CN201915043U - Heating element made of carbon materials - Google Patents
Heating element made of carbon materials Download PDFInfo
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- CN201915043U CN201915043U CN2011200053481U CN201120005348U CN201915043U CN 201915043 U CN201915043 U CN 201915043U CN 2011200053481 U CN2011200053481 U CN 2011200053481U CN 201120005348 U CN201120005348 U CN 201120005348U CN 201915043 U CN201915043 U CN 201915043U
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Abstract
The utility model discloses a heating element made of carbon materials. An anti-oxidant layer is coated on the surface of the heating element made of carbon materials, and the heating element comprises a base body (1) made of carbon/carbon composite materials or graphite materials. The heating element is characterized in that a transitional layer (2) consisting of in-site growth silicon carbide whiskers is arranged on the surface of the base body (1). The layer of silicon carbide whiskers are formed on the carbon-material base body in an in-situ growth manner, size and amount of cracks in the coating layer are reduced by means of extracting and bridging of the silicon carbide whiskers and a crack turning mechanism, anti-oxidant performance and thermal shock resistance performance of the silicon carbide coating layer are improved greatly, the whole preparation process can be completed by means of chemical gas-phase deposition continuously, so that the preparation process of the coating layer are simplified greatly. The heating element made of carbon materials can be used as an auxiliary heating element for zone purification of semiconductor materials.
Description
Technical field
The utility model relates to a kind of high temperature field heating element, specifically a kind of carbon material heating element, and particularly relating to a kind of is the heating element of matrix by carbon/carbon compound material or graphite material.
Background technology
A series of excellent characteristics such as carbon/carbon compound material or graphite material have good heat resistance, thermal-shock resistance is good, thermal conductivity is high, thermal expansivity is low, easy processing, high-temperature machinery intensity height, it is the optimal candidate material of preparation heating element, but because there are a fatal shortcoming in carbon/carbon compound material or graphite, high temperature is very easily oxidized.Therefore, the heating element of carbon/carbon compound material or graphite material preparation can only or have under the protective atmosphere condition in vacuum and uses.Yet, in actual production, require heating element in air or under the aerobic environment, to use sometimes, this just requires heating element itself to have resistance of oxidation.
Zone-refine is the important method of preparation semiconductor material and other high-purity material (metal, mineral compound and organic compound).As when preparing monocrystalline germanium, need purify to the germanium raw material, its method of purification mainly is a zone-refine, being about to germanium ingot (by high-purity germanium dioxide reduction) places in the high purity graphite boat, graphite boat places silica tube, outside silica tube, load radio-frequency induction coil, radio-frequency induction coil places an end of germanium ingot, the induced current that produces by high-frequency induction magnetic field heats graphite boat, thereby heating germanium ingot, rising along with temperature, self also becomes conductor the germanium ingot, cause the germanium ingot to be higher than other position in the temperature of radio-frequency induction coil one end, when temperature is higher than the fusing point of germanium, can produce local melting zone in this zone, move silica tube with certain speed then, make the melting zone move to the other end from an end, in mobile melting zone, the germanium of fusing also solidifies gradually earlier, because sosoloid is selectable crystallization, elder generation's crystalline germaniumcrystal enters solute (impurity) in the germanium melt of melt portions, so after the melting range was walked to go over, the impurity in the germanium ingot will be enriched in the other end, repeats can reach several times the purpose of purifying germanium ingot, at last enrichment impurity end is removed get final product high-purity polycrystalline germanium, by vertical pulling method etc. polycrystalline germanium is drawn into monocrystalline germanium then.
Above-mentioned method is suitable for preparing the germanium single crystal that purity is 6N, but in actual applications, sometimes needing purity is the germanium single crystal of 9N even 12N, this has higher purity with regard to requiring the polycrystalline germanium after the zone-refine, but because the pollution of graphite boat, be difficult to prepare the polycrystalline germanium of purity greater than 9N even 12N, therefore, in actual production, generally being to be that the polycrystalline germanium of 6N is a raw material with purity, is that carrier carries out further zone-refine with the high purity quartz boat, but because quartz can not produce induction heating, so before the heating of germanium energy autonomous induction, must have auxiliary heating element heating to make germanium ingot temperature reach the temperature that germanium changes conductor into.Auxiliary heating element is made ring-type by graphite material usually, adjacent with radio-frequency induction coil, together be enclosed within an end of silica tube, in the inducedmagnetic field that radio-frequency induction coil produces, graphite annulus produces induced current and generates heat, thereby the germanium ingot in heated quarty tube and the pipe, germanium ingot temperature in the silica tube termination is raise, and when germanium ingot temperature was elevated to about 900 ℃, the germanium ingot became conductor, remove auxiliary heating element then, carry out zone-refine by high-frequency induction heating germanium ingot.Because Heating temperature is up to 900 ℃, and be to heat under unprotect atmosphere, the heating element of graphite material preparation can very fast oxidation and lost efficacy, and has influenced normally carrying out of producing.
Summary of the invention
The purpose of this utility model provides the carbon material heating element that a kind of surface has oxidation resistant coating.
At present, method commonly used is to adopt the chemical vapor deposition (CVD) legal system to be equipped with coating, and the characteristics that the CVD method prepares oxidation resistant coating are: the coating densification is smooth, purity is high, and can realize the design to coating structure, pattern, composition and thickness.Therefore, the CVD coating technology is widely used in semi-conductor, metallurgy industry etc. with high temperature, highly purified various heat structure parts surface coatings, and is wherein extensive with the SiC coatings applications.It is bigger that SiC has unreactiveness, the excellent high-temperature mechanical property, and thermal shock resistance and resistance of oxidation, high fusing point, and also the reaction of SiC high temperature oxidation can generate continuous, even, fine and close SiO
2The oxidation protection film is so SiC coating and SiC compound coating are the preferred material of carbon material oxidation resistant coating.
But the thermal expansivity of carbon/carbon compound material and graphite material and SiC coating does not match, and the coating of preparation and the associativity of matrix are relatively poor, come off easily, thereby the oxidation-resistance of whole coating, thermal shock resistance is not ideal enough.
Silicon carbide whisker is that a kind of diameter is an extremely micron-sized single crystal fibre of nano level, has good characteristics such as high strength, high rigidity, high elastic coefficient and density are low, corrosion-resistant, chemical property stable, oxidation-resistance property is strong.
The utility model is to adopt following technical scheme to realize its goal of the invention, a kind of carbon material heating element, and it comprises the matrix of being made up of carbon/carbon compound material or graphite material, the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ.
The utility model is further to improve anti-oxidation of coating, and transition layer is provided with the top layer of being made up of compact silicon carbide.
Owing to adopt technique scheme, the utility model has been realized goal of the invention preferably, growth in situ one deck silicon carbide whisker on the carbon material heating element, the silicon carbide skin of refabrication densification, thereby between the silicon carbide top layer of matrix and densification, form the SiCw transition layer, its thermal expansivity is between matrix and silicon carbide, can effectively reduce because the thermal stresses that thermal expansivity does not match and produces, simultaneously, utilize extract bridging and the crackle of silicon carbide whisker to turn to mechanism to reduce crack size and quantity in the coating, help increasing substantially the antioxidant property and the thermal shock resistance of coat of silicon carbide, and whole process of preparation can be finished continuously by chemical vapour deposition, simplified the preparation process of oxidation resistant coating greatly, can in semiconductor material regions is purified, use as auxiliary heating element.
Description of drawings
Fig. 1 is that the utility model is at the structural representation of carbon material heating element surface preparation by the transition layer of being made up of silicon carbide whisker;
Fig. 2 is the surface scan electromicroscopic photograph of the utility model at the silicon carbide whisker of carbon material heating element surface in situ growth;
Fig. 3 is the X-Ray diffracting spectrum of the utility model at the silicon carbide whisker of carbon material heating element surface in situ growth;
Fig. 4 is the cross section stereoscan photograph of the utility model at the silicon carbide whisker of carbon/carbon compound material heating element surface in situ growth;
Fig. 5 is the utility model is reached the top layer of being made up of compact silicon carbide by the transition layer of being made up of silicon carbide whisker in carbon material heating element surface preparation a structural representation;
Fig. 6 be the utility model when carbon material heating element surface preparation has transition layer and top layer, the surface scan electromicroscopic photograph on top layer;
Fig. 7 is the utility model embodiment 3(curve II), embodiment 4(curve III), embodiment 1(curve IV), embodiment 5(curve V) with SiC coating sample (curve I) isothermal oxidation weight loss curve in 1100 ℃ of air of traditional chemical vapour deposition process preparation;
Fig. 8 is the utility model embodiment 3(curve II), embodiment 4(curve III), embodiment 1(curve IV), embodiment 5(curve V) with SiC coating sample (curve I) air of traditional chemical vapour deposition process preparation in 15 1100 ℃ * 3min of experience ← → the oxidation weight loss curve of room temperature * 3min thermal cycling;
Fig. 9 is the utility model embodiment 6(curve II), embodiment 7(curve III), embodiment 2(curve IV), embodiment 8(curve V) with SiC coating sample (curve I) isothermal oxidation weight loss curve in 1100 ℃ of air of traditional chemical vapour deposition process preparation;
Figure 10 is the utility model embodiment 6(curve II), embodiment 7(curve III), embodiment 2(curve IV), embodiment 8(curve V) with SiC coating sample (curve I) air of traditional chemical vapour deposition process preparation in 15 1100 ℃ * 3min of experience ← → the oxidation weight loss curve of room temperature * 3min thermal cycling.
Embodiment
The utility model is described in further detail below in conjunction with drawings and Examples.
Embodiment 1:
As shown in Figure 1, a kind of carbon material oxidation resistant coating, it comprises the matrix of being made up of carbon/carbon compound material or graphite material 1, the surface of matrix 1 is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ 2.
A kind of preparation method of the oxidation resistant coating of carbon material as mentioned above, it may further comprise the steps:
⑴ get the raw materials ready: with 1 polishing of carbon material matrix, polishing, dry for standby after the washes clean; The matrix 1 of present embodiment carbon material heating element is a carbon/carbon compound material.
⑵ Preparation of Catalyst: the presoma alcohol solution of preparation catalyzer makes Ni in the solution
2+: Al
3+=(5～15): (1～3) (present embodiment is Ni
2+: Al
3+=5:1), 5%～20%(present embodiment that the alcoholic acid volume accounts for overall solution volume is 20%), add aqueous solution of urea, regulate making Ni
2+Concentration for (0.05～0.2) mol/L(present embodiment be 0.1mol/L), transfer in the reactor after stirring;
⑶ loading catalyst: it is 10 h that step ⑴ gained matrix 1 is put into reactor solution normal pressure dipping 5h～12h(present embodiment), reacting 1h～3h(present embodiment in the oil bath with reactor immersion 95 ℃～120 ℃ (present embodiment is 110 ℃) then is 2h), after reactor is chilled to room temperature with cold water matrix 1 is therefrom taken out, the back of drying in the shade at normal temperatures is stand-by;
⑷ growth in situ silicon carbide whisker: step ⑶ gained matrix 1 is put into chemical vapor deposition stove; be evacuated to 0.1kPa; feed argon gas; under argon shield, heat up; depositing temperature is 950 ℃～1250 ℃ (present embodiment is 1100 ℃); 10min～60min(present embodiment is 15min before arriving depositing temperature) close argon gas; feeding hydrogen reduces to catalyzer; hydrogen flowing quantity is that 100mL/min～300mL/min(present embodiment is 200mL/min); reach that to be incubated 10min～60min(present embodiment behind the depositing temperature be 15min); then with hydrogen as carrier gas and diluent gas; throughput ratio is 1:1; with Bubbling method trichloromethyl silane is introduced in the cvd furnace; the container bottle of splendid attire trichloromethyl silane places water bath with thermostatic control, and 18 ℃～25 ℃ of bath temperatures (present embodiment is 22 ℃), depositing time are that 1h～50h(present embodiment is 6h); pressure is normal pressure, the transition layer of being made up of the silicon carbide whisker of growth in situ in matrix 1 surface preparation 2.
A kind of application of the carbon material heating element by method for preparing is to be used as auxiliary heating element in the zone-refine of semiconductor material.As in the monocrystalline germanium preparation, using.
Embodiment 2:
Present embodiment is in step ⑴, and the matrix 1 of carbon material heating element is a graphite material.
Surplus with embodiment 1.
As shown in Figure 2, the silicon carbide whisker of the utility model preparation is even in carbon material heating element surface arrangement.
As shown in Figure 3, the utility model is β-SiCw at the silicon carbide whisker of carbon material heating element surface in situ growth.
As shown in Figure 4, when the utility model is carbon/carbon compound material at the matrix 1 of carbon material heating element, cross section stereoscan photograph explanation silicon carbide whisker transition layer 2 porous and fine and close gradually along the direction of carbon/carbon composite material base body, this explanation transition layer 2 combines fine with matrix 1, simultaneously, transition layer 2 porous surfaces are when being provided with the top layer of being made up of compact silicon carbide thereon again, help alleviating the thermal stresses of coating inside, avoid coating cracking and come off.
Embodiment 3:
As shown in Figure 5, the utility model is further to improve anti-oxidation of coating, is provided with the top layer of being made up of compact silicon carbide 3 on transition layer 2.
Its preparation technology is in step ⑴, and the matrix 1 of carbon material heating element is a carbon/carbon compound material, and in step ⑷, depositing time is 2h.
After step ⑷ is intact, diluent gas is changed into argon gas, carrier gas is a hydrogen, and the adjustment diluting gas flow is 2:1 with the carrier gas flux ratio, depositing temperature is 950 ℃～1250 ℃ (present embodiment is 1100 ℃), and depositing time is that 1h～50h(present embodiment is 4h), pressure is normal pressure.The top layer 3 that preparation is made up of compact silicon carbide on the transition layer of being made up of the growth in situ silicon carbide whisker 2.
As shown in Figure 6, compact silicon carbide top layer 3 densifications, smooth are attended by a small amount of little crackle, but do not have tangible hole, compact silicon carbide top layer 3 be describeds in the evenly formation of silicon carbide whisker transition layer 2 surfaces, good consistency are arranged between two-layer.
Surplus with embodiment 1.
Embodiment 4:
In step ⑷, depositing time is 3h, and during preparation top layer 3, depositing time is 3h.
Surplus with embodiment 1, embodiment 3.
Embodiment 5:
In step ⑷, depositing time is 5h, and during preparation top layer 3, depositing time is 1h.
Surplus with embodiment 1, embodiment 3.
As shown in Figure 7, the resistance of oxidation of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, and oxidation 10h rate of weight loss is 41.11% in 1100 ℃ of air, among Fig. 7 shown in the curve I.
Oxidation 10h rate of weight loss is respectively in 1100 ℃ of air of four embodiment coating samples of the utility model preparation: 8.87%(embodiment 3, shown in the curve II), 5.50%(embodiment 4, shown in the curve III), 2.07%(embodiment 1, shown in the curve IV) and 0.87%(embodiment 5, shown in the curve V), its average rate of weight loss is 4.33%.
As shown in Figure 8, the thermal shock resistance of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, 1100 ℃ * 3min ← → 15 thermal cyclings of room temperature * 3min after rate of weight loss be 33.17%, among Fig. 8 shown in the curve I.
And four embodiment coating sample rate of weight loss of the utility model preparation are respectively: 11.09%(embodiment 3, shown in the curve II), 5.66%(embodiment 4, shown in the curve III), 0.51%(embodiment 1 is shown in the curve IV) and 0.22%(embodiment 5, shown in the curve V).
Embodiment 6:
As shown in Figure 5, the utility model is further to improve anti-oxidation of coating, is provided with the top layer of being made up of compact silicon carbide 3 on transition layer 2.
Its preparation technology is in step ⑴, and the matrix 1 of carbon material heating element is a graphite material, and in step ⑷, depositing time is 2h.
After step ⑷ is intact, diluent gas is changed into argon gas, carrier gas is a hydrogen, and the adjustment diluting gas flow is 2:1 with the carrier gas flux ratio, depositing temperature is 950 ℃～1250 ℃ (present embodiment is 1100 ℃), and depositing time is that 1h～50h(present embodiment is 4h), pressure is normal pressure.The top layer 3 that preparation is made up of compact silicon carbide on the transition layer of being made up of the growth in situ silicon carbide whisker 2.
Surplus with embodiment 1.
Embodiment 7:
In step ⑴, the matrix 1 of carbon material heating element is a graphite material, and in step ⑷, depositing time is 3h, and during preparation top layer 3, depositing time is 3h.
Surplus with embodiment 1, embodiment 6.
Embodiment 8:
In step ⑴, the matrix 1 of carbon material heating element is a graphite material, and in step ⑷, depositing time is 5h, and during preparation top layer 3, depositing time is 1h.
Surplus with embodiment 1, embodiment 6.
As shown in Figure 9, the resistance of oxidation of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, and oxidation 10h rate of weight loss is 32.82% in 1100 ℃ of air, among Fig. 9 shown in the curve I.
Oxidation 10h rate of weight loss is respectively in 1100 ℃ of air of four embodiment coating samples of the utility model preparation: 8.63%(embodiment 6, shown in the curve II), 5.36%(embodiment 7, shown in the curve III), 2.03%(embodiment 2, shown in the curve IV) and 0.85%(embodiment 8, shown in the curve V), its average rate of weight loss is 4.22%.
As shown in Figure 10, the thermal shock resistance of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, 1100 ℃ * 3min ← → 15 thermal cyclings of room temperature * 3min after rate of weight loss be 28.83%, among Figure 10 shown in the curve I.
And four embodiment coating sample rate of weight loss of the utility model preparation are respectively: 10.83%(embodiment 6, shown in the curve II), 5.54%(embodiment 7, shown in the curve III), 0.49%(embodiment 2 is shown in the curve IV) and 0.21%(embodiment 8, shown in the curve V).
The SiC coating for preparing for the ease of the coating of relatively the utility model preparation and traditional chemical vapour deposition process is in the difference aspect antioxidant property and the thermal shock resistance, the depositing time of all embodiment floating coats of the utility model is identical, and promptly the depositing time of the depositing time of growth in situ silicon carbide whisker or growth in situ silicon carbide whisker and fine and close SiC coating depositing time sum are 6h.
The utility model is by matrix 1 surface preparation growth in situ SiCw coating and the toughness reinforcing SiCw-SiC coating of SiCw at carbon/carbon compound material or graphite material heating element, the oxidation-resistance of coating and thermal shock resistance height, realized the coating preparation of serialization under the normal pressure, preparation technology is simple, can use as auxiliary heating element in semiconductor material regions is purified.
Claims (2)
1. carbon material heating element, it comprises the matrix of being made up of carbon/carbon compound material or graphite material (1), it is characterized in that the surface of matrix (1) is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ (2).
2. carbon material heating element according to claim 1 is characterized in that transition layer (2) is provided with the top layer of being made up of compact silicon carbide (3).
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|---|---|---|---|
| CN2011200053481U CN201915043U (en) | 2011-01-10 | 2011-01-10 | Heating element made of carbon materials |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200053481U CN201915043U (en) | 2011-01-10 | 2011-01-10 | Heating element made of carbon materials |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102123527A (en) * | 2011-01-10 | 2011-07-13 | 湖南金博复合材料科技有限公司 | Application and preparation method of carbon material heating body |
| CN103570378A (en) * | 2012-08-01 | 2014-02-12 | 苏州宏久航空防热材料科技有限公司 | Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
| CN103703865A (en) * | 2011-08-09 | 2014-04-02 | 法国圣戈班玻璃厂 | Electrical contact composites and method for producing electrical contact composites |
| CN104179322A (en) * | 2014-09-10 | 2014-12-03 | 太仓派欧技术咨询服务有限公司 | Electric heating flooring heating system |
-
2011
- 2011-01-10 CN CN2011200053481U patent/CN201915043U/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102123527A (en) * | 2011-01-10 | 2011-07-13 | 湖南金博复合材料科技有限公司 | Application and preparation method of carbon material heating body |
| CN103703865A (en) * | 2011-08-09 | 2014-04-02 | 法国圣戈班玻璃厂 | Electrical contact composites and method for producing electrical contact composites |
| CN103703865B (en) * | 2011-08-09 | 2016-09-14 | 法国圣戈班玻璃厂 | Electric contact composite material, the method manufacturing electric contact composite material |
| US9837732B2 (en) | 2011-08-09 | 2017-12-05 | Saint-Gobain Glass France | Electrical contact composites and method for producing electrical contact composites |
| US10770806B2 (en) | 2011-08-09 | 2020-09-08 | Saint-Gobain Glass France | Electrical contact composites and method for producing electrical contact composites |
| CN103570378A (en) * | 2012-08-01 | 2014-02-12 | 苏州宏久航空防热材料科技有限公司 | Method for direct deposition of silicon carbide (SiC) coating on carbon material surface in graphite heat-generating body heating furnace |
| CN104179322A (en) * | 2014-09-10 | 2014-12-03 | 太仓派欧技术咨询服务有限公司 | Electric heating flooring heating system |
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Address after: 413000 Hunan province Yiyang Yingbin Road No. 2 Patentee after: Hunan gold carbon Limited by Share Ltd Address before: 413000 Hunan province Yiyang Yingbin Road No. 2 Patentee before: Hunan KBCarbon Composite Science and Technology Co., Ltd. |
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Granted publication date: 20110803 |
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