CN101754497B - Silicon nitride heat generator and manufacturing method thereof - Google Patents

Silicon nitride heat generator and manufacturing method thereof Download PDF

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Publication number
CN101754497B
CN101754497B CN 201010044457 CN201010044457A CN101754497B CN 101754497 B CN101754497 B CN 101754497B CN 201010044457 CN201010044457 CN 201010044457 CN 201010044457 A CN201010044457 A CN 201010044457A CN 101754497 B CN101754497 B CN 101754497B
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silicon nitride
heat generating
parts
generating body
nitride heat
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CN101754497A (en
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邓湘凌
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贺连英
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Abstract

The invention provides a silicon nitride heat generator and a manufacturing method thereof. The silicon nitride heat generator comprises a heat generating source and a heat generating main body, wherein the heat generating source is a tungsten filament; the heat generating main body is prepared from the following components in part by weight: 88-92 parts of silicon nitride, 6.5-8.5 parts of aluminum oxide and 1.5-3.5 parts of yttrium oxide. The invention has the advantages that the manufacture processing is simple, and the operation process is easy to control; the silicon nitride heat generator manufactured by the method has higher qualified rate of the finished product, higher heat conducting property and higher heat efficiency; and the silicon nitride also has good thermal shock property.

Description

Silicon nitride heat generating body and preparation method thereof
Technical field
The present invention relates to thermo electric material, relate in particular to a kind of silicon nitride heat generating body and preparation method thereof.
Background technology
Having on the domestic market at present uses silicon nitride as instant electric water heater and the Instant heating type tap supply of heater.Quick electric water heater compared to gas heater and water-storage electric heater have that Fast Heating, sustainable heat supply water, volume are small and exquisite, safety and advantages such as environmental protection.The silicon nitride heat generating body firing rate is fast, and need not to wait for is sustainable use, so the water utilization rate almost is 100%, the power and energy saving, and heat-generating pipe is also less scaling, longer service life.
Existing silicon nitride heat generating body is generally a disposable heater that is sintered into one, for example, a kind of silicon nitride heat generating body and manufacture method thereof are disclosed in Chinese patent 99113534.2, adopting silicon nitride as the heating body, is pyrotoxin with the tungsten filament, forms through hot pressed sintering, the prescription following (percetage by weight) of its heating body: silicon nitride 82%~93%, alundum (Al 0.1%~5%, yttria 4%~8%, aluminium nitride 3%~5%.The heat conductivility of this silicon nitride heat generating body is also not too high, and the heat efficiency remains further to be improved, and its temperature range is also not too wide, and thermal shock performance also remains further to be improved.
The production method of silicon nitride heat generating body has two kinds now: the one, and adopt and in silicon nitride powder, bury heating wire, disposable sinter molding in mould then, the silicon nitride heat generating body that this technology is produced forms sintering stress easily, fraction defective height in the production process, and fracture easily in use.Another processing mode is the silicon nitride raw material upper surface printing Electric radiant Heating Film at software, and then carries out sintering, constitutes silicon nitride ceramics heating element, and silicon nitride raw material and Electric radiant Heating Film are when burning altogether, and atmosphere is restive, and qualification rate is low.
Summary of the invention
The objective of the invention is to, a kind of silicon nitride heat generating body is provided, it has high heat-conducting property, and its thermal shock performance is higher.
Another object of the present invention is to, a kind of manufacture method of above-mentioned silicon nitride heat generating body is provided, this method making flow process is simple, and process is easily controlled, and the silicon nitride heat generating body qualification rate height of producing, and has high heat-conducting property and thermal shock performance.
For being implemented in above-mentioned purpose, the invention provides a kind of silicon nitride heat generating body, it comprises: pyrotoxin and heating body, this pyrotoxin is tungsten filament, component and the content of described heating body are as follows, by weight: 88~92 parts of silicon nitrides, 6.5~8.5 parts of alundum (Als, 1.5~3.5 parts of yttrias.
The present invention also provides a kind of manufacture method of above-mentioned silicon nitride heat generating body, comprising:
Step 1, raw material preparation: the raw material of making the heating body is provided and is mixed with slurry;
Step 2, plain embryo forming: with prepared slurry injection moulding, make plain embryo with injection (mo(u)lding) machine;
Step 3, layout pyrotoxin: pyrotoxin is arranged in the corresponding position at a plain embryo, then another plain embryo alignment is buckled in this above element embryo, the combination of formin embryo;
Step 4, Vacuum Package: adopt plastic film that Vacuum Package is carried out in above-mentioned plain embryo combination;
Step 5, high temperature insostatic pressing (HIP): the plain embryo combination after the plastic film encapsulation is put in the isostatic pressing machine in 75~85 ℃ the hot pressing oil, and adds 95~105 atmospheric pressure, the little molten bonding of plastic cement;
Step 6, presintering: be heated to 560~600 ℃ earlier, vacuum degree is less than or equal to 20Pa, carries out the vacuum binder removal; Inflated with nitrogen is heated to 1400 ℃~1440 ℃ then;
Step 7, air pressure stove sintering: inflated with nitrogen under 4~5 atmospheric pressures, is heated to 1790~1830 ℃;
Step 8, cooling makes silicon nitride heat generating body.
Material component and the content of described heating body are as follows, by weight: 88~92 parts of silicon nitrides, 6.5~8.5 parts of alundum (Als, 1.5~3.5 parts of yttrias, 1.1~1.7 parts in paraffin, 1.1~1.7 parts of microwaxes, 0.1~0.3 part of stearin candle, 6.5~7.5 parts in plastic cement.
Described plain embryo is provided with accepting groove accommodating pyrotoxin, and this accepting groove is along a center line of plain embryo and is symmetrical arranged.
In the step 3, another plain embryo is provided with one of accepting groove simultaneously places facing to the plain embryo that is laid with pyrotoxin.
Described plastic cement is selected PE, PP, HIPS, PET a kind of or its combination wherein for use.
This pyrotoxin is a tungsten filament.
Described step 6 presintering: be heated to 580~600 ℃ earlier, vacuum degree is less than or equal to 20Pa, continues 9~11 hours, carries out the vacuum binder removal; Inflated with nitrogen is heated to 1400 ℃~1440 ℃ then, continues 5~7 hours.
Described step 7 air pressure stove sintering: inflated with nitrogen, under 5 atmospheric pressures, be heated to 1790~1830 ℃, continue 9~11 hours.
Beneficial effect of the present invention: silicon nitride heat generating body provided by the invention and preparation method thereof, it is made, and flow process is simple, operating process is easily controlled; The silicon nitride heat generating body that utilizes this method to make, the qualification rate of its finished product is higher, has high heat-conducting property, and the heat efficiency is higher, and this silicon nitride also has higher thermal shock performance simultaneously.
In order further to understand feature of the present invention and technology contents, see also following about detailed description of the present invention and accompanying drawing, yet accompanying drawing only provide with reference to and the explanation usefulness, the present invention is limited.
Description of drawings
Below in conjunction with accompanying drawing, by the specific embodiment of the present invention is described in detail, will make technical scheme of the present invention and other beneficial effect apparent.
In the accompanying drawing,
Fig. 1 is the flow chart of silicon nitride heat generating body manufacture method of the present invention;
The floor map of Fig. 2 plain embryo of the present invention.
Embodiment
For further setting forth technological means and the decorative effect thereof that the present invention takes, be described in detail below in conjunction with the preferred embodiments of the present invention and accompanying drawing thereof.
The invention provides a kind of silicon nitride heat generating body, it comprises: pyrotoxin and heating body, and this pyrotoxin is tungsten filament, component and the content of described heating body are as follows, by weight: 88~92 parts of silicon nitrides, 6.5~8.5 parts of alundum (Als,, 1.5~3.5 parts of yttrias
Shown in Figure 1), the present invention also provide a kind of silicon nitride heat generating body manufacture method (, this method comprises:
Step 1, raw material preparation: the raw material of making the heating body is provided and is mixed with slurry.Wherein, material component and the content of this heating body are as follows, by weight: 88~92 parts of silicon nitrides, 6.5~8.5 parts of alundum (Als, 1.5~3.5 parts of yttrias, 1.1~1.7 parts in paraffin, 1.1~1.7 parts of microwaxes, 0.1~0.3 part of stearin candle, 6.5~7.5 parts in plastic cement.In the present invention, this plastic cement can be selected PE, PP, HIPS, PET a kind of or its combination wherein for use.
Step 2, plain embryo forming: with prepared slurry injection moulding, make plain embryo 20 (shown in Figure 2) with injection (mo(u)lding) machine.Plain embryo is provided with accepting groove 22 accommodating pyrotoxin, and this accepting groove is along a center line of plain embryo and is symmetrical arranged.
Step 3, layout pyrotoxin: pyrotoxin is arranged in the corresponding position at a plain embryo, then another plain embryo alignment is buckled in this above element embryo, the combination of formin embryo, and this pyrotoxin is a tungsten filament.In step 3, another plain embryo is provided with one of accepting groove simultaneously places facing to the plain embryo that is laid with pyrotoxin.
Step 4, Vacuum Package: adopt plastic film that Vacuum Package is carried out in above-mentioned plain embryo combination.
Step 5, high temperature insostatic pressing (HIP): the plain embryo combination after the plastic film encapsulation is put in the isostatic pressing machine in 75~85 ℃ the hot pressing oil, and adds 95~105 atmospheric pressure, the little molten bonding of plastic cement.
Step 6, presintering: be heated to 560~600 ℃ earlier, preferred 580~600 ℃, vacuum degree is less than or equal to 20Pa, continues 9~11 hours, carries out the vacuum binder removal; Inflated with nitrogen is heated to 1400 ℃~1440 ℃ then, continues 5~7 hours.
Step 7, air pressure stove sintering: inflated with nitrogen, under 4~5 atmospheric pressures, be heated to 1790~1830 ℃, continue 9~11 hours.
Step 8, cooling makes silicon nitride heat generating body.
In sum, silicon nitride heat generating body provided by the invention and preparation method thereof, it is made, and flow process is simple, operating process is easily controlled; The silicon nitride heat generating body that utilizes this method to make, the qualification rate of its finished product is higher, has high heat-conducting property, and the heat efficiency is higher, and this silicon nitride also has higher thermal shock performance simultaneously.
The above; for the person of ordinary skill of the art; can make other various corresponding changes and distortion according to technical scheme of the present invention and technical conceive, and all these changes and distortion all should belong to the protection range of accompanying Claim of the present invention.

Claims (7)

1. the manufacture method of a silicon nitride heat generating body is characterized in that, comprising:
Step 1, raw material preparation: the raw material of making the heating body is provided and is mixed with slurry; Material component and the content of described heating body are as follows, by weight: 88~92 parts of silicon nitrides, 6.5~8.5 parts of alundum (Als, 1.5 ~ 3.5 parts of yttrias, 1.1~1.7 parts in paraffin, 1.1~1.7 parts of microwaxes, 0.1~0.3 part of stearin candle, 6.5~7.5 parts in plastic cement;
Step 2, plain embryo forming: with prepared slurry injection moulding, make plain embryo with injection (mo(u)lding) machine;
Step 3, layout pyrotoxin: pyrotoxin is arranged in the corresponding position at a plain embryo, then another plain embryo alignment is buckled in this above element embryo, the combination of formin embryo;
Step 4, Vacuum Package: adopt plastic film that Vacuum Package is carried out in above-mentioned plain embryo combination;
Step 5, high temperature insostatic pressing (HIP): the plain embryo combination after the plastic film encapsulation is put in the isostatic pressing machine in 75~85 ℃ the hot pressing oil, and adds 95~105 atmospheric pressure, the little molten bonding of plastic cement;
Step 6, presintering: be heated to 560 ~ 600 ℃ earlier, vacuum degree is less than or equal to 20Pa, carries out the vacuum binder removal; Inflated with nitrogen is heated to 1400 ℃~1440 ℃ then;
Step 7, air pressure stove sintering: inflated with nitrogen under 4 ~ 5 atmospheric pressures, is heated to 1790 ~ 1830 ℃;
Step 8, cooling makes silicon nitride heat generating body.
2. the manufacture method of silicon nitride heat generating body as claimed in claim 1 is characterized in that, described plain embryo is provided with accepting groove accommodating pyrotoxin, and this accepting groove is along a center line of plain embryo and is symmetrical arranged.
3. the manufacture method of silicon nitride heat generating body as claimed in claim 2 is characterized in that, in the step 3, another plain embryo is provided with one of accepting groove simultaneously places facing to the plain embryo that is laid with pyrotoxin.
4. the manufacture method of silicon nitride heat generating body as claimed in claim 1 is characterized in that, described plastic cement is selected PE, PP, HIPS, PET a kind of or its combination wherein for use.
5. the manufacture method of silicon nitride heat generating body as claimed in claim 1 is characterized in that, this pyrotoxin is a tungsten filament.
6. the manufacture method of silicon nitride heat generating body as claimed in claim 1 is characterized in that, described step 6 presintering: be heated to 580 ~ 600 ℃ earlier, vacuum degree is less than or equal to 20Pa, continues 9 ~ 11 hours, carries out the vacuum binder removal; Inflated with nitrogen is heated to 1400 ℃~1440 ℃ then, continues 5 ~ 7 hours.
7. the manufacture method of silicon nitride heat generating body as claimed in claim 1 is characterized in that, described step 7 air pressure stove sintering: inflated with nitrogen, under 5 atmospheric pressures, be heated to 1790 ~ 1830 ℃, and continue 9 ~ 11 hours.
CN 201010044457 2010-01-20 2010-01-20 Silicon nitride heat generator and manufacturing method thereof Expired - Fee Related CN101754497B (en)

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Publication number Priority date Publication date Assignee Title
CN102329134A (en) * 2010-07-12 2012-01-25 邓湘凌 Manufacturing method of silicon nitride heating plate
CN101945506A (en) * 2010-08-17 2011-01-12 钟秉霖 Ceramic energy heating element
CN102300347B (en) * 2011-07-13 2012-12-05 邓湘凌 Silicon nitride composite heat-generation body and manufacturing method thereof
CN102595665B (en) * 2012-02-28 2014-07-09 威海兴泰金属制造有限公司 Silicon nitride heating sheet and manufacturing method thereof
CN104446507A (en) * 2014-11-19 2015-03-25 东莞市国研电热材料有限公司 Manufacturing method of ceramic heating element and ceramic heating element
CN106493370A (en) * 2016-10-21 2017-03-15 邓湘凌 Without preparation method of the magnetic without nickel metal furnishings
CN106518089B (en) * 2016-11-25 2019-05-14 中国工程物理研究院材料研究所 A kind of preparation method of high performance and big size silicon nitride ceramic material
CN108264359B (en) * 2018-01-26 2019-09-17 东莞市日进德新材料技术有限公司 Ceramic heating element and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1229829A (en) * 1999-03-15 1999-09-29 广州石潮高性能陶瓷总公司 Silicon nitride heat generating body and its prodn. method
CN1412268A (en) * 2001-10-09 2003-04-23 刘庆昌 Nano-grade silicon nitride composite material heating body and its production process
CN1849017A (en) * 2005-04-05 2006-10-18 郜长福 Silicon nitride heating body and its pressureless lower temperature sintering producing method
CN101318822A (en) * 2008-07-04 2008-12-10 冷水江市明玉陶瓷工具有限责任公司 Silicon nitride composite ceramics heater

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1229829A (en) * 1999-03-15 1999-09-29 广州石潮高性能陶瓷总公司 Silicon nitride heat generating body and its prodn. method
CN1412268A (en) * 2001-10-09 2003-04-23 刘庆昌 Nano-grade silicon nitride composite material heating body and its production process
CN1849017A (en) * 2005-04-05 2006-10-18 郜长福 Silicon nitride heating body and its pressureless lower temperature sintering producing method
CN101318822A (en) * 2008-07-04 2008-12-10 冷水江市明玉陶瓷工具有限责任公司 Silicon nitride composite ceramics heater

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