and mullite are principal crystalline phase, ZrO 2for inferior crystalline phase, the mullite crystalline substance of needle-like is woven into netted, becomes the crystalline framework of porcelain, corundum and ZrO 2uniform crystal particles is distributed in porcelain body.Due under different temperatures, ZrO 2with three kinds of paramorphs, exist, i.e. cubic system, tetragonal crystal system, monoclinic system, the conversion of monoclinic system and tetragonal crystal system is attended by 1% change in volume, during heating, by monocline, turns m-ZrO 2become cubic t-ZrO 2, volume contraction, when cooling by t-ZrO 2change m-ZrO into 2volumetric expansion.But this contraction does not occur in same temperature with expanding, the former is about 1200 ℃, and the latter is about 1000 ℃, therefore, and in order to obtain ZrO 2transformation toughening and quality structure, inventor has designed lowest total of the melting point firing temperature at 1350 ℃, and adds 0.3% yittrium oxide and do sintering aid, can guarantee ZrO like this 2all change Tetragonal t-ZrO into 2, after burning till, when temperature is down to 1000 ℃, the glassy phase in porcelain body is firm, t-ZrO 2particle dispersion is in porcelain matrix, because both have different thermal coefficient of expansions, t-ZrO 2brilliant ladder grain has different stressing conditions around, when it is subject to constraining of matrix, ZrO 2phase transformation also will be suppressed, thereby reach formula Design object, and interactive flexibly.Thereby starting preparation 95% aluminium oxide ceramics is low temperature formula and the low-temperature sintering new technology of hot pin, and can match with tungsten metal paste.
In the aluminium oxide ceramic chips preparation process of resistive film of the present invention, mixed solvent dimethylbenzene/n-butanol is best to the wettability of powder, the suspendability of powder and slurry rheological property can be best, thereby prepare the aluminium oxide ceramic chips that is applicable to curtain coating and high-power circuit use insulated substrate.Not only work simplification of this ceramics preparation method, composition is easy to control, and density rapid growth during sintering shifts to higher temperature, is conducive to burnout from the organic substance of raw cook and slurry and reduces the high temperature deformation of substrate.Meanwhile, this aluminium oxide ceramic chips has moderate dielectric constant, lower dielectric loss, the less characteristics such as temperature coefficient, can meet ceramic dielectric and other power circuit board serviceability and technological requirement.
Owing to having adopted above structure, the present invention has following beneficial effect:
The present invention is simple and compact for structure, and volume is little; Programming rate is fast, and heating-up temperature reaches as high as 950 ℃; Homogeneous heating, rapid heat dissipation; The adstante febre flames of anger, is used safety; Heating circuit and air are isolated, element acid and alkali-resistance and other corrosive substances; Element itself and production process meet environmental requirement; The harmful substances such as not leaded, mercury, cadmium, Cr VI, poly-dibromodiphenyl ether, benzene, meet the environmental requirement of European Union (ROHS and WEEE).
Safety of the present invention, environmental protection, energy-conservation, market prospects are large.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
In figure: 1. ceramic rod, 2. resistive film, 3. aluminium oxide ceramic chips, 4. tungsten metal heating circuit film, 5. external electrode, 6. ceramic flange.
Embodiment
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Referring to Fig. 1, a kind of Instant heating type ceramic heating pipe, comprises ceramic rod 1 and resistive film 2, and described resistive film 2 is usingd aluminium oxide ceramic chips 3 as substrate, and on substrate, prints tungsten metal heating circuit film 4, and external electrode 5 is drawn in 4 solderings of described tungsten metal heating circuit film; Described aluminium oxide ceramic chips 3 is coated on the outside of described ceramic rod 1, and burns altogether and form integral body with described ceramic rod 1.
In the present invention, on described ceramic rod 1, be provided with ceramic flange 6.
Embodiment 1
A processing technology for Instant heating type ceramic heating pipe, comprises the steps:
S1. ceramic rod preparation
Described ceramic rod comprises following raw material:
Alpha-alumina 93.5kg
Suzhou soil 1.55kg
Calcium carbonate and SiO 2mixture 2.65kg
Yittrium oxide 0.3kg
Zirconia 2kg
The overall flow of processing step is: raw material processing-baking-batching-ball milling-add wax stir-to make the biscuiting-inspection of semifinished product of gatch-moulding-blank check-de-waxing, wherein, after raw material mixing and ball milling, add that the wax of 11.3kg is hot-forming at the temperature of 60 ℃, biscuiting is described ceramic rod at 1350 ℃;
S2. resistive film preparation
The aluminium oxide ceramic chips of resistive film comprises following raw material:
Alpha-alumina 93kg
Suzhou soil 1kg
Calcium carbonate 1kg
Adhesive polyethylene alcohol 2kg
First in above-mentioned raw materials powder, add the porcelain of the deionized water of 15kg, the zirconium dioxide of 12kg and 7.5kg to carry out mix grinding for the first time, obtain slurry, after slurry ball milling 6h, cross 270 mesh sieves, in the slurry of 10 ℃ of refrigerations, add again dimethylbenzene/n-butanol intermixture of 10 weight portions to carry out for the second time ball milling 18 hours, and add defrother tributyl phosphate to carry out vacuum stirring 30 minutes, de-bubble, technique flow casting molding is made aluminium oxide ceramic chips routinely; Overall flow is: the configuration-barreling-refrigeration-ball milling-froth in vacuum-flow casting molding-section-check of adhesive configuration-slurry; Then take aluminium oxide ceramic chips as substrate, print tungsten metal heating circuit film thereon;
S3. ceramic rod is combined with resistive film
The aluminium oxide ceramic chips substrate resistance film making is coated on to the outside of described ceramic rod, hot pressing, then at 1500 ℃ of temperature, burns altogether, both are integrally combined.
Finally by later continuous check, ceramic flange is installed, the soldering of tungsten metal heating circuit film is drawn to external electrode, test, final packaging warehouse-in.
The crystalline phase of the ceramic rod that the present embodiment is produced becomes corundum, mullite, ZrO 2crystal grain, in described ceramic rod, the crystalline phase part by weight of corundum and described mullite is 3:1, and the crystalline phase weight of described corundum is 55% of ceramic rod weight, and the crystalline phase weight of described mullite is 10% of ceramic rod weight, described ZrO 2the crystalline phase weight of crystal grain is 1% of ceramic rod weight, and ceramic rod has good sintering character and thermal coefficient of expansion.
Embodiment 2
A processing technology for Instant heating type ceramic heating pipe, comprises the steps:
S1. ceramic rod preparation
Described ceramic rod comprises following raw material:
Alpha-alumina 93.5kg
Suzhou soil 1.55kg
Calcium carbonate and SiO 2mixture 2.65kg
Yittrium oxide 0.3kg
Zirconia 2kg
The overall flow of processing step is: raw material processing-baking-batching-ball milling-add wax stir-to make the biscuiting-inspection of semifinished product of gatch-moulding-blank check-de-waxing, wherein, after raw material mixing and ball milling, add that the wax of 11.3kg is hot-forming at the temperature of 60 ℃, biscuiting is described ceramic rod at 1350 ℃;
S2. resistive film preparation
The aluminium oxide ceramic chips of resistive film comprises following raw material:
Alpha-alumina 96kg
Suzhou soil 2kg
Calcium carbonate 3kg
Adhesive polyethylene alcohol 3kg
First in above-mentioned raw materials powder, add the porcelain of the deionized water of 15kg, the zirconium dioxide of 12kg and 7.5kg to carry out mix grinding for the first time, after slurry ball milling 6h, cross 270 mesh sieves, in the slurry of 20 ℃ of refrigerations, add again dimethylbenzene/n-butanol intermixture of 10 weight portions to carry out for the second time ball milling 18 hours, and add defrother tributyl phosphate to carry out vacuum stirring 30 minutes, de-bubble, technique flow casting molding is made aluminium oxide ceramic chips routinely; Overall flow is: the configuration-barreling-refrigeration-ball milling-froth in vacuum-flow casting molding-section-check of adhesive configuration-slurry; Then take aluminium oxide ceramic chips as substrate, print tungsten metal heating circuit film thereon;
S3. ceramic rod is combined with resistive film
The aluminium oxide ceramic chips substrate resistance film making is coated on to the outside of described ceramic rod, hot pressing, then at 1500 ℃ of temperature, burns altogether, both are integrally combined.
Finally by later continuous check, ceramic flange is installed, the soldering of tungsten metal heating circuit film is drawn to external electrode, test, final packaging warehouse-in.
The crystalline phase of the ceramic rod that the present embodiment is produced becomes corundum, mullite, ZrO 2crystal grain, in described ceramic rod, the crystalline phase part by weight of corundum and described mullite is 3:1, and the crystalline phase weight of described corundum is 50% of ceramic rod weight, and the crystalline phase weight of described mullite is 12% of ceramic rod weight, described ZrO 2the crystalline phase weight of crystal grain is 10% of ceramic rod weight, and ceramic rod has good sintering character and thermal coefficient of expansion.
Embodiment 3
A processing technology for Instant heating type ceramic heating pipe, comprises the steps:
S1. ceramic rod preparation
Described ceramic rod comprises following raw material:
Alpha-alumina 93.5kg
Suzhou soil 1.55kg
Calcium carbonate and SiO 2mixture 2.65kg
Yittrium oxide 0.3kg
Zirconia 2kg
The overall flow of processing step is: raw material processing-baking-batching-ball milling-add wax stir-to make the biscuiting-inspection of semifinished product of gatch-moulding-blank check-de-waxing, wherein, after raw material mixing and ball milling, add that the wax of 11.3kg is hot-forming at the temperature of 60 ℃, biscuiting is described ceramic rod at 1350 ℃;
S2. resistive film preparation
The aluminium oxide ceramic chips of resistive film comprises following raw material:
Alpha-alumina 95kg
Suzhou soil 1.5kg
Calcium carbonate 2kg
Adhesive polyethylene alcohol 2.5kg
First in above-mentioned raw materials powder, add the porcelain of the deionized water of 15kg, the zirconium dioxide of 12kg and 7.5kg to carry out mix grinding for the first time, after slurry ball milling 6h, cross 270 mesh sieves, in the slurry of 15 ℃ of refrigerations, add again dimethylbenzene/n-butanol intermixture of 10 weight portions to carry out for the second time ball milling 18 hours, and add defrother tributyl phosphate to carry out vacuum stirring 30 minutes, de-bubble, technique flow casting molding is made aluminium oxide ceramic chips routinely; Overall flow is: the configuration-barreling-refrigeration-ball milling-froth in vacuum-flow casting molding-section-check of adhesive configuration-slurry; Then take aluminium oxide ceramic chips as substrate, print tungsten metal heating circuit film thereon;
S3. ceramic rod is combined with resistive film
The aluminium oxide ceramic chips substrate resistance film making is coated on to the outside of described ceramic rod, hot pressing, then at 1500 ℃ of temperature, burns altogether, both are integrally combined.
Finally by later continuous check, ceramic flange is installed, the soldering of tungsten metal heating circuit film is drawn to external electrode, test, final packaging warehouse-in.
The crystalline phase of the ceramic rod that the present embodiment is produced becomes corundum, mullite, ZrO 2crystal grain, in described ceramic rod, the crystalline phase part by weight of corundum and described mullite is 3:1, and the crystalline phase weight of described corundum is 55% of ceramic rod weight, and the crystalline phase weight of described mullite is 13% of ceramic rod weight, described ZrO 2the crystalline phase weight of crystal grain is 8% of ceramic rod weight, and ceramic rod has good sintering character and thermal coefficient of expansion.
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof
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.

Claims (5)

1. an Instant heating type ceramic heating pipe, comprises ceramic rod and resistive film, it is characterized in that: described resistive film is usingd aluminium oxide ceramic chips as substrate, and on substrate, prints tungsten metal heating circuit film, and external electrode is drawn in the soldering of described tungsten metal heating circuit film; Described aluminium oxide ceramic chips is coated on the outside of described ceramic rod, and burns altogether and form integral body with described ceramic rod.
2. a kind of Instant heating type ceramic heating pipe as claimed in claim 1, is characterized in that: on described ceramic rod, be provided with ceramic flange.
3. a processing technology for Instant heating type ceramic heating pipe as claimed in claim 1, is characterized in that: comprise the steps:
S1. ceramic rod preparation
Described ceramic rod comprises the raw material of following weight portion:
Alpha-alumina 93.5
Suzhou soil 1.55
Calcium carbonate and SiO 2mixture 2.65
Yittrium oxide 0.3
Zirconia 2
The wax that adds 11.3 weight portions after above raw material mixing and ball milling is hot-forming at the temperature of 60 ℃, biscuiting is described ceramic rod at 1350 ℃;
S2. resistive film preparation
The aluminium oxide ceramic chips of resistive film comprises the raw material of following weight portion:
Alpha-alumina 93-96
Suzhou soil 1-2
Calcium carbonate 1-3
Adhesive 2-3
First in above-mentioned raw materials powder, add the porcelain of the deionized water of 15 weight portions, the zirconium dioxide of 12 weight portions and 7.5 weight portions to carry out mix grinding for the first time, after slurry mix grinding 6h, cross 270 mesh sieves, in the slurry of 10-20 ℃ of refrigeration, add again dimethylbenzene/n-butanol intermixture of 10 weight portions to carry out for the second time ball milling 18 hours, and add defrother to carry out vacuum stirring 30 minutes, de-bubble, flow casting molding is made aluminium oxide ceramic chips; Take aluminium oxide ceramic chips as substrate, print tungsten metal heating circuit film thereon;
S3. ceramic rod is combined with resistive film
The aluminium oxide ceramic chips substrate resistance film making is coated on to the outside of described ceramic rod, hot pressing, then at 1500 ℃ of temperature, burns altogether, both are integrally combined.
4. an Instant heating type ceramic heat pipe processing technique as claimed in claim 3, is characterized in that: in step S2, described adhesive comprises polyvinyl alcohol.
5. an Instant heating type ceramic heat pipe processing technique as claimed in claim 3, is characterized in that: in step S2, described defrother comprises tributyl phosphate.
CN201210280046.4A 2012-08-08 2012-08-08 Instant ceramic heating tube and processing technology thereof Pending CN103582193A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104027831A (en) * 2014-06-26 2014-09-10 胡积献 Essential oil sustained-release catalyzing device and air fragrance machine applying same
CN104185317A (en) * 2014-08-14 2014-12-03 厦门格睿伟业电子科技有限公司 Double-layer cladding ceramic heating pipe
CN107318179A (en) * 2017-07-20 2017-11-03 湖北国瓷科技有限公司 A kind of method that toughened aluminum oxide makes high temperature co-firing heat-generating pipe
CN109028943A (en) * 2018-06-28 2018-12-18 珠海华宇宏瑞科技有限公司 A kind of connection method of cermet heating element and flange
CN110818394A (en) * 2019-11-13 2020-02-21 嘉兴艾尔格电热技术有限公司 Production process and manufacturing method of ceramic heating ring
CN111278179A (en) * 2020-03-30 2020-06-12 余昆龙 Liquid heater and composite ceramic tube formula
CN114180943A (en) * 2020-09-15 2022-03-15 日本碍子株式会社 Composite sintered body, semiconductor manufacturing apparatus member, and method for manufacturing composite sintered body

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CN201403215Y (en) * 2009-03-31 2010-02-10 福建闽航电子有限公司 Ceramic heating rod
CN102281653A (en) * 2011-05-13 2011-12-14 黄本香 Liquid heating rod provided with electric heating film heating tube
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DE19615243C1 (en) * 1996-04-18 1997-08-28 Manfried Steinmetz Ceramic electrical infrared radiant heater of rod or bar shape e.g for cooker element
EP1051371B1 (en) * 1998-12-04 2004-09-01 Robert Bosch Gmbh Sintered stick-shaped heater
JP2001126852A (en) * 1999-10-26 2001-05-11 Ngk Spark Plug Co Ltd Method of manu7facturing ceramic heater
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104027831A (en) * 2014-06-26 2014-09-10 胡积献 Essential oil sustained-release catalyzing device and air fragrance machine applying same
CN104185317A (en) * 2014-08-14 2014-12-03 厦门格睿伟业电子科技有限公司 Double-layer cladding ceramic heating pipe
CN104185317B (en) * 2014-08-14 2016-09-07 厦门格睿伟业电子科技有限公司 A kind of double-deck bag pressure ceramic heating tube
CN107318179A (en) * 2017-07-20 2017-11-03 湖北国瓷科技有限公司 A kind of method that toughened aluminum oxide makes high temperature co-firing heat-generating pipe
CN109028943A (en) * 2018-06-28 2018-12-18 珠海华宇宏瑞科技有限公司 A kind of connection method of cermet heating element and flange
CN110818394A (en) * 2019-11-13 2020-02-21 嘉兴艾尔格电热技术有限公司 Production process and manufacturing method of ceramic heating ring
CN111278179A (en) * 2020-03-30 2020-06-12 余昆龙 Liquid heater and composite ceramic tube formula
CN114180943A (en) * 2020-09-15 2022-03-15 日本碍子株式会社 Composite sintered body, semiconductor manufacturing apparatus member, and method for manufacturing composite sintered body
CN114180943B (en) * 2020-09-15 2023-06-27 日本碍子株式会社 Composite sintered body, semiconductor manufacturing device member, and method for manufacturing composite sintered body

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Application publication date: 20140212