CN1344810A - In-situ compounding process of preparing silicon carbide particle reinforced molybdenum silicide based composite material - Google Patents
In-situ compounding process of preparing silicon carbide particle reinforced molybdenum silicide based composite material Download PDFInfo
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- CN1344810A CN1344810A CN 01141978 CN01141978A CN1344810A CN 1344810 A CN1344810 A CN 1344810A CN 01141978 CN01141978 CN 01141978 CN 01141978 A CN01141978 A CN 01141978A CN 1344810 A CN1344810 A CN 1344810A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 39
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000002245 particle Substances 0.000 title claims abstract description 12
- 230000008569 process Effects 0.000 title claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 7
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 238000013329 compounding Methods 0.000 title claims description 4
- 229910021344 molybdenum silicide Inorganic materials 0.000 title claims description 4
- 229910016006 MoSi Inorganic materials 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000007731 hot pressing Methods 0.000 claims abstract description 13
- 239000011159 matrix material Substances 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000007704 transition Effects 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000011521 glass Substances 0.000 abstract 1
- 229910021343 molybdenum disilicide Inorganic materials 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 3
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 238000005649 metathesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001595 flow curve Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001239 high-resolution electron microscopy Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 210000001170 unmyelinated nerve fiber Anatomy 0.000 description 1
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Abstract
一种制备碳化硅颗粒增强二硅化钼基复合材料的原位复合方法,主要通过控制原位复合工艺参数,消除Mo、Si和C三元素粉末之间的低温固一固反应,而利用它们之间的固－液反应原位合成MoSi2－SiC复合粉末,并用二次热压致密该MoSi2－SiC复合粉末,来制备界面洁净、无SiO2玻璃相和Mo5Si3,Mo≤5Si3C≤1等其他过渡相、细小弥散SiC颗粒增强MoSi2两相复合材料。使该复合材料在不降低MoSi2抗高温氧化性的前提下,最大限度地改善MoSi2－SiC复合材料的低温和高温力学性能,并且工艺易于控制、设备简单。
An in-situ composite method for preparing silicon carbide particle-reinforced molybdenum disilicide-based composite materials, mainly by controlling the in-situ composite process parameters, eliminating the low-temperature solid-solid reaction between Mo, Si and C three-element powders, and utilizing their The MoSi 2 -SiC composite powder was synthesized in situ by the solid-liquid reaction between them, and the MoSi 2 -SiC composite powder was densified by secondary hot pressing to prepare a clean interface, no SiO 2 glass phase and Mo 5 Si 3 , Mo ≤ 5 Si 3 C ≤ 1 and other transition phases, fine dispersed SiC particles reinforced MoSi 2 two-phase composites. The composite material can maximize the low-temperature and high-temperature mechanical properties of the MoSi 2 -SiC composite material without reducing the high-temperature oxidation resistance of the MoSi 2 , and the process is easy to control and the equipment is simple.
Description
Technical field:
The invention belongs to the alloy material preparation field, particularly the preparation of intermetallic compound silicon molybdenum thing based composites.
Background technology:
MoSi
2Has fusing point, lower density (6.24g/cm up to 2030～2050 ℃
3), good resistance of oxidation with the thermal conductivity of metal same level and low thermal expansivity, can satisfy the basic demand as high-temperature structural material.The more important thing is that though this compound shows the fragility same with pottery in room temperature, it has the tough-brittle transition behavior, more than ductile-brittle transition temperature, the motion of dislocation and significant reaction activate, and intensity is controlled by plastic deformation.Therefore, under use temperature, will have higher reliability than structural ceramics.In addition, MoSi
2Can or form matrix material with considerable element and compounds aurification, make it keep Thermodynamically stable.Like this, just multiple means and possibility are provided for improving performance.Therefore, MoSi
2Be considered to the high-temperature structural material that has competitive power that occurs after the structural ceramics of Ni, Ti superalloy and use temperature＞1000 of 800～1000 ℃ of use temperatures ℃, getting a good chance of as use temperature is that 1000～1600 ℃ various high-temperature structural materials are used.
But low toughness under the room temperature, high temperature down with the deficiency of ceramic phase specific tenacity, particularly lower creep resistance is hanged down and has been limited MoSi
2Application as high-temperature structural material.Therefore keeping MoSi
2Under the prerequisite that oxidation-resistance does not reduce substantially, how to improve MoSi
2Low-temperature flexibility and hot strength are exploitation MoSi
2The key of high-temperature structural material.Existing work shows that soft or hard second phase can be improved its room temperature and mechanical behavior under high temperature simultaneously.In numerous enhancing bodies, SiC has good chemical stability, high intensity and Young's modulus, and low thermal expansivity, high fusing point is with MoSi
2Good chemical compatibility and physical compatibility are arranged, same MoSi
2-sample has good oxidation-resistance, is considered to strengthen MoSi
2One of the most effective enhancing body.
At present, preparation MoSi
2The original position recombining process of-SiC matrix material has: replacement(metathesis)reaction, reactive plasma deposition, mechanical alloying, XD
TM, burning synthetic induction heating thermal explosion pattern, the auxiliary SHS that reaches of electric field add quasi-hot isostatic pressing simultaneously, and the reaction of direct hot pressing element simple substance mixture and element powders is synthetic synchronously etc.Wherein, replacement(metathesis)reaction (Henager C H Jr, et al.Mater.Sci.Eng.A, 1992, A155:109～114), reactive plasma deposition (Lawrynowicz D E, et al.High-Temperature Ordered IntermetallicsAlloy VI, P923.), mechanical alloying (Jayashankar S, et al.J.Mater.Res., 1428～1441.), XD 1993,8 (6):
TMIn the sample of (Aikin R M Jr, et al.Mater.Sci.Eng.A, 1992, A155:121～133.) these prepared except MoSi
2Outside the SiC two-phase, all there is other transition phases (Mo for example to some extent
5Si
3, Mo
≤ 5Si
3C
≤ 1Deng) and glassy phase, and former three second phase volume fraction can not arbitrarily be regulated and control XD
TMProcess using hot pressing and hot isostatic pressing two procedures are compact formed, and preparation section is many, control is quite complicated; Burning synthetic sample is because the too fast structural constituent of reaction is difficult to control, there is macrosegregation, tissue odds is even, sometimes also reaction is incomplete, the hot-forming back second phase SiC particle is obviously assembled, size big (up to 20 μ m), and equipment complexity (Chrysanthou A, et al.J.Mater.Sci., 1996,31 (16): 4221～4226; Bartlett A H et al.J.Mater.Sci., 1998,33 (6): 1653～1660.); Direct hot pressing element simple substance mixture (Alman D E, et al.Scrip.Metall.Mater., 1994,273～278.) and synthetic synchronously (the Alman D E of the reaction of element powders 31 (3):, et al.Scrip.Metall.Mater., 1993,28 (12): 1525～1530) also have transition phase in Zhi Bei the sample, and the former C fiber does not change into SiC fully, reaction not exclusively, the synthetic synchronously compact formed matrix material of hot isostatic pressing technique that adopts of the reaction of element powders, the equipment complexity, the cost height, the second phase SiC particle size is big, assemble serious, skewness.The MoSi of above-mentioned many prepared
2The mechanical property that the appearance meeting of glassy phase significantly reduces material in the-SiC matrix material is mechanical behavior under high temperature especially, and the second phase SiC particle size is big, assemble remarkable improvement serious, that skewness also is unfavorable for composite materials property, and Mo
5Si
3Can reduce the high temperature oxidation resistance of matrix material etc. the existence of transition phase.
The objective of the invention is to prepare silicon carbide particle reinforced molybdenum silicide based composite material, do not reducing MoSi by control original position recombining process parameter
2Under the prerequisite of high temperature oxidation resistance, improve MoSi to greatest extent
2The low temperature of-SiC matrix material and mechanical behavior under high temperature, and technology is easy to control, equipment is simple.
Summary of the invention:
The present invention is by control original position recombining process parameter, solid eliminate low temperature between Mo, Si and the C element powder solid-reaction, and utilize the solid-liquid reaction original position between them to synthesize MoSi
2-SiC composite powder, and with fine and close this MoSi of secondary hot pressing
2-SiC composite powder prepares interface cleaning, no SiO
2Glassy phase and Mo
5Si
3, Mo
≤ 5Si
3C
≤ 1Wait other transition phases, small and dispersed SiC particle to strengthen MoSi
2Two-phase composite material.The concrete related MoSi of the present invention
2The chemical constitution of-SiC matrix material by volume per-cent is MoSi
2-0%SiC～MoSi
2-100%SiC, the content of element powders calculates by the stoichiometric ratio of corresponding composition proportioning matrix material.The concrete preparation process of matrix material is as follows: be pressed into the green compact sample after element powders is weighed up and mixes by proportioning, green density is 60～75% of a mixed powder theoretical density.The green compact sample carries out reaction in and synthesizes after 400～600 ℃ of vacuum outgass in the mobile pure argon, stove is chilled to room temperature then.Reaction in synthetic technology is: 1410～1470 ℃ of temperature, 120 ℃/min of temperature rise rate, soaking time 0.5～1h.After material fragmentation with reaction in after synthetic becomes 180 μ m～450 μ m powder, carry out hot-forming, 1700～1750 ℃ of temperature, soaking time 1～2h, 30～the 40MPa that exerts pressure is cooled to 400～500 ℃ with the speed of 10～20 ℃/min, naturally cools to room temperature at last.Decompression gradually behind pressurize to 1200 in the process of cooling after hot pressing～1300 ℃.All the time feeding mobile Ar gas in the hot pressing protects.
The invention has the advantages that by control original position recombining process parameter, solid can eliminate low temperature between Mo, Si and the C element powder solid-reaction, effectively utilize the solid-liquid reaction original position between them to synthesize MoSi
2～SiC composite powder by secondary hot pressing, makes the matrix material of the densification of acquisition can guarantee to have only MoSi again
2With the SiC two-phase, interface cleaning, no SiO
2Glassy phase and Mo
5Si
3, Mo
≤ 5Si
3C
≤ 1Wait other transition phases, the second phase SiC particle small and dispersed to be distributed in MoSi
2On the matrix, therefore, this matrix material can be guaranteed do not reducing MoSi
2In the time of high temperature oxidation resistance, can improve the low temperature and the mechanical behavior under high temperature of matrix material to greatest extent.Because the present invention only need control original position recombining process parameter, need not hot isostatic apparatus, so technology easy, be easy to control, equipment is simple.
Description of drawings:
Fig. 1 is MoSi
2The XRD spectral line of-SiC matrix material.
Fig. 2 is MoSiC30 matrix material MoSi
2HREM picture with SiC two-phase phase boundary.
Fig. 3 is the metallographic structure of MoSiC30 matrix material.
Fig. 4 is MoSi
2-SiC matrix material room temperature fracture toughness property is with the variation of SiC volume fraction.
Fig. 5 is single MoSi
2(a) and MoSiC30 (b) compression true stress-strain curve.
Synthetic and the commercial powder MoSi that mixes of hot pressing of original position when Fig. 6 is stress 80MPa
2The creep curve of-30%SiC relatively.
Embodiment
Embodiment: test MoSi
2The chemical constitution of-SiC matrix material by volume per-cent is MoSi
2-30%SIC writes a Chinese character in simplified form into MoSiC30, and the content of element powders is calculated as by the stoichiometric ratio of forming MoSiC30: Mo: Si: C=51.71: 42.90: 5.39wt%.Used starting material are Mo powder, Si powder and Graphite Powder 99, and mean particle size and purity are Mo:8 μ m, 99.0%; Si:7 μ m, 99.0%; C:22, μ m, 99.9%.After element powders weighed up by proportioning, add the different ZrO of an amount of diameter
2Ball and dehydrated alcohol, wet mixing 10h on the roller ball mill.The powder that mixes is pressed into φ 30 * 15mm circle base sample, and pressed density is 70% of a mixed powder theoretical density.Circle base sample carries out original position in the pure argon 99.91% after 500 ℃ of vacuum outgass synthetic, and stove is chilled to room temperature then.Concrete technology is: 1450 ℃ of temperature, 120 ℃/min of temperature rise rate, soaking time 1h.After material fragmentation with reaction in after synthetic becomes 180 μ m powder, carry out hot-formingly, pressed compact is of a size of about φ 50mm * 8mm, 1740 ℃ of temperature, soaking time 2h, 40MPa exerts pressure, speed with 10 ℃/min is cooled to 500 ℃, naturally cools to room temperature at last.Decompression gradually after the pressurize to 1300 ℃ in the process of cooling after hot pressing.All the time feeding mobile Ar gas in the hot pressing protects.
The MoSiC30 matrix material that obtains through above-mentioned technology only contains MoSi
2With the SiC two-phase, do not contain Mo
5Si
3, Mo
≤ 5Si
3C
≤ 1Wait other transition phases, nor have SiO
2Glassy phase, interface cleanness are seen Fig. 1, Fig. 2.The SiC particle size is 3～5 μ m, and evenly tiny, disperse is distributed in MoSi
2On the matrix, see Fig. 3.The porosity of this matrix material is (0.044 ± 0.014) %, can think to reach complete densification.The room temperature fracture toughness property of this material is than single MoSi
2Have clear improvement, see Fig. 4.1000 ℃, 1200 ℃, 1400 ℃ high temperature compressed flow curve is apparently higher than single MoSi
2, its high-temperature stream varying stress, yield strength significantly improve, and see Fig. 5.Its high temperature creep drag is much higher than the MoSi of the prior powder metallurgy prepared that adopts the commercial mixed powder of hot pressing
2-30%SiC matrix material is seen Fig. 6.
Claims (2)
1, a kind of in-situ compounding process for preparing silicon carbide particle reinforced molybdenum silicide based composite material, MoSi
2The chemical constitution of-SiC matrix material by volume per-cent is MoSi
2-0%SiC～MoSi
2-100%SiC, the content of element powders calculates by the stoichiometric ratio of forming this matrix material, it is characterized in that reaction in synthetic technology is: 1410～1470 ℃ of temperature, temperature rise rate 〉=120 ℃/min, soaking time 0.5～1h.After material fragmentation with reaction in after synthetic becomes-40～-80 order powder, carry out hot-forming, 1700～1750 ℃ of temperature, soaking time 1～2h, 30～the 40MPa that exerts pressure is cooled to 400～500 ℃ with the speed of 10～20 ℃/min, naturally cools to room temperature at last.Decompression gradually after 1200～1300 ℃ in the process of cooling after hot pressing.
2, in-situ compounding process as claimed in claim 1, the preparation that it is characterized in that matrix material are to be pressed into the green compact sample after element powders is weighed up and mixes by proportioning, and green density is 60～75% of a mixed powder theoretical density.The green compact sample carries out reaction in and synthesizes after 400～600 ℃ of vacuum outgass in the mobile pure argon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01141978 CN1215185C (en) | 2001-09-26 | 2001-09-26 | In-situ compounding process of preparing silicon carbide particle reinforced molybdenum silicide based composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01141978 CN1215185C (en) | 2001-09-26 | 2001-09-26 | In-situ compounding process of preparing silicon carbide particle reinforced molybdenum silicide based composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1344810A true CN1344810A (en) | 2002-04-17 |
| CN1215185C CN1215185C (en) | 2005-08-17 |
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|---|---|---|---|
| CN 01141978 Expired - Fee Related CN1215185C (en) | 2001-09-26 | 2001-09-26 | In-situ compounding process of preparing silicon carbide particle reinforced molybdenum silicide based composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321092C (en) * | 2006-03-14 | 2007-06-13 | 西北工业大学 | Method for preparing anti-oxidation multiple phase coating of carbon/carbon composite material surface |
| CN101812622B (en) * | 2010-02-08 | 2011-07-20 | 吉林大学 | Ceramic-intermetallic compound composite material containing binder and preparation method thereof |
| CN101386551B (en) * | 2008-10-29 | 2011-12-28 | 陕西科技大学 | Method for preparing carbon/carbon compound material nano silicon carbide-silicon molybdenum composite coating |
| CN104261835A (en) * | 2014-09-19 | 2015-01-07 | 中南大学 | Method for preparing molybdenum disilicide heating element |
| CN105731471A (en) * | 2016-01-28 | 2016-07-06 | 陕西科技大学 | A kind of preparation method of MoSi2-Mo5Si3-SiO2 composite material |
-
2001
- 2001-09-26 CN CN 01141978 patent/CN1215185C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321092C (en) * | 2006-03-14 | 2007-06-13 | 西北工业大学 | Method for preparing anti-oxidation multiple phase coating of carbon/carbon composite material surface |
| CN101386551B (en) * | 2008-10-29 | 2011-12-28 | 陕西科技大学 | Method for preparing carbon/carbon compound material nano silicon carbide-silicon molybdenum composite coating |
| CN101812622B (en) * | 2010-02-08 | 2011-07-20 | 吉林大学 | Ceramic-intermetallic compound composite material containing binder and preparation method thereof |
| CN104261835A (en) * | 2014-09-19 | 2015-01-07 | 中南大学 | Method for preparing molybdenum disilicide heating element |
| CN105731471A (en) * | 2016-01-28 | 2016-07-06 | 陕西科技大学 | A kind of preparation method of MoSi2-Mo5Si3-SiO2 composite material |
| CN105731471B (en) * | 2016-01-28 | 2017-12-05 | 陕西科技大学 | A kind of MoSi2‑Mo5Si3‑SiO2The preparation method of composite |
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| Publication number | Publication date |
|---|---|
| CN1215185C (en) | 2005-08-17 |
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