CN1164524C - Process for preparing silicon carbide/carbon and boron carbide/carbon functional gradient material - Google Patents
Process for preparing silicon carbide/carbon and boron carbide/carbon functional gradient material Download PDFInfo
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- CN1164524C CN1164524C CNB011004495A CN01100449A CN1164524C CN 1164524 C CN1164524 C CN 1164524C CN B011004495 A CNB011004495 A CN B011004495A CN 01100449 A CN01100449 A CN 01100449A CN 1164524 C CN1164524 C CN 1164524C
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Abstract
The present invention relates to a method for preparing a SiC/C and B4 C/C functional gradient material by component distribution design and a hot pressed sintering method. The present invention is characterized in that A sintering auxiliary agent is added into a raw material of a low atomic number ceramic-carbon block gradient material. Active carbon powder and B powder are adopted as sintering auxiliary agents of SiC for SiC/C FGM. The B+C content of the sintering auxiliary agents of the SiC is from 1 to 10 wt%, and the content of carbon material additive B is from 1 to 10 wt%. The SiC is added into B4 C/C FGM to enhance performance. The distributed design of linear components is adopted by the SiC/C FGM, and the distributed design of S-shaped components is adopted by the B4 C/C FGM. The pressure in the argon atmosphere is from 15 to 50MPa, the temperature in the argon atmosphere is from 1900 DEG C to 2200 DEG C, and the temperature is kept for 1 to 3 hours. The present invention has the advantages of excellent high temperature resistant plasma flushing performance, thermal shock resistant performance and chemical sputtering resistant performance.
Description
Technical field
The present invention relates to a kind of employing composition profiles design and hot pressed sintering and prepare SiC/C and B
4The method of C/C Functionally Graded Materials.
Background technology
The quick hero of Japan's scholar's horizontal well, Xinye people such as grade has just proposed these material new ideas of Functionally Graded Materials in 1986, and successively with chemical vapour deposition (Chemical Vapor Deposition, CVD) and chemical vapor infiltration (Chemical Vapor Infiltration CVI) has prepared the SiC/C Functionally Graded Materials.CVD technology SiCl
4-CH
4-H
2As unstripped gas, be deposited under 1400 ℃ and 1500 ℃ and carry out, total gaseous tension scope is 1.3-6.5KPa, by SiC/C ratio in the suitable variation unstripped gas, on graphite matrix, obtain thickness and be 0.2-0.8mm the SiC/C Functionally Graded Materials (Functionally Graded Material, FGM).CVI technology is that the combustion chamber matrix that the carbon fiber control of two-dimensional braided constitutes feeds CH under 1100 ℃ of-1500 ℃ of conditions
4And SiCl
4Form the good SiC/C Functionally Graded Materials of resistance to air loss.
Produce SiC and B with the powder metallurgy heat pressing process
4C pottery, Functionally Graded Materials have many reports.But prepare block SiC/C FGM and B with heat pressing process
4C/C FGM does not appear in the newspapers as yet.
Summary of the invention
The objective of the invention is to: provide a kind of employing composition profiles design and hot pressed sintering to prepare SiC/C and B
4The method of C/C Functionally Graded Materials is with graphite good thermal shock resistance and SiC and B
4The high temperature resistant plasma body that C is good washes away and anti-CD
4The chemical sputtering performance combines, and not only makes the thickness of gradient material bring up to 6～10mm, and compares the production cycle of having accelerated material preparation greatly with chemical vapor infiltration with chemical vapour deposition, has reduced production cost.
The formation of invention:
The present invention adopts hot pressed sintering to prepare SiC/C and B
4The C/C Functionally Graded Materials, it is characterized in that in low atomic number pottery-carbon block gradient material raw material, adding sintering aid, for SiC/C FGM, wherein active C powder and B powder are as the sintering aid of SiC, SiC ceramic post sintering auxiliary agent B+C should be at 3-10wt% (weight percent), C content can change in the 3-10wt% scope, and C content is preferentially selected 3-5wt%; B content changes in the 0-2wt% scope, and B content is preferentially selected 1-2wt%.The content of carbon body meterial additive B should be at 1-10wt%, and the content of carbon body meterial additive B is preferentially selected 3-5wt%.B
4Add SiC among the C/C FGM to improve performance.
Raw material adopts commercially available SiC powder, active C powder, B powder and B
4The C powder.The physical and chemical performance of raw material is as shown in table 1.
Table 1: the physical and chemical performance of raw material
| Powder | Granularity (μ) | Purity (%) |
| SiC | ?0.05～0.5 | ＞97 |
| Active C | ?＜1 | ＞95 |
| B | ?2～3 | ＞90 |
| B 4C | ?20 | ＞90 |
The composition profiles of SiC/C FGM adopts linear composition profiles.For B
4C/C FGM, B
4The reason that the C slabbing is opened is B
4The C layer line coefficient of expansion is big, is subjected to tension stress and B in sintering process
4The Young's modulus of C one end is also much bigger than C, so should slow down B
4The composition of C end changes.C layer intensity is low, and the variation of C end composition also will relax.The two ends composition all relaxes, and the composition profiles curve has just become the S type.The composition profiles function of S type is suc as formula (1). is the volume fraction of one of them phase; X is the relative distance from the surface; δ is the Functionally Graded Materials sample thickness; N is an index, and it is a parameter of graded feature.
Dispose SiC/C or B respectively
4C-SiC/C is the batching (and each gradient layer of gradient material) of 0～100% different volumes ratio, places agate jar ethanol medium ball milling to mix 6 hours batching, dries in air, and mixed powder is crossed 100 mesh sieves.Preparation SiC/C FGM and B
4C-SiC/C FGM is according to different composition profiles parameters, calculate the quality of each gradient layer, and the manual lamination cloth of the batching of each gradient layer placed φ 40mm graphite jig, in Ar atmosphere, hot pressed sintering under 15-50MPa pressure, 1900 ℃ of-2200 ℃ of hot conditionss, be incubated 0.5-3 hour, obtain SiC/C FGM and B
4C-SiC/C FGM.
The invention has the advantages that: prepare block SiC/C FGM and B
4C-SiC/C FGM, its SiC and B
4The C-SiC layer thickness reaches 1-2mm, compares with the SiC/C FGM of CVD and CVI prepared, and scour resistance improves greatly.Simultaneously with production cycle of the SiC/C FGM of CVD and CVI prepared more than 100 hours, and adopt hot pressed sintering, the production cycle shortens greatly.The present invention also in the preparation of function-graded material, especially has broad application prospects in the preparation of block gradient function gradient material except that can be used as nuclear fusion stack material, heatshield material, hot machine material.SiC/C FGM and B
4Preparation technology's synoptic diagram of C-SiC/C FGM is seen Fig. 1.
Description of drawings
The present invention will be further described below in conjunction with accompanying drawing.
Fig. 1 is preparation technology's schema of the present invention, and wherein (1) is batch mixing, and (2) are the lamination cloth, and (3) are the sample compacting, and (4) are hot pressing, and (5) are the FGM sample.
Fig. 2 is the organization chart of SiC layer behind the SiC/C FGM original position pre-irradiation of the present invention, (a) is pre-irradiation, (b) be irradiation after.
Fig. 3 is n=2 of the present invention, and the 1st layer of c is 20% S type B
4C-SiC/C FGM composition profiles graphic representation.(6) be the S type composition profiles curve of index n=2, (7) are linear composition profiles curve, and (8) are the power function composition profiles curve of index n=2.
Fig. 4 is B of the present invention
4The CD of C-SiC/C FGM and graphite
4The chemical sputtering collection of illustrative plates.Wherein BSC990706 and BSC990707 are B
4C-SiC/C FGM, SMF800 are secondarily purified graphite.
Embodiment
Example 1:
Prepared 7 layers of SiC/C Functionally Graded Materials by following composition, every layer thickness is 1mm.In Ar atmosphere, hot pressed sintering under 25MPa pressure, 1 hour the condition of 1950 ℃ of following insulations of high temperature obtains SiC/C FGM.
100％C+(60％C+40％SiC)+(40％C+60％SiC)+(20％C+80％SiC)+
10%C+90%SiC)+(5%C+95%SiC)+100%SiC, (vol% volume percent)
Xinan Nuclear Physics Research Academy is detected the high temperature resistant plasma body performance of flushing of material, and the SiC/C FGM that with B+C is sintering aid is at D
+The chemical sputtering rate has only 20～30% of SMF-graphite under the irradiation, this result is consistent with the original position silication coating (＜1000 ) of employing now among the HL-1M, but because SiC/C FGM thickness is millimeter magnitude (as 1mm), press each the discharge to the etching rate 5 calculating of PFM among the HL-1M, SiC/C FGM can experience 2 * 10
6Inferior discharge, this compares with original position silication coating discharge time is to have improved greatly.
The CD of SiC/C FGM
4The venting rate is well below the CD of SMF graphite
4Venting rate, the SiD of SiC/C FGM simultaneously
4The venting rate is much smaller than the CD of SiC/C FGM
4The venting rate, they all differ an order of magnitude.The D of SiC/CFGM
2And CD
4Peak temperature also obviously greater than the D of graphite
2And CD
4Peak temperature, prove the D of SiC/CFGM
2And CD
4The distillation intensity of activation be higher than graphite far away.
To place by the SiC/C FGM of manufacturing of the present invention and carry out original position irradiation on the HL-1M tokamak device, before and after this material irradiation, microtexture does not have considerable change, meets the technical requirement towards plasma material of fusion reactor fully.
The weave construction of SiC layer (a) is pre-irradiation as shown in Figure 2 behind the SiC/C FGM original position pre-irradiation, (b) be irradiation after.
Example 2:
Get n=2, the 1st layer of c is 20%, in Ar gas, is warmed up to 2000 ℃, and pressure 20MPa is incubated 1 hour, prepares 11 layers, and thickness is the B of 6mm
4C-SiC/C FGM, its S type composition profiles curve as shown in Figure 3.
11 layers of 80%B of S type
4Flawless after C-20%SiC/C (volume percent) the FGM hot pressing, a strip bending strength is 189MPa; Hardening behind 500 ℃ of insulations of another strip 0.5h, bending strength is 216MPa, therefore, the heat-shock resistance Δ
Fc＞500 ℃.80%B
4The CD of C-20%SiC/C FGM (BSC990706 and BSC990707)
4Yield only is the about 50% of secondarily purified graphite (SMF800), and Fig. 4 is B
4The chemical sputtering collection of illustrative plates of C/C FGM and graphite.
Claims (1)
1, a kind of preparation SiC, B
4The method of C-carbon body Functionally Graded Materials is characterized in that: to SiC, B
4Add sintering aid in the C-carbon body Functionally Graded Materials raw material, for SiC/C FGM, adopt activated carbon powder and B powder to make the sintering aid of SiC, the sintering aid B+C content of SiC is 3-10 weight %, and the content of carbon body meterial additive B is 1-10 weight %; C content changes in 3-10 weight % scope, and B content changes in 0-2 weight % scope; SiC/C FGM adopts linear composition profiles design; B
4C-SiC/CFGM adopts the design of S type composition profiles; is the volume fraction of one of them phase; X is the relative distance from the surface; δ is the Functionally Graded Materials sample thickness; N is an index, and it is a parameter of graded feature; The design of S type composition profiles is represented with following formula:
Sintering process is: in argon gas atmosphere, pressure is that 15-50MPa, temperature are 1900 ℃-2200 ℃, is incubated 0.5-3 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011004495A CN1164524C (en) | 2001-01-12 | 2001-01-12 | Process for preparing silicon carbide/carbon and boron carbide/carbon functional gradient material |
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|---|---|---|---|
| CNB011004495A CN1164524C (en) | 2001-01-12 | 2001-01-12 | Process for preparing silicon carbide/carbon and boron carbide/carbon functional gradient material |
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|---|---|
| CN1364745A CN1364745A (en) | 2002-08-21 |
| CN1164524C true CN1164524C (en) | 2004-09-01 |
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| CNB011004495A Expired - Fee Related CN1164524C (en) | 2001-01-12 | 2001-01-12 | Process for preparing silicon carbide/carbon and boron carbide/carbon functional gradient material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2857660B1 (en) * | 2003-07-18 | 2006-03-03 | Snecma Propulsion Solide | THERMOSTRUCTURAL COMPOSITE STRUCTURE HAVING A COMPOSITION GRADIENT AND METHOD OF MANUFACTURING THE SAME |
| CN1313419C (en) * | 2003-12-19 | 2007-05-02 | 李文辉 | Producing method for composite carbide ceramic material by liquid-phase sintering and ceramic products |
| CN100430339C (en) * | 2003-12-19 | 2008-11-05 | 李文辉 | Ceramic slide bearing and its producing method |
| CN103723729B (en) * | 2013-12-27 | 2015-04-22 | 黑龙江工程学院 | Preparation method of gradient activated carbon |
| CN113816755B (en) * | 2021-10-14 | 2023-09-01 | 西安鑫垚陶瓷复合材料有限公司 | Two-dimensional silicon carbide/silicon carbide composite bar and preparation method of connecting piece |
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