CN102021648B - Guide cylinder antioxidation coating and preparation method thereof - Google Patents
Guide cylinder antioxidation coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a guide cylinder antioxidation coating with simple process and good oxidation resistance. The guide cylinder antioxidation coating comprises a matrix prepared from a carbon/carbon composite material and is characterized in that the surface of the matrix is provided with a transition layer (2) composed of silicon carbide whisker grown in situ. The preparation method comprises the steps: (1) providing material; (2) preparing a catalyst; (3) loading the catalyst; and (4) growing the silicon carbide whisker in situ. The matrix of the guide cylinder provided by the invention is convenient to process, a silicon carbide whisker layer is grown in situ on the matrix of the guide cylinder, the extraction bridging and crack steering mechanism of the silicon carbide whisker layer is utilized to reduce dimension and number of cracks in the coating, thus being beneficial to greatly improving oxidation resistance and thermal shock resistance of the silicon carbide coating, and the whole preparation process can be continuously completed by chemical vapour deposition, thus greatly simplifying the preparation process of the coating and improving the comprehensive performance of the guide cylinder.
Description
Technical field
The present invention relates to a kind of thermal field of single crystal furnace part guide shell, specifically a kind of guide shell ORC and preparation method, particularly relating to a kind of is the surface oxidation-resistant coating and the preparation method of matrix by carbon/carbon compound material.
Background technology
Guide shell is the crucial thermal field component that monocrystalline silicon draw machines must be used, and is mainly used in the thermograde and guiding argon gas stream of control thermal field, and this will ask the heat-insulating property of guide shell own to get well, and have certain anti-airflow scouring ability.At present single-crystal furnace guide shell is generally made up with the carbon felt by graphite piece and processes, and promptly goes out inner core and urceolus with machining graphite, and the carbon felt is clipped in the middle of inner core and the urceolus, through fastening piece the three is combined again.The shortcoming of this guide shell is: (1) causes guide shell shorter work-ing life because graphite intensity is low; (2), cause heat-preservation cylinder processing to use comparatively loaded down with trivial details because the good heat conductivity of graphite in order to improve heat-insulating property, must add one deck carbon felt between graphite inner core and urceolus; (3) large size guide shell shaping difficulty, consumptive material is more.Therefore, in recent years, the whole guide shell of many silicon single-crystal manufacturer's employing carbon-fibre composites replaces graphite carbon felt combination guide shell to carry out the drawing of silicon single crystal rod, makes the problems referred to above obtain solving preferably.
But because guide shell is under the high temperature silicon steam condition, to use, the molten silicon under the high temperature has extremely strong reactive behavior; Generate oxidizing substance such as SiO with quartz crucible reaction and volatilize from bath surface; Oxidizing substances such as the SiO that volatilizes are centered around the outside surface of guide shell, and along with the prolongation of time, the guide shell outside surface is corroded gradually and forms the hole, hole; Influence its result of use, reduced work-ing life.Therefore, in order to improve the resistance to corrosion of guide shell under the high temperature silicon steam condition, further improving its work-ing life, is best choice in guide shell surface preparation coating, and the erosion-resisting characteristic of coating will prolong the work-ing life of guide shell.
For improving the anti-oxidant and anti-thermal shock ability of guide shell, therefore, need be at carbon/carbon compound material guide shell surface preparation ORC.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 ORC 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/carbon compound material ORC.But the oxidation-protective effect of SiC coating that develops at present and SiC compound coating is far away from theoretical value, and its major cause is well not resolve the structure problem of coating.Like application number is 200910310354.5; Publication No. is CN101717992A; Denomination of invention is that a kind of CZ silicon crystal growth oven carbon one carbon composite guide shell and preparation method thereof discloses and a kind ofly guide shell is carried out surface oxidation-resistant anti-impact erosion resisting coating handles, and the guide shell surface is provided with coat of silicon carbide.Because carbon/carbon composite material base body and SiC thermal expansivity do not match, the prepared SiC coating and the associativity of carbon/carbon composite material base body are relatively poor, come off easily, ftracture, and do not have well to solve the problem of the anti-airflow scouring ability of guide shell.
Simultaneously; Adopt the whole preparation of carbon/carbon compound material guide shell, when precast body is made, its flange be formed with certain degree of difficulty; And because of the deformation factor in the subsequent thermal processing process that will consider whole guide shell precast body; Often do the flange of whole guide shell precast body thicker, increased difficulty of processing, consumptive material is also more.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology; The guide shell ORC and the preparation method of coating good in oxidation resistance; Particularly provide a kind of on the guide shell matrix growth in situ one deck silicon carbide whisker, make the preparation method who forms the silicon carbide whisker transition layer between matrix and the fine and close silit top layer.
The present invention adopts following technical scheme to realize its goal of the invention, a kind of guide shell ORC, and it comprises that the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ by the matrix of carbon/carbon compound material preparation.
The present invention further improves anti-oxidation of coating, and transition layer is provided with the top layer of being made up of compact silicon carbide.
The present invention is easy to process, and described matrix comprises cylindrical shell, flange, and cylindrical shell, flange connect through web member.
A kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of web member of the present invention.
A kind of preparation method of above-mentioned guide shell ORC, it may further comprise the steps:
⑴ get the raw materials ready: with the polishing of guide shell matrix, polishing, dry for standby after the washes clean;
⑵ Preparation of Catalyst: the presoma alcohol solution of preparation catalyzer makes Ni in the solution
2+: Al
3+=(5～15): (1～3), the alcoholic acid volume accounts for 5%～20% of overall solution volume, adds aqueous solution of urea, regulates making Ni
2+Concentration be (0.05～0.2) mol/L, transfer in the reaction kettle after stirring;
⑶ loading catalyst: step ⑴ gained matrix is put into reaction kettle solution normal pressure dipping 5h～12h; React 1h～3h in the oil bath with 95 ℃～120 ℃ of reaction kettle immersions then; After reaction kettle is chilled to room temperature with cold water matrix is therefrom taken out, the back of drying in the shade at normal temperatures is for use;
⑷ growth in situ silicon carbide whisker: step ⑶ gained matrix is put into chemical vapor deposition stove, vacuumize, feed argon gas; Under argon shield, heat up, depositing temperature is 950 ℃～1250 ℃, and 10min～60min closes argon gas before arriving depositing temperature; Feed hydrogen catalyzer reduced, be incubated 10min～60min after reaching depositing temperature, then with hydrogen as carrier gas and diluents; Throughput ratio is 1:1, with Bubbling method trichloromethyl silane is introduced in the cvd furnace, and the container bottle of splendid attire trichloromethyl silane places water bath with thermostatic control; 18 ℃～25 ℃ of bath temperatures; Depositing time is 1h～50h, and pressure is normal pressure, prepares the transition layer of the silicon carbide whisker composition of growth in situ at matrix surface.
The present invention further improves anti-oxidation of coating, and the top layer that preparation is made up of compact silicon carbide on the transition layer that silicon carbide whisker is formed is after the silicon carbide whisker deposition is accomplished; Diluents is changed into argon gas; Carrier gas is a hydrogen, and adjustment diluting gas flow and carrier gas flux be than being 2:1, and depositing temperature is 950 ℃～1250 ℃; Depositing time is 1h～50h, and pressure is normal pressure.
The present invention is in step ⑴, and described matrix comprises cylindrical shell, flange, and cylindrical shell, flange connect through web member.
A kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of web member of the present invention.
Because adopt technique scheme, the present invention has realized goal of the invention preferably, the guide shell matrix is easy to process; Growth in situ one deck silicon carbide whisker on the guide shell matrix, the silit skin that refabrication is fine and close, thus between the silit top layer of matrix and densification, form the SiCw transition layer; Its thermal expansivity is between matrix and silit; Can effectively reduce because the thermal stresses that thermal expansivity does not match and produces simultaneously, utilizes the bridging of extracting of silicon carbide whisker to turn to crack size and quantity in the mechanism reduction coating with crackle; Help increasing substantially the antioxidant property and the thermal shock resistance of coat of silicon carbide; And whole process of preparation can accomplish through chemical vapour deposition continuously, simplified the preparation process of coating greatly, improved guide shell over-all properties.
Description of drawings
Fig. 1 is the structural representation of guide shell of the present invention;
Fig. 2 is that the present invention is at the structural representation of guide shell matrix surface preparation by the transition layer of being made up of silicon carbide whisker;
Fig. 3 is the surface scan electromicroscopic photograph of the present invention at the silicon carbide whisker of guide shell matrix surface growth in situ;
Fig. 4 is the X-Ray diffracting spectrum of the present invention at the silicon carbide whisker of guide shell matrix surface growth in situ;
Fig. 5 is the cross section stereoscan photograph of the present invention at the silicon carbide whisker of guide shell matrix surface growth in situ;
Fig. 6 is the A place enlarged diagram of Fig. 1;
Fig. 7 is the present invention when the preparation of guide shell matrix surface has transition layer and top layer, the surface scan electromicroscopic photograph on top layer;
Fig. 8 is SiC coating sample (curve I) isothermal oxidation weight loss curve in 1100 ℃ of air of the embodiment of the invention 6 (curve II), embodiment 8 (curve III), embodiment 2 (curve IV), embodiment 10 (curve V) and the preparation of traditional chemical vapour deposition process;
Fig. 9 be the embodiment of the invention 6 (curve II), embodiment 8 (curve III), embodiment 2 (curve IV), embodiment 10 (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
Below in conjunction with accompanying drawing and embodiment the present invention is described further.
Embodiment 1:
Can know by Fig. 1, Fig. 2, a kind of guide shell ORC, it comprises that the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ 2 by the matrix of carbon/carbon compound material preparation.
A kind of preparation method of the ORC of guide shell as stated, it may further comprise the steps:
⑴ get the raw materials ready: with the polishing of guide shell matrix, polishing, dry for standby after the washes clean;
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), the alcoholic acid volume accounts for 5%～20% (present embodiment is 20%) of overall solution volume, adds aqueous solution of urea, regulates making Ni
2+Concentration be (0.05～0.2) mol/L (present embodiment is 0.1mol/L), transfer in the reaction kettle after stirring;
⑶ loading catalyst: step ⑴ gained matrix is put into reaction kettle solution normal pressure dipping 5h～12h (present embodiment is 10 h); React 1h～3h (present embodiment is 2h) in the oil bath with reaction kettle immersion 95 ℃～120 ℃ (present embodiment is 110 ℃) then; After reaction kettle 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 for use;
⑷ growth in situ silicon carbide whisker: step ⑶ gained matrix 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 ℃), and 10min～60min (present embodiment is 15min) closes argon gas before arriving depositing temperature; Feed hydrogen catalyzer is reduced, hydrogen flowing quantity is 100mL/min～300mL/min (present embodiment is 200mL/min), is incubated 10min～60min (present embodiment is 15min) after reaching depositing temperature; Then with hydrogen as carrier gas and diluents; Throughput ratio is 1:1, with Bubbling method trichloromethyl silane is introduced in the cvd furnace, and the container bottle of splendid attire trichloromethyl silane places water bath with thermostatic control; 18 ℃～25 ℃ of bath temperatures (present embodiment is 22 ℃); Depositing time is 1h～50h (present embodiment is 6h), and pressure is normal pressure, prepares the transition layer of being made up of the silicon carbide whisker of growth in situ 2 at matrix surface.
Embodiment 2:
Present embodiment is convenient processing, and in step ⑴, described guide shell matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect through web member 5.A kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for processing with carbon/carbon compound material.
Surplus with embodiment 1.
Can know that by Fig. 3 the silicon carbide whisker of the present invention's preparation is evenly distributed at the guide shell matrix surface.
Can know that by Fig. 4 the present invention is β-SiCw at the silicon carbide whisker of guide shell matrix surface growth in situ.
Can know by Fig. 5; Cross section stereoscan photograph explanation silicon carbide whisker transition layer 2 porous of guide shell matrix and fine and close gradually along the direction of carbon/carbon composite material base body, this explanation transition layer 2 is fine with matrix bond, simultaneously; Transition layer 2 porous surfaces; When being provided with the top layer of forming by compact silicon carbide above that again, help alleviating the inner thermal stresses of coating, avoid coating cracking and come off.
Embodiment 3:
Can know that by Fig. 6 the present invention further improves anti-oxidation of coating, on transition layer 2, is provided with the top layer of being made up of compact silicon carbide 3.
Its preparation technology is in step ⑷, and depositing time is 2h.
After step ⑷ is intact, diluents 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 1h～50h (present embodiment is 4h), and 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.
Can know that by Fig. 7 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 described, good consistency arranged between two-layer in the evenly formation of silicon carbide whisker transition layer 2 surfaces.
Surplus with embodiment 1.
Embodiment 4:
Present embodiment is convenient processing, and in step ⑴, described matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect through web member 5.A kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for processing with carbon/carbon compound material.
Surplus with embodiment 1, embodiment 3.
Embodiment 5:
In step ⑷, depositing time is 3h, and during preparation top layer 3, depositing time is 3h.
Surplus with embodiment 1, embodiment 3.
Embodiment 6:
Present embodiment is convenient processing, and in step ⑴, described matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect through web member 5.A kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for processing with carbon/carbon compound material.
In step ⑷, depositing time is 3h, and during preparation top layer 3, depositing time is 3h.
Surplus with embodiment 1, embodiment 3.
Embodiment 7:
In step ⑷, depositing time is 5h, and during preparation top layer 3, depositing time is 1h.
Surplus with embodiment 1, embodiment 3.
Embodiment 8:
Present embodiment is convenient processing, and in step ⑴, described matrix comprises cylindrical shell 1, flange 4, and cylindrical shell 1, flange 4 connect through web member 5.A kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member 5, the pin of present embodiment for processing with carbon/carbon compound material.
In step ⑷, depositing time is 5h, and during preparation top layer 3, depositing time is 1h.
Surplus with embodiment 1, embodiment 3.
Can be known that by Fig. 8 the resistance of oxidation of the SiC coating sample of traditional chemical vapour deposition process preparation is the poorest, oxidation 10h rate of weight loss is 41.11% in 1100 ℃ of air, among Fig. 8 shown in the curve I.
Oxidation 10h rate of weight loss is respectively in 1100 ℃ of air of four embodiment coating samples of the present invention preparation: 8.87% (embodiment 4; Shown in the curve II), 5.50% (embodiment 6; Shown in the curve III), 2.07% (embodiment 2; Shown in the curve IV) and 0.87% (embodiment 8, shown in the curve V), its average rate of weight loss is 4.33%.
Can know that by Fig. 9 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. 9 shown in the curve I.
And four embodiment coating sample rate of weight loss of the present invention preparation are respectively: 11.09% (embodiment 4, shown in the curve II), and 5.66% (embodiment 6; Shown in the curve III); 0.51% (embodiment 2, shown in the curve IV) and 0.22% (embodiment 8, shown in the curve V).
The SiC coating for preparing for the ease of the coating of relatively the present invention's 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 present invention 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.
Silicon carbide whisker is that a kind of diameter is nano level to a micron-sized single crystal fibre, has good characteristics such as HS, high firmness, high elastic coefficient and density are low, corrosion-resistant, chemical property stable, oxidation-resistance property is strong.The present invention is through in surface preparation growth in situ SiCw coating that is prepared guide shell by carbon/carbon compound material and the toughness reinforcing SiCw-SiC coating of SiCw; The oxidation-resistance of coating and thermal shock resistance increase substantially than the SiC coating of traditional method preparation; And realized the coating prepn of serialization under the normal pressure; Adopt plurality of raw materials, several different methods to prepare the technology of coating with respect to other; The present invention has simplified the preparation process of coating greatly, improved greatly guide shell over-all properties, help promoting the use of of coating.
Claims (8)
1. the preparation method of a guide shell ORC is characterized in that it may further comprise the steps:
⑴ get the raw materials ready: will be by the polishing of guide shell matrix, the polishing of carbon/carbon compound material preparation, dry for standby after the washes clean;
⑵ Preparation of Catalyst: the presoma alcohol solution of preparation catalyzer makes Ni in the solution
2+: Al
3+=(5～15): (1～3), the alcoholic acid volume accounts for 5%～20% of overall solution volume, adds aqueous solution of urea, regulates making Ni
2+Concentration be 0.05 mol/L～0.2mol/L, transfer in the reaction kettle after stirring;
⑶ loading catalyst: step ⑴ gained matrix is put into reaction kettle solution normal pressure dipping 5h～12h; React 1h～3h in the oil bath with 95 ℃～120 ℃ of reaction kettle immersions then; After reaction kettle is chilled to room temperature with cold water matrix is therefrom taken out, the back of drying in the shade at normal temperatures is for use;
⑷ growth in situ silicon carbide whisker: step ⑶ gained matrix is put into chemical vapor deposition stove, vacuumize, feed argon gas; Under argon shield, heat up, depositing temperature is 950 ℃～1250 ℃, and 10min～60min closes argon gas before arriving depositing temperature; Feed hydrogen catalyzer reduced, be incubated 10min～60min after reaching depositing temperature, then with hydrogen as carrier gas and diluents; Throughput ratio is 1:1, with Bubbling method trichloromethyl silane is introduced in the cvd furnace, and the container bottle of splendid attire trichloromethyl silane places water bath with thermostatic control; 18 ℃～25 ℃ of bath temperatures; Depositing time is 1h～50h, and pressure is normal pressure, prepares the transition layer (2) of the silicon carbide whisker composition of growth in situ at matrix surface.
2. the preparation method of guide shell ORC according to claim 1 is characterized in that the transition layer of forming at silicon carbide whisker (2) upward prepares the top layer of being made up of compact silicon carbide (3), after the silicon carbide whisker deposition is accomplished; Diluents is changed into argon gas; Carrier gas is a hydrogen, and adjustment diluting gas flow and carrier gas flux be than being 2:1, and depositing temperature is 950 ℃～1250 ℃; Depositing time is 1h～50h, and pressure is normal pressure.
3. the preparation method of guide shell ORC according to claim 1 and 2 is characterized in that in step ⑴, and described matrix comprises cylindrical shell (1), flange (4), and cylindrical shell (1), flange (4) connect through web member (5).
4. the preparation method of guide shell ORC according to claim 3 is characterized in that a kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member (5).
5. guide shell ORC of method preparation according to claim 1, it comprises by the matrix of carbon/carbon compound material preparation, it is characterized in that the surface of matrix is provided with the transition layer of being made up of the silicon carbide whisker of growth in situ (2).
6. the guide shell ORC like the said method preparation of claim 2 is characterized in that transition layer (2) is provided with the top layer of being made up of compact silicon carbide (3).
7. according to claim 5 or 6 described guide shell ORCs, it is characterized in that described matrix comprises cylindrical shell (1), flange (4), cylindrical shell (1), flange (4) connect through web member (5).
8. guide shell ORC according to claim 7 is characterized in that a kind of in the screw processed with carbon/carbon compound material or bolt or double-screw bolt or the pin of described web member (5).
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| CN102296355B (en) * | 2011-06-27 | 2013-12-11 | 湖南金博复合材料科技有限公司 | Guide shell made from carbon/carbon composite material and production method |
| CN102242348A (en) * | 2011-06-30 | 2011-11-16 | 山东理工大学 | Preparation method of silicon carbide composite film of reflector used in space |
| CN105568368A (en) * | 2015-06-16 | 2016-05-11 | 杭州海纳半导体有限公司 | Thermal field and method for protecting thermal field component to reduce loss |
| CN114232074B (en) * | 2021-12-20 | 2023-03-21 | 中南大学 | Quartz fiber/carbon fiber reinforced carbon-based composite guide cylinder and preparation method thereof |
| CN116768653B (en) * | 2023-06-15 | 2024-04-02 | 湖南世鑫新材料有限公司 | Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof |
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