CN102612180A - Dry-point silicon nitride electric heating element and manufacturing method thereof - Google Patents
Dry-point silicon nitride electric heating element and manufacturing method thereof Download PDFInfo
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- CN102612180A CN102612180A CN2012100772900A CN201210077290A CN102612180A CN 102612180 A CN102612180 A CN 102612180A CN 2012100772900 A CN2012100772900 A CN 2012100772900A CN 201210077290 A CN201210077290 A CN 201210077290A CN 102612180 A CN102612180 A CN 102612180A
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Abstract
The invention discloses a dry-point silicon nitride electric heating element and a manufacturing method. The dry-point silicon nitride electric heating element consists of a heating source and a heating body. The heating body comprises the following components: by weight percentage, 85-96% of nanometer silicon nitride, 1-4% of aluminum oxide and 4-8% of yttria, and is formed by preparing the components, making biscuit and sintering and the like. The dry-point silicon nitride electric heating element is resistant to high temperature and corrosion and excellent in thermohardening and wear resistance and can work for long time at the temperature within 1200 DEG C.
Description
Technical field
The present invention relates to thermo electric material, especially a kind of type silicon nitride electric heating element and manufacturing approach thereof done.
Background technology
The electric heating element that in the air field, heats at present both at home and abroad all is that they all have a common shortcoming with resistance wire, metal tube, silicon carbon material, PTC and coating heating: useful life is short, security reliability is low, poor corrosion resistance and resistance wire, metal tube, PTC can't use in hot environment.
Summary of the invention
In order to solve above-mentioned technical deficiency, the purpose of this invention is to provide a kind of type silicon nitride electric heating element of doing, it is corrosion-resistant, high temperature resistant, life-span length, safe and reliable.
Another object of the present invention provides the above-mentioned manufacturing approach of doing type silicon nitride electric heating element.
The object of the invention can be realized in the following manner:
A kind of type silicon nitride electric heating element of doing; Be made up of pyrotoxin and heating body, it is characterized in that: count by weight percentage, the prescription of said heating body comprises following component: nano-silicon nitride 85%-96%; Alundum (Al 1%-4%, yttria 4%-8%.
Described pyrotoxin is a tungsten filament.
Described nano-silicon nitride particle size range is between 40-60nm.
The above-mentioned manufacturing approach of doing type silicon nitride electric heating element is characterized in that may further comprise the steps:
(1) preparation of raw material: by above-mentioned prescription weighing, ball milling is dried, sieves to such an extent that powder is for use;
(2) biscuit is made: through die forming, it is for use that biscuit is taken out in form removal with pyrotoxin, above-mentioned powder;
(3) sintering: biscuit is packed in the graphite mo(u)ld, put into the hot pressing furnace sintering then, sintering process is: in 20-40 minute, be heated to 900-1015 ℃ under the normal temperature; Continue to heat up and begin pressurization, in 30-120 minute, be heated to 1700-1800 ℃, kept 5-60 minute; Then; In 5-60 minute, be cooled to 1300-1700 ℃, rose to 1700-1800 ℃ at 5-30 minute and kept 5-60 minute, last natural cooling, release.
It is raw material that the present invention adopts nano silicon nitride powders, alundum (Al, yttria, form through hot pressed sintering, so it has following performance:
1, high temperature resistant: can long-term work in interior environment at 1200 ℃;
2, corrosion-resistant: silicon nitride electric heating element of the present invention carries out boiling test in 6 hours in 30% sodium hydroxide solution, average corrosion rate is 0.43g/m
2H carries out boiling test in 6 hours in 5% sulfuric acid solution, average corrosion rate is 9.21g/m
2H.And stainless steel rate of corrosion under equivalent environment reaches 81-121g/m
2H.So the soda acid ability of silicon nitride material of the present invention is far longer than metal material;
3, thermohardening, anti-wear performance are good: the hardness of silicon nitride material is higher than any metal material, is only second to diamond and can reduce hardness because ambient temperature raises at 1000 ℃ with interior work, thus silicon nitride material not only good, the high-temperature self-lubrication superior performance of thermohardening and resistance to wear are splendid.
4, comprehensive complete above-mentioned performance, silicon nitride material of the present invention are not only to be used for the electric heating element field, can also apply to the structural ceramic material industry that ceramic bearing industry, high-temperature operation industry etc. are had relatively high expectations.
Embodiment
The present invention is a kind of type silicon nitride electric heating element of doing, and is made up of pyrotoxin and heating body.Count by weight percentage, the prescription of said heating body comprises following component: nano-silicon nitride 85%-96%, alundum (Al 1%-4%, yttria 4%-8%.Because: the nano-silicon nitride size will directly have influence on the growth of whisker, cause product quality undesirable phenomenon possibly occur, and therefore preferred, the nano-silicon nitride particle size range is between 40-60nm.Pyrotoxin adopts tungsten filament.
The above-mentioned manufacturing approach of doing type silicon nitride electric heating element may further comprise the steps:
(1) preparation of raw material: by above-mentioned prescription weighing, ball milling is dried, sieves to such an extent that powder is for use.Ball-milling technology: add distilled water, silicon nitride ball grinding 5-60 hour, the rotating speed of grinder can be set according to equipment is different, and being generally 50/min changes.Viscosity after the grinding reaches 150-200mm
2/ S is good.Put into then sieve after the drying in oven for use.
(2) biscuit is made: through die forming, it is for use that biscuit is taken out in form removal with tungsten filament, above-mentioned powder.Mould is the metal die of processing by the type of the doing silicon nitride electric heating element Dimensions requirement that will produce.Processing during biscuit, earlier with tungsten filament put into the tungsten filament jig, half powder of pouring a biscuit into to mould, wipe powder off, put into the mould push-down head, turn over turnback then and take out the tungsten filament jig, add second half powder again and wipe off and put into the mould seaming chuck; Be placed on press molding on the press that ram pressures is 5-50Mpa, it is for use that biscuit is taken out in last form removal.
(3) sintering: biscuit is packed in the graphite mo(u)ld; Put into the hot pressing furnace sintering then; Sintering process is: in 20-40 minute, be heated to 900-1015 ℃ under the normal temperature, continue to heat up and begin pressurization, in 30-120 minute, be heated to 1700-1800 ℃; And all speed adds to total head, total lifting surface area * 200-300kg/cm of said total head=biscuit
2, kept 5-60 minute, then; In 5-60 minute, be cooled to 1300-1700 ℃, rose to 1700-1800 ℃ at 5-30 minute and kept 5-60 minute, last natural cooling, release; When temperature in the hot pressing furnace was lower than 120 ℃, graphite mo(u)ld was taken out in blow-on, and goods are taken out in form removal.Graphite mo(u)ld is with the graphite mo(u)ld of high purity graphite by the Dimensions processing of doing type silicon nitride electric heating element, and is pasting two-layer graphite paper with the biscuit contact-making surface, biscuit is packed into put into the hot pressing furnace sintering in the graphite mo(u)ld then.
Below in conjunction with embodiment, the present invention is done further explain, but the present invention is not limited to this specific examples.
The type of the doing silicon nitride electric heating element of embodiment 1-4, process through following steps:
1, preparation of raw material: by the weighing of table one prescription and put into the nylon bucket, add distilled water, silicon nitride ball, grinding reached 150-200mm until viscosity in 20 hours under grinder rotating speed 50/min
2Between/the S, then pour into container, putting into drying in oven cooling back, to cross 30 mesh sieves for use.
Table one. the body prescription unit of silicon nitride electric heating element: gram
2, biscuit is made: by the type of the doing silicon nitride electric heating element Dimensions requirement processing metal mould of 70 * 15 * 3mm; Processing during biscuit, earlier with tungsten filament put into the tungsten filament jig, half powder of pouring a biscuit into to mould, wipe powder off, put into the mould push-down head, turn over turnback then and take out the tungsten filament jig, add second half powder again and wipe off and put into the mould seaming chuck; Be placed on press molding on the press that ram pressures is 7Mpa, it is for use that biscuit is taken out in last form removal.
3, sintering process and process:
1), graphite mo(u)ld processing: by the Dimensions processing graphite mould that 70 * 15 * 3mm does type silicon nitride electric heating element, pasting two-layer graphite paper with the biscuit contact-making surface with high purity graphite.
2), dress mould: biscuit packed into put into the hot pressing furnace sintering then in the graphite mo(u)ld.
3), sintering process:
Embodiment 1
The biscuit that adopts formula I to make, its sintering process is: the normal temperature graphite mo(u)ld is heated to 1015 ℃ in 35 minutes, and continuing to heat up also begins pressurization; In 90 minutes, once more graphite mo(u)ld is heated to 1780 ℃, and all speed is forced into 29 and rams the loose soil with a stone-roller after sowing, (individual layer burns 10) kept 10 minutes; Then; In 5 minutes, graphite mo(u)ld is cooled to 1750 ℃, rose to 1760 ℃ at 5 minutes and kept 35 minutes, shutdown natural cooling, release.
Embodiment 2
The biscuit that adopts formula I I to make, its sintering process is: the normal temperature graphite mo(u)ld is heated to 1000 ℃ in 40 minutes, and continuing to heat up also begins pressurization; In 70 minutes, once more graphite mo(u)ld is heated to 1785 ℃, and all speed is forced into 29 and rams the loose soil with a stone-roller after sowing, (individual layer burns 10) kept 8 minutes; Then; In 5 minutes, graphite mo(u)ld is cooled to 1680 ℃, rose to 1760 ℃ at 10 minutes and kept 40 minutes, shutdown natural cooling, release.
Embodiment 3
The biscuit that adopts formula I II to make, its sintering process is: the normal temperature graphite mo(u)ld is heated to 1015 ℃ in 30 minutes, and continuing to heat up also begins pressurization; In 85 minutes, once more graphite mo(u)ld is heated to 1750 ℃, and all speed is forced into 29 and rams the loose soil with a stone-roller after sowing, (individual layer burns 10) kept 4 minutes; Then; In 5 minutes, graphite mo(u)ld is cooled to 1730 ℃, rose to 1760 ℃ at 7 minutes and kept 20 minutes, shutdown natural cooling, release.
Embodiment 4
The biscuit that adopts formula I V to make, its sintering process is: the normal temperature graphite mo(u)ld is heated to 950 ℃ in 30 minutes, and continuing to heat up also begins pressurization; In 75 minutes, once more graphite mo(u)ld is heated to 1770 ℃, and all speed is forced into 26 and rams the loose soil with a stone-roller after sowing, (individual layer burns 10) kept 10 minutes; Then; In 10 minutes, graphite mo(u)ld is cooled to 1740 ℃, rose to 1770 ℃ at 5 minutes and kept 30 minutes, shutdown natural cooling, release.
4), form removal: when temperature in the hot pressing furnace was lower than 120 ℃, graphite mo(u)ld was taken out in blow-on, and goods are taken out in form removal.Tungsten filament is in as pyrotoxin in the middle of the body, at 6V-220V voltage, designs its length and size according to desired different capacity.
Embodiment 1-4 resulting product is made an experiment, and data are seen table 2.
Table 2.
Claims (9)
1. do type silicon nitride electric heating element for one kind; Be made up of pyrotoxin and heating body, it is characterized in that: count by weight percentage, the prescription of said heating body comprises following component: nano-silicon nitride 85%-96%; Alundum (Al 1%-4%, yttria 4%-8%.
2. the type silicon nitride electric heating element of doing according to claim 1, it is characterized in that: described pyrotoxin is a tungsten filament.
3. the type silicon nitride electric heating element of doing according to claim 1, it is characterized in that: described nano-silicon nitride particle size range is between 40-60nm.
4. the said manufacturing approach of doing type silicon nitride electric heating element of arbitrary claim among the claim 1-3 is characterized in that may further comprise the steps:
(1) preparation of raw material: by the prescription weighing, ball milling is dried, sieves to such an extent that powder is for use;
(2) biscuit is made: through die forming, it is for use that biscuit is taken out in form removal with pyrotoxin, above-mentioned powder;
(3) sintering: biscuit is packed in the graphite mo(u)ld, put into the hot pressing furnace sintering then, sintering process is: in 20-40 minute, be heated to 900-1015 ℃ under the normal temperature; Continue to heat up and begin pressurization, in 30-120 minute, be heated to 1700-1800 ℃, kept 5-60 minute; Then; In 5-60 minute, be cooled to 1300-1700 ℃, rose to 1700-1800 ℃ at 5-30 minute and kept 5-60 minute, last natural cooling, release.
5. the manufacturing approach of doing type silicon nitride electric heating element according to claim 4 is characterized in that: the ball-milling technology in the said step (1) is: add distilled water, silicon nitride ball grinding 5-60 hour, the viscosity after the grinding is 150-200mm
2/ S.
6. the manufacturing approach of doing type silicon nitride electric heating element according to claim 4; It is characterized in that: in the said step (2) mould be the metal die of processing by the type of the doing silicon nitride electric heating element Dimensions requirement that will produce; Processing during biscuit, earlier with tungsten filament put into the tungsten filament jig, half powder of pouring a biscuit into to mould, wipe powder off, put into the mould push-down head, turn over turnback then and take out the tungsten filament jig, add second half powder again and wipe off and put into the mould seaming chuck; Be placed on press molding on the press that ram pressures is 5-50Mpa, it is for use that biscuit is taken out in last form removal.
7. the manufacturing approach of doing type silicon nitride electric heating element according to claim 4; It is characterized in that: the graphite mo(u)ld in the said step (3) is with the graphite mo(u)ld of high purity graphite by the Dimensions processing of doing type silicon nitride electric heating element, and is posting graphite paper with the biscuit contact-making surface.
8. the manufacturing approach of doing type silicon nitride electric heating element according to claim 4; It is characterized in that: in the said step (3); In 30-120 minute, be heated to 1700-1800 ℃ of equal speed of while and add to total head, total lifting surface area * 200-300kg/cm of said total head=biscuit
2
9. the manufacturing approach of doing type silicon nitride electric heating element according to claim 4 is characterized in that: in the said step (3), when temperature in the hot pressing furnace was lower than 120 ℃, graphite mo(u)ld was taken out in blow-on at last, and goods are taken out in form removal.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102798143A (en) * | 2012-08-31 | 2012-11-28 | 黎石红 | Ceramic igniter and making method thereof |
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| 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 |
| CN101318637A (en) * | 2008-07-15 | 2008-12-10 | 北京科技大学 | Process for producing nano-silicon nitride ceramics powder |
| CN101747045A (en) * | 2008-12-11 | 2010-06-23 | 李明 | Silicon nitride heating body and method for manufacturing same |
| CN101846333A (en) * | 2009-03-25 | 2010-09-29 | 上海汉源特种陶瓷有限公司 | Silicon carbonitride igniter and manufacturing method thereof |
| CN101854749A (en) * | 2009-04-03 | 2010-10-06 | 上海汉源特种陶瓷有限公司 | Silicon nitride heating element and making method thereof |
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Patent Citations (5)
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| 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 |
| CN101318637A (en) * | 2008-07-15 | 2008-12-10 | 北京科技大学 | Process for producing nano-silicon nitride ceramics powder |
| CN101747045A (en) * | 2008-12-11 | 2010-06-23 | 李明 | Silicon nitride heating body and method for manufacturing same |
| CN101846333A (en) * | 2009-03-25 | 2010-09-29 | 上海汉源特种陶瓷有限公司 | Silicon carbonitride igniter and manufacturing method thereof |
| CN101854749A (en) * | 2009-04-03 | 2010-10-06 | 上海汉源特种陶瓷有限公司 | Silicon nitride heating element and making method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102798143A (en) * | 2012-08-31 | 2012-11-28 | 黎石红 | Ceramic igniter and making method thereof |
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