CN101765253A - Method for preparing SiC heating element having long service life - Google Patents
Method for preparing SiC heating element having long service life Download PDFInfo
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- CN101765253A CN101765253A CN201010104213A CN201010104213A CN101765253A CN 101765253 A CN101765253 A CN 101765253A CN 201010104213 A CN201010104213 A CN 201010104213A CN 201010104213 A CN201010104213 A CN 201010104213A CN 101765253 A CN101765253 A CN 101765253A
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Abstract
The invention discloses a method for preparing a SiC (silicon carbide) heating element having long service life. The method comprises the following steps: proportioning the following components by mass percentage: 75% to 90% of SiC, 1% to 5% of Al2O3, 1% to 5% of ZrO2, 1% to 3% SiO2, 4% to 10% of Si and 1% to 5% of C; preparing the components into a hollow pipe by using the extrusion molding process; drying at 80 to 300 DEG C; sintering at 1,450 to 1,650 DEG C in the presence of protective nitrogen, cutting into a heating part, and testing the resistance of the heating part for later use; proportioning the following components by mass percentage: 70% to 90% of SiC, 1% to 5% of Ni, 1% to 5% of Mo, 1% to 5% of Ti, 1% to 5% of TiC, 5% to 10% of Si and 1% to 5% of C; sintering the components by using the same process of forming and sintering as the heating part, cutting into a cold-side part, testing the resistance of the cold-side part for later use; and welding the cold-side parts at two ends of the heating part at the local-welding temperature of 1,500 to 1,600 DEG C, to complete the preparation of the entire heating element.
Description
Technical field
The present invention relates to a kind of preparation method of heater element, particularly a kind of preparation method of SiC heater element.
Background technology
SiC (carborundum) heater element claims Elema again, forms (Fig. 1) by heat generating part and cold end two parts usually.Heat generating part generally forms by SiC recrystallization sintering, and sintering temperature is usually about 2200 ℃.The porosity reaches 15～20%, and intensity is 75～100Mpa; Resistivity is bigger, is generally 15～20 times of cold end.The cold end material is at present main to be adopted reaction-sintered to ooze Si to handle, and the porosity is less than 1%, fine and close, intensity is little up to 250MPa, resistivity.The best serviceability temperature of Elema is generally at 800 ℃～1350 ℃, heat generating part at high temperature, the SiC surface produces oxidation reaction: 2SiC+3O with oxygen
2→ 2SiO
2+ 2CO ↑, SiO
2Generate diaphragm at the SiC particle surface, protect the further oxidation of SiC, realized the high-temperature oxidation resistance of SiC pottery.But when using for a long time, on the one hand, because heat generating part contains 15～20% the porosity, oxygen can be in the free flow of SiC material internal; On the other hand, SiO
2Though generation the SiC particle is had the certain protection effect, local electrical resistance is raise, cause this place local temperature to raise, make the selective oxidation aggravation again, cause the excellent life-span of SiC limited.
The high porosity (about 20%) that changes heat generating part is 0% fine and close SiC, and oxidized area is reduced greatly, thereby improves the life-span.How to obtain low-cost fine and close SiC: the technology that at present the simplest industrial method adopts reaction-sintered to ooze Si.Subject matter be gained reaction-sintered SiC (Si) though densification (0% porosity), resistivity is little, should not be used for heat generating part.
Summary of the invention
The present invention is directed to short problem of traditional silicon carbon-point life-span, a kind of preparation method of SiC heating element having long service life is provided.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of preparation method of SiC heating element having long service life is characterized in that, comprises the steps:
(1) preparation of heat generating part: following component is prepared burden by mass percentage: SiC, 75～90%; Al
2O
3, 1～5%; ZrO
2, 1～5%; SiO
2, 1～3%; Si, 4～10%; C, 1～5%; Adopt extrusion forming process to make hollow pipe; 80 ~ 300 ℃ of oven dry; Nitrogen protection, 1450～1650 ℃ are burnt till, standby after cutting, the check resistance value;
(2) preparation of cold end: following component is prepared burden by mass percentage: SiC, 70～90%, Ni, 1～5%; Mo, 1～5%; Ti, 1～5%; TiC, 1～5%; Si, 5～10%; C, 1～5%; Adopt moulding and the sintering process identical to burn till with step (1), standby after cutting, the check resistance value;
(3) welding: cold end is gone up in the two ends welding of heat generating part, finishes the preparation of whole heater element, and wherein the resistance ratio of heat generating part and cold end is chosen in 15～20.
In the said method, the resistance ratio of heat generating part and cold end preferably is chosen in 20.In the welding step, welding temperature is 1500～1600 ℃.The temperature of described check resistance value is 1100 ℃.
Compared with prior art, the present invention adopts and adds oxide ceramics additive (ZrO in fine and close SiC (Si) material
2, SiO
2, Al
2O
3) improve the resistivity of this material, as the heat generating part of Elema, this heat generating part material is because the porosity is near zero.Air can't pass through at material internal.Have only the surface can oxidation, the oxidation area be very little, and local electrical resistance changes very little after the oxidation.Thereby can significantly improve the useful life of Elema.
Description of drawings
The present invention is described in further detail below in conjunction with the drawings and the specific embodiments.
Fig. 1 is the structure chart of SiC heater element.Among the figure: 1, heat generating part; 2, cold end.
Fig. 2 is a process chart of the present invention.
Embodiment
Referring to Fig. 2 SiC heater element of the present invention preparation technology flow chart, heat generating part 1 and cold end 2 all relate to wherein batching, mixing, moulding, dry, burn till and check 1 operation.The specific embodiment of heat generating part is as shown in table 1.The specific embodiment of cold end is as shown in table 2.
The prescription of table 1 heat generating part is formed and technological parameter
The prescription of table 2 cold end is formed and technological parameter
In operation shown in Figure 2, checking 1 operation is that detected temperatures is 1100 ℃ to the hot detection of the resistance value (resistivity) of the heat generating part 1 that sinters or cold end 2.
Welding sequence is that heat generating part through checking 1 operation 1 and cold end 2 are welded as integral body, and the local welding temperature of weld is 1500～1600 ℃.The resistance ratio of heat generating part and cold end is chosen in 15～20, preferably is chosen in 20.Checking 2 operations is that the resistance of the whole heater element after welding is finished is measured.
The present invention forms code name for heat 1 heat generating part and code name are that Elema A is made in the cold 4 cold end welding of forming; Heat generating part and code name that code name is formed for heat 2 are that Elema B is made in the cold 3 cold end welding of forming; Heat generating part and code name that code name is formed for heat 3 are that Elema C is made in the cold 2 cold end welding of forming; Heat generating part and code name that code name is formed for heat 4 are that Elema D is made in the cold 1 cold end welding of forming; Its performance is listed in table 3
The Elema performance of table 3 the present invention preparation
| Code name | Elema A | Elema B | Elema C | Elema D |
| Applicable temperature (℃) | ??800~1200 | ??900~1300 | ??900~1350 | ??900~1350 |
| The hot junction porosity (%) | ??1 | ??0.65 | ??0.32 | ??0.06 |
| Useful life (moon) | ??＞12 | ??＞18 | ??＞18 | ??＞18 |
Existing Elema heat generating part lost efficacy or the reason damaged is: the best serviceability temperature of Elema is generally at 800 ℃～1350 ℃, heat generating part at high temperature, the SiC surface produces oxidation reaction, the SiO of generation with oxygen
2Form diaphragm at the SiC particle surface; though can protect the further oxidation of SiC; but local electrical resistance is raise; cause this place's local temperature to raise; in addition because the present recrystallization SiC porosity height that uses, oxygen is inside and outside easily to flow and passes through, and causes Elema selective oxidation aggravation; oxide film breakdown, overheated and fracture and aging.
Innovative point of the present invention is:
1, the high porosity (about 20%) that at first changes heating part greatly reduces oxidized area, thereby improves the life-span near 0% fine and close SiC.
2, by respectively to the composition of the suitable increase resistance of heating part and cold end Material Addition, such as ZrO2，Al
2O
3，SiO
2Deng and reduce the component of resistance, such as Ni, Mo, Ti, TiC etc. significantly increase heating part resistance, cold end resistance significantly reduces, thereby satisfies the specification requirement of the two resistance ratio 15～20.
Claims (4)
1. the preparation method of a SiC heating element having long service life is characterized in that, comprises the steps:
(1) preparation of heat generating part: following component is prepared burden by mass percentage: SiC, 75～90%; Al
2O
3, 1～5%; ZrO
2, 1～5%; SiO
2, 1～3%; Si, 4～10%; C, 1～5%; Adopt extrusion forming process to make hollow pipe; 80 ~ 300 ℃ of oven dry; Nitrogen protection, 1450～1650 ℃ are burnt till, standby after cutting, the check resistance value;
(2) preparation of cold end: following component is prepared burden by mass percentage: SiC, 70～90%, Ni, 1～5%; Mo, 1～5%; Ti, 1～5%; TiC, 1～5%; Si, 5～10%; C, 1～5%; Adopt moulding and the sintering process identical to burn till with step (1), standby after cutting, the check resistance value;
(3) welding: cold end is gone up in the two ends welding of heat generating part, finishes the preparation of whole heater element, and wherein the resistance ratio of heat generating part and cold end is chosen in 15～20.
2. the preparation method of SiC heating element having long service life as claimed in claim 2 is characterized in that, the resistance ratio of heat generating part and cold end is chosen in 20.
3. the preparation method of SiC heating element having long service life as claimed in claim 1 is characterized in that, in the welding step, welding temperature is 1500～1600 ℃.
4. the preparation method of SiC heating element having long service life as claimed in claim 1 is characterized in that, the temperature of described check resistance value is 1100 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101042130A CN101765253B (en) | 2010-02-02 | 2010-02-02 | Method for preparing SiC heating element having long service life |
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|---|---|---|---|
| CN2010101042130A CN101765253B (en) | 2010-02-02 | 2010-02-02 | Method for preparing SiC heating element having long service life |
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| CN101765253A true CN101765253A (en) | 2010-06-30 |
| CN101765253B CN101765253B (en) | 2012-01-04 |
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173812A (en) * | 2011-01-29 | 2011-09-07 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of molybdenum silicide type heating component |
| CN103152847A (en) * | 2013-02-28 | 2013-06-12 | 包头稀土研究院 | Method for manufacturing lanthanum chromite electric heating element in welding manner |
| CN105934005A (en) * | 2016-05-06 | 2016-09-07 | 武汉航空仪表有限责任公司 | Novel heater of icing detector |
| CN108934087A (en) * | 2017-05-26 | 2018-12-04 | Lg电子株式会社 | Carbon heating body |
| CN108966379A (en) * | 2017-05-26 | 2018-12-07 | Lg电子株式会社 | The manufacturing method of carbon heater |
| CN109288140A (en) * | 2018-12-06 | 2019-02-01 | 广东国研新材料有限公司 | A kind of electronic cigarette Multi-hole ceramic heating element and preparation method thereof |
| US11097985B2 (en) | 2017-05-10 | 2021-08-24 | Lg Electronics Inc. | Carbon composite composition and carbon heater manufactured using the same |
-
2010
- 2010-02-02 CN CN2010101042130A patent/CN101765253B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173812A (en) * | 2011-01-29 | 2011-09-07 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of molybdenum silicide type heating component |
| CN102173812B (en) * | 2011-01-29 | 2013-10-30 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of molybdenum silicide type heating component |
| CN103152847A (en) * | 2013-02-28 | 2013-06-12 | 包头稀土研究院 | Method for manufacturing lanthanum chromite electric heating element in welding manner |
| CN105934005A (en) * | 2016-05-06 | 2016-09-07 | 武汉航空仪表有限责任公司 | Novel heater of icing detector |
| US11097985B2 (en) | 2017-05-10 | 2021-08-24 | Lg Electronics Inc. | Carbon composite composition and carbon heater manufactured using the same |
| CN108934087A (en) * | 2017-05-26 | 2018-12-04 | Lg电子株式会社 | Carbon heating body |
| CN108966379A (en) * | 2017-05-26 | 2018-12-07 | Lg电子株式会社 | The manufacturing method of carbon heater |
| US11096249B2 (en) | 2017-05-26 | 2021-08-17 | Lg Electronics Inc. | Carbon heating element and method for manufacturing a carbon heating element |
| CN108966379B (en) * | 2017-05-26 | 2021-12-24 | Lg电子株式会社 | Method for manufacturing carbon heater |
| CN108934087B (en) * | 2017-05-26 | 2022-06-14 | Lg电子株式会社 | Carbon heating element |
| CN109288140A (en) * | 2018-12-06 | 2019-02-01 | 广东国研新材料有限公司 | A kind of electronic cigarette Multi-hole ceramic heating element and preparation method thereof |
| CN109288140B (en) * | 2018-12-06 | 2021-08-27 | 广东国研新材料有限公司 | Porous ceramic heating element for electronic cigarette and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN101765253B (en) | 2012-01-04 |
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