CN101240417A - Method for preparing silicon carbide reflecting mirror material and CVI forming device thereof - Google Patents
Method for preparing silicon carbide reflecting mirror material and CVI forming device thereof Download PDFInfo
- Publication number
- CN101240417A CN101240417A CNA2007100343800A CN200710034380A CN101240417A CN 101240417 A CN101240417 A CN 101240417A CN A2007100343800 A CNA2007100343800 A CN A2007100343800A CN 200710034380 A CN200710034380 A CN 200710034380A CN 101240417 A CN101240417 A CN 101240417A
- Authority
- CN
- China
- Prior art keywords
- sic
- cvi
- graphite
- gas
- deposition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a preparing method for SiC reflector material and a CVI forming device for the preparing method. The method is: using 50 to 200 mesh Sic power as raw material put in the graphite cavity of the CVI forming device, methyltrichlorosilane as Sic gas source, H2 as eluant gas and diluent gas, Ar as protective gas, under a temperature of 1000 to 1300 DEG C, depositing SiC to form a blank by CVI method; after shucking off the graphite cavity, repeatedly CVI depositing SiC to intensify the blank and mechanically processing for several times; and preparing SiC reflecting layer on the surface of the SiC blank by CVD method. For reflector material prepared by the invention, crackle is not easy to appear, since the base and coating have same heat performance, the production period is greatly reduced, the production cost is lowered, and multiple workpieces can be deposited at the same time.
Description
Technical field
The present invention relates to the preparation method and the employed CVI building mortion of this method of SiC reflecting mirror material.
Background technology
At present, the SiC speculum is widely used in each field such as large-scale space telescope, large-scale ground visual telescope, early warning satellite, sounding satellite, reconnaissance satellite, weather satellite, high energy laser weapon, laser radar system, vacuum ultraviolet ray visual telescope and high resolution space camera.The method for preparing the SiC reflecting mirror material both at home and abroad mainly contains hot isostatic pressing method (Hot Isostatic Pressing, HIP), reaction sintering (ReactionBoned, RB) and chemical vapor infiltration/chemical Vapor deposition process (Chemical VaporInfiltration/Chemical Vapor Deposition, CVI/CVD).Wherein, the SiC material density of HIP and the preparation of RB method is not high, and the optics working accuracy is low.The material of CVI/CVD method preparation is owing to have the density height, the optics good processability, and isotropy, do not have shrink, near advantage such as size shaping, be the method for preparing SiC (or C/SiC) reflecting mirror material of present widespread use.
At present, being equipped with the main technological process of SiC (or C/SiC) reflecting mirror material with the CVI/CVD legal system is: low close porous SiC (or C/SiC) base substrate of preparation earlier, mainly contain 3 kinds of modes at present: 1. use (normally Polycarbosilane, PCS) compacting formation base substrate, the pyrolysis again of SiC powder and precursor; 2. be matrix with low close C/C, chemical vapor infiltration SiC or fusion siliconising; 3. pyrolysis porous thermohardening polymkeric substance obtains the porous carbon skeleton, adopts CVI method surface deposition SiC within it then, obtains open celled foam SiC.After preparing low close porous SiC (or C/SiC) base substrate, obtain density SiC (or C/SiC) material by CVI method deposition SiC again, carry out surperficial mechanical workout after, at last in material surface deposition one deck SiC coating as plane of reflection.
Above several method is perhaps owing to exist the polymer unwinds residue, perhaps owing to there is heterogeneous material such as C fiber, still there is some difference between the thermal characteristics of matrix thermal characteristics and SiC coating, therefore, when coating arrives certain thickness, still be easy to generate crackle.On the other hand, the production cycle of traditional C VD technology vapor phase growth SiC material is longer, the production cost height.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of new SiC reflecting mirror material, solve matrix and be coated with the problem that interlayer easily cracks, and this method is with short production cycle, preparation cost is low, the global density of material is low.
Detailed technology scheme of the present invention is: with 50～200 order SiC powder is raw material, contain in the graphite cavity, and be the SiC source of the gas with trichloromethyl silane (MTS), H
2As carrier gas and diluent gas, Ar is a shielding gas, and CVI method deposition SiC forms base substrate; Repetition CVI deposition SiC makes base substrate density and mechanical workout several times after sloughing the graphite cavity; The CVD method prepares the SiC reflecting layer in the SiC billet surface.
Among the present invention, CVI gas mole ratio proportioning is preferably MTS: H
2=1: 4～1: 12, Ar: H
2≈ 1: 1.
CVI of the present invention is preferably isothermal CVI, and depositing temperature is 1000～1300 ℃, and deposition pressure preferably is not higher than 10KPa.
For the CVI/CVD method of existing preparation SiC reflecting mirror material, blank of material of the present invention is made up of SiC powder and CVI-SiC, and this material thermal expansion coefficient is 2.4～4.0 * 10 in the time of 100～800 ℃
-6K
-1, and the thermal expansivity of the CVD-SiC coating of billet surface is 2.2～3.8 * 10
-6K
-1, the two is very approaching, and therefore, the reflecting mirror material of the present invention preparation because thermal characteristics is consistent, therefore is difficult for cracking between its matrix and the coating, and optics processing back mirror surfaceness reaches 8
Below the RMS.
The present invention adopts the SiC powder as CVI deposition matrix additive, has shortened the time of CVI deposition SiC greatly, and is with short production cycle.In addition, because the present invention adopts isothermal CVI depositing operation, sedimentary province has identical deposition effect, can realize that multiplex's part deposits simultaneously, and production cost reduces.
Because the SiC matrix of CVI method preparation has density gradient, density of material is increased to the surface gradually by core, and surface density greatly reduces the weight of speculum near the SiC theoretical density.Density of material is lower than reaction sintering SiC and hot isostatic pressing SiC, lightweight efficient about 30%.
The present invention is that raw material passes through CVI method formation of deposits base substrate with the SiC powder directly, therefore, the present invention also provides the CVI building mortion of a special use, this device is in conventional CVI device inside, set up a graphite chamber for SiC powder CVI deposition formation, the graphite chamber is movable detachable type, establishes a plurality of gas ports on the stone ink cavity wall, and the inwall of graphite chamber part with holes is established charcoal fibrous reticulum tire.
For the ease of slough the graphite chamber in follow-up CVI process, the porous graphite chamber is set to movable detachable type, can be made up of two semicircular cylinders with holes as cavity, or be made up of a cylinder and mobilizable up and down two porous gaskets.Certainly, the formation of detachable cavity is not limited to above two kinds.
Because air guide aperture ratio SiC powder is big, the SiC powder may be taken out of from gas port by air-flow in the CVI process, therefore, establishes charcoal fibrous reticulum tire at the inwall at position with holes, graphite chamber and can prevent that the SiC powder from spilling from the hole.
Simultaneously, for the ease of the demoulding and in order to penetrate gas better, one deck perforate graphite paper also can be set between the charcoal fibrous reticulum tire of graphite cavity wall and the stone ink cavity wall, but the aperture of the little pore distribution stone ink cavity wall of graphite paper matches.
In order to prevent to constitute the contact site bonding of graphite cavity each several part, or SiC powder bonded in order to prevent that the graphite chamber is inner with it, can be in graphite cavity each several part contact site, and fill up graphite paper between graphite cavity wall and the SiC powder.
Description of drawings
Fig. 1 SiC powder CVI building mortion synoptic diagram;
Air guide Graphite pad synoptic diagram among Fig. 2 Fig. 1.
Embodiment
Describe the specific embodiment of the present invention in detail below in conjunction with Figure of description.
Embodiment 1
The CVI building mortion is to increase a graphite chamber and constitute in conventional CVI cvd furnace.Graphite cavity 2 is made up of two semicircular cylinders and upper and lower two air guide Graphite pads 4, for the ease of the demoulding, and contact surface pad graphite paper 5, graphite cavity 2 is by graphite outer die casing 1 banding.Between SiC powder 3 and graphite cavity 2 inwalls is one deck graphite paper 5, prevent SiC powder 3 in the CVI process with the 2 inwall adhesions of graphite cavity.Because air guide Graphite pad 4 aperture ratio SiC powder are big, the SiC powder may be taken out of by air-flow in the CVI process, it between SiC powder 3 and air guide Graphite pad 4 one deck charcoal fibrous reticulum tire 7, equally for the ease of the demoulding, charcoal fibrous reticulum tire 7 is one deck graphite paper 5 with air guide Graphite pad 4, and its aperture distribution situation and air guide Graphite pad 4 are identical.In the CVI process, reactant gases gradually to SiC powder 3 internal divergence, is adsorbed on SiC particle surface generation chemical reaction by two ends graphite air guide pad 4, graphite paper 5 and charcoal fibrous reticulum tire 7, and reacted gas is finished the CVI process to the powder external diffusion.
Preparation size is the SiC reflecting mirror material of φ 150 * 20mm.Preparation process and correlation parameter are as follows: (1) is that 50 purposes β-SiC powder is packed in the graphite chamber with granularity.(2) make the SiC powder forming in 1100 ℃ of following CVI deposition SiC density.Processing parameter is: MTS: H
2=1: 12, the Ar airshed is 200ml/min, and deposition pressure 300Pa, depositing time are 50h; (3) slough the graphite cavity after, CVI density 50h once more; (4) on diamond grinders' dop, the SiC base substrate is carried out preliminary mechanical workout, increase surface porosity factor and make base substrate have certain planeness; (5) repeat CVI deposition SiC density 2 times, each depositing time is 50h, and depositing temperature is 1300 ℃, MTS: H
2=1: 8, the Ar flow is 300ml/min, and deposition pressure is controlled at about 5kPa, needs billet surface is carried out mechanical workout before each density; (6) in the CVD SiC coating of the about 500 μ m of billet surface deposition one deck, processing parameter is identical with step 2.Sample sees Table 1 in the density of different steps in the preparation process.
Table 1
| Frequency of depositing | 1 |
2 |
3 CVI | 4 CVI | The CVD coating |
| Density (g/cm 3) | 2.0 | ?2.17 | ?2.24 | ?2.24 | ?2.30 |
Adopt 50 order SiC powder as CVI matrix additive, blank density is 2.0g/cm after being shaped by CVI
3, in follow-up compaction process, the density of base substrate increases to some extent, but blank density is much smaller than CVDSiC theoretical density 3.2g/cm
3
Preparation is by the SiC reflecting mirror material of varigrained SiC powder, identical CVI depositing operation, and sample size is φ 50 * 15mm.Its preparation process and correlation parameter are: (1) is respectively 50 orders, 200 purpose SiC powder with granularity and packs in the graphite chamber.(2) in 1100 ℃ of following CVI deposition SiC density the matrix additive is shaped.Processing parameter is: MTS: H
2=1: 12, the Ar flow is 200ml/min, and deposition pressure 300Pa, depositing time are 50h; (3) slough the graphite cavity after, CVI density 50h once more; (4) on diamond grinders' dop, the SiC base substrate is carried out preliminary mechanical workout, increase surface porosity factor and make base substrate have certain planeness; (5) repeat density 2 times, each depositing time is 50h, and depositing temperature is 1300 ℃, MTS: H
2=1: 8, the Ar flow is 300ml/min, and deposition pressure is controlled at about 5kPa, needs billet surface is carried out mechanical workout before each density; (6) in the CVD SiC coating of the about 500 μ m of billet surface deposition one deck, the CVD processing parameter is identical with step 2; (7) speculum is carried out optics processing.Each sample sees Table 2 in the parameter of different steps in the preparation process.
Table 2
Two kinds of varigrained SiC powder are as CVI matrix additive, and the back density that is shaped is respectively 1.85g/cm
3, 1.91g/cm
3Sample 1 and its surfaceness of sample 2 optics processing back are 3RMS and 8RMS.
Claims (7)
1. the preparation method of a silicon carbide reflecting mirror material, it is characterized in that comprising following steps: with 50～200 order SiC powder is raw material, contain in the graphite cavity, with the trichloromethyl silane SiC source of the gas, H
2As carrier gas and diluent gas, Ar is a shielding gas, and CVI method deposition SiC forms base substrate; Repetition CVI deposition SiC makes base substrate density and mechanical workout several times after sloughing the graphite cavity; The CVD method prepares the SiC reflecting layer in the SiC billet surface.
2. the method for claim 1, it is characterized in that: CVI gas mole ratio proportioning is MTS: H
2=1: 4～1: 12, Ar: H
2≈ 1: 1.
3. the method for claim 1, it is characterized in that: CVI is isothermal CVI, and depositing temperature is 1000 ℃～1300 ℃, and deposition pressure is not higher than 10KPa.
4. CVI device, comprise the CVI cvd furnace, it is characterized in that: a graphite chamber for SiC powder CVI deposition formation also is set in stove, and the graphite chamber is movable detachable type, establish a plurality of gas ports on the stone ink cavity wall, the inwall at position with holes, graphite chamber is established charcoal fibrous reticulum tire.
5. device as claimed in claim 4 is characterized in that: described graphite cavity is made up of two semicircular cylinders with holes, or is made up of a cylinder and mobilizable up and down two porous gaskets.
6. device as claimed in claim 4 is characterized in that: establish one deck perforate graphite paper between the charcoal fibrous reticulum tire of graphite cavity wall and the stone ink cavity wall.
7. device as claimed in claim 4 is characterized in that: in graphite cavity each several part contact site, and fill up graphite paper between graphite cavity wall and the SiC powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100343800A CN100557078C (en) | 2007-02-05 | 2007-02-05 | A kind of preparation method of silicon carbide reflecting mirror material and CVI building mortion thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100343800A CN100557078C (en) | 2007-02-05 | 2007-02-05 | A kind of preparation method of silicon carbide reflecting mirror material and CVI building mortion thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101240417A true CN101240417A (en) | 2008-08-13 |
| CN100557078C CN100557078C (en) | 2009-11-04 |
Family
ID=39932238
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100343800A Expired - Fee Related CN100557078C (en) | 2007-02-05 | 2007-02-05 | A kind of preparation method of silicon carbide reflecting mirror material and CVI building mortion thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100557078C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728682A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Foam silicon reflecting mirror and manufacturing method thereof |
| CN104152869A (en) * | 2014-08-22 | 2014-11-19 | 中国科学院宁波材料技术与工程研究所 | Plasma thin film deposition device and deposition method |
| WO2017132902A1 (en) * | 2016-02-03 | 2017-08-10 | 深圳市商德先进陶瓷股份有限公司 | High-purity silicon carbide ceramic preparation method and ceramic substrate |
| CN109352374A (en) * | 2018-11-19 | 2019-02-19 | 中国航空工业集团公司洛阳电光设备研究所 | A kind of SiC reflecting mirror pre-made powder green body mitigates the clamping tooling and processing method of slot |
| CN109581556A (en) * | 2018-11-26 | 2019-04-05 | 中国科学院长春光学精密机械与物理研究所 | A kind of carbon fiber composite material reflector preparation process |
| CN110483001A (en) * | 2019-08-19 | 2019-11-22 | 扬州霞光光学仪器有限公司 | Silicon carbide optical frames and preparation method thereof |
| CN113333374A (en) * | 2021-06-10 | 2021-09-03 | 厦门士兰明镓化合物半导体有限公司 | Method for cleaning graphite plate |
| CN116143548A (en) * | 2023-03-06 | 2023-05-23 | 吉林大学 | Method for preparing reflection-increasing film based on laser processing reaction sintering silicon carbide |
-
2007
- 2007-02-05 CN CNB2007100343800A patent/CN100557078C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728682A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | Foam silicon reflecting mirror and manufacturing method thereof |
| CN104152869A (en) * | 2014-08-22 | 2014-11-19 | 中国科学院宁波材料技术与工程研究所 | Plasma thin film deposition device and deposition method |
| WO2017132902A1 (en) * | 2016-02-03 | 2017-08-10 | 深圳市商德先进陶瓷股份有限公司 | High-purity silicon carbide ceramic preparation method and ceramic substrate |
| CN109352374A (en) * | 2018-11-19 | 2019-02-19 | 中国航空工业集团公司洛阳电光设备研究所 | A kind of SiC reflecting mirror pre-made powder green body mitigates the clamping tooling and processing method of slot |
| CN109581556A (en) * | 2018-11-26 | 2019-04-05 | 中国科学院长春光学精密机械与物理研究所 | A kind of carbon fiber composite material reflector preparation process |
| CN110483001A (en) * | 2019-08-19 | 2019-11-22 | 扬州霞光光学仪器有限公司 | Silicon carbide optical frames and preparation method thereof |
| CN113333374A (en) * | 2021-06-10 | 2021-09-03 | 厦门士兰明镓化合物半导体有限公司 | Method for cleaning graphite plate |
| CN116143548A (en) * | 2023-03-06 | 2023-05-23 | 吉林大学 | Method for preparing reflection-increasing film based on laser processing reaction sintering silicon carbide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100557078C (en) | 2009-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100557078C (en) | A kind of preparation method of silicon carbide reflecting mirror material and CVI building mortion thereof | |
| CN109721377B (en) | Carbon fiber reinforced silicon carbide ceramic matrix composite and preparation method thereof | |
| CN108706978B (en) | Method for preparing silicon carbide ceramic matrix composite by combining spray granulation with 3DP and CVI | |
| CN103724014B (en) | Preparation method of diamond doped silicon carbide (SiC) ceramics with high heat conductivity | |
| CN110105075B (en) | High-purity carbon fiber reinforced silicon carbide composite material and preparation method thereof | |
| CN102276279B (en) | Preparation method of silicon carbide fiber reinforced silicon carbide composite material | |
| CN104311090B (en) | A kind of hot pressed sintering/presoma cracking process prepares the method for Cf/ZrC-SiC ultrahigh temperature ceramic composite | |
| CN107698271B (en) | High-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material and preparation method thereof | |
| CN110171976A (en) | The preparation method and product of SiC base ceramic part based on increasing material manufacturing | |
| CN102924106A (en) | Method for preparing carbon-silicon carbon composite material and product thereof | |
| JPH02279575A (en) | Production of sintered ceramic body having dense ceramic film | |
| CN102617178A (en) | C/SiC composite material, preparation method of composite material and friction plate | |
| CN110372390A (en) | Continuous fiber reinforced SiC part preparation method and product based on increasing material manufacturing | |
| CN106946582A (en) | A kind of Large Size Special Shaped C-base composte material component and preparation method thereof | |
| EP3700876B1 (en) | Particulate ceramic composite material, part comprising the same, and method for the production of said part | |
| CN105198437A (en) | Method for preparing porous silicon carbide ceramics | |
| CN103724046B (en) | A kind of SiC foam and preparation method thereof | |
| US20180044249A1 (en) | A method of fabricating a composite material part by self-propagating high temperature synthesis | |
| CN108911789A (en) | A kind of preparation method of C/C composite material surface SiC coating | |
| CN109251049A (en) | A method of limitation matrices of composite material propagation of internal cracks | |
| CN109180161B (en) | High-purity titanium silicon carbide/alumina composite material and preparation method thereof | |
| CN103058696A (en) | Preparation method for silicon nitride matrix | |
| CN102184873A (en) | Method for preparing diamond-silicon carbide electronic packaging material fast | |
| CN104451886A (en) | Preparation method of composite seed tray for growing A1N single crystals by PVT method | |
| CN105347799A (en) | Preparation method of large-particle-diameter Diamond/SiC composite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091104 Termination date: 20100205 |