CN101824576B - Zirconium-aluminum-silicon-carbon-silicon carbide composite material and preparation method thereof - Google Patents
Zirconium-aluminum-silicon-carbon-silicon carbide composite material and preparation method thereof Download PDFInfo
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- CN101824576B CN101824576B CN2009100105619A CN200910010561A CN101824576B CN 101824576 B CN101824576 B CN 101824576B CN 2009100105619 A CN2009100105619 A CN 2009100105619A CN 200910010561 A CN200910010561 A CN 200910010561A CN 101824576 B CN101824576 B CN 101824576B
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Abstract
The invention relates to ultrahigh temperature resistant ceramic and preparation technology thereof, in particular provides a zirconium-aluminum-silicon-carbon-silicon carbide composite material and a method for preparing the zirconium-aluminum-silicon-carbon-silicon carbide composite material by in-situ reactive hot pressing. Zr powder, Al powder, Si powder and C powder in a certain stoichiometric ratio are used as raw materials; the raw materials are mixed for 5 to 50 hours by using a physical and mechanical method and are cold-pressed into cakes under the pressure of 5 to 20MPa; and the cakes are filled into a graphite mold and are heated to 1,600 to 2,400 DEG C in a hot pressing furnace into which inert gas serving as protective gas is introduced (or in vacuum) for in-situ hot pressing reaction for 0.1 to 4 hours under the hot pressing pressure of 20 to 40MPa. In the invention, the zirconium-aluminum-silicon-carbon-silicon carbide composite material with high hardness, high strength, high toughness, high ultrahigh-temperature resistance and the like can be synthesized at a relatively low temperature in a short time; and the material obtained by the method can be used at the ultrahigh temperature of above 1,600 DEG C.
Description
Technical field
The present invention relates to superhigh temperature resistant pottery and technology of preparing thereof, a kind of zirconium-aluminum-silicon-carbon-silit (Zr is provided especially
2[Al (Si)]
4C
5The hot pressing of-SiC) matrix material, and reaction in prepares the method for zirconium-aluminum-silicon-carbon-composite material of silicon carbide.
Background technology
Zirconium-aluminum-silicon-carbon (Zr
2[Al (Si)]
4C
5) pottery is novel superhigh temperature resistant, oxidation resistant structured material (J.SolidState Chem. (solid state chemistry magazine) 180 (2007) 1809; J.Am.Ceram.Soc. (American Ceramic Society's will) (2009)).It combines high-modulus, high firmness, anti-oxidant, corrosion-resistant, high conductivity, stronger advantages such as destruction tolerance.All have wide practical use at high-technology fields such as Aeronautics and Astronautics, nuclear industry and ultrahigh-temperature structural parts.But as a kind of structured material, its hardness, intensity and toughness are on the low side, have limited its widespread use.Introducing hard ceramic particles is one of effective ways that improve ceramics strength, and for example, human in-situ hot pressings such as Wan generate silit enhancing titanium Si-C composite material and improved titanium silicon-carbon (Ti significantly
3SiC
2) ceramic hardness, intensity and friction resistant polishing machine (Ceram.Inter. (ceramic international magazine) 32 (2006) 883).Humans such as Chen add alumina particle and strengthen titanium aluminium carbon (Ti
3AlC
2) ceramic hardness, intensity, toughness and friction resistant polishing machine (Scripta Mater. (material wall bulletin) 50 (2004) 897).But, also do not have Zr at present
2[Al (Si)]
4C
5The report of reinforcement aspect.
Summary of the invention
The object of the present invention is to provide that a kind of mechanical property is good, purity is high, simple to operate, easy control of process conditions, zirconium-aluminum-silicon-carbon-silit (Zr that cost is low
2[Al (Si)]
4C
5-SiC) matrix material and preparation method thereof can solve zirconium-aluminum-silicon-carbon ceramic hardness, intensity and toughness problem of lower.
Technical scheme of the present invention is following:
A kind of zirconium-aluminum-silicon-carbon-composite material of silicon carbide is made up of silicon-carbide particle wild phase and zirconium-aluminum-silicon-carbon matrix, and silicon-carbide particle wild phase disperse equably is distributed in the zirconium-aluminum-silicon-carbon matrix, and wherein the percent by volume of silicon-carbide particle wild phase is 5～30%.
Plant the method for zirconium-aluminum-silicon-carbon-composite material of silicon carbide, concrete steps are following:
1) raw material is formed and composition range:
As raw material, wherein the mol ratio of Zr: Al: Si: C is 2: (3～4): (0.5～3.5): (4～8) with simple substance Zr powder, Al powder, Si powder and C powder.
2) preparation technology:
Raw material mixed 5～50 hours through physical mechanical method, was cold-pressed into pie under the pressure normal temperature with 5～20MPa, colded pressing 1～30 minute time, and in the graphite jig of packing into, (or under the vacuum, vacuum tightness is higher than 10 as protection gas being connected with rare gas element (like argon gas)
-1Pa) (be preferably 5～30 ℃/min) temperature rise rate and rise to 0.1～4 hour (being preferably 0.5～2 hour) of 1600 ℃～2400 ℃ in-situ hot pressings reactions, hot pressing pressure is 20～40MPa (being preferably 30MPa) with 2～50 ℃/min in the hot pressing furnace.
Among the present invention, the granularity of Zr powder, Al powder, Si powder and C powder is 200～400 orders; Zirconium-aluminum-silicon-carbon-composite material of silicon carbide the size that adopts the inventive method acquisition is at Φ (25～100) mm * (2～50) mm; Said physical mechanical method is employed in ball milling in the alcohol medium.
Characteristics of the present invention are:
1. the present invention selects for use raw material simple, is respectively Zr powder, Al powder, Si powder and C powder.
2. the present invention is through reaction in hot pressing, and sintering and densification are carried out simultaneously, obtains fine and close zirconium-aluminum-silicon-carbon-silit two-phase composite material.
3. the matrix material that adopts the inventive method to obtain at room temperature has higher hardness, intensity and toughness than single zirconium-aluminum-silicon-carbon pottery, and can under greater than 1600 ℃ ultrahigh-temperature, use.
Description of drawings
Fig. 1 is Zr
3[Al (Si)]
4C
6The X-ray diffracting spectrum of-20vol.%SiC matrix material.
Fig. 2 is Zr
3[Al (Si)]
4C
6The X-ray diffracting spectrum of-30vol.%SiC matrix material.
Fig. 3 is Zr
3[Al (Si)]
4C
6The polish etch surface of-30vol.%SiC matrix material and the stereoscan photograph of crimped section; (a) be the polish etch surface; (b) crimped section.
Fig. 4 is Zr
3[Al (Si)]
4C
6And Zr
3[Al (Si)]
4C
6The contrast of-30vol.%SiC matrix material high temperature rigid.
Embodiment
Through embodiment the present invention is detailed below.
Embodiment 1.
It is Zr powder 100.0 grams, Al powder 53.5 grams, Si powder 19.5 grams and C powder 35.6 grams about 350 orders that raw material adopts granularity; Ball milling is 10 hours in the alcohol medium; Under the pressure of 10MPa, be cold-pressed into pie, cold pressing 20 minutes time, in the graphite jig of packing into; Temperature rise rate with 5 ℃/min in the hot pressing furnace that is connected with rare gas element (argon gas) conduct protection gas rises to 1850 ℃ of reaction in hot pressing 1 hour, and hot pressing pressure is 40MPa.That obtain is Zr
3[Al (Si)]
4C
6-10vol.%SiC matrix material, silicon-carbide particle wild phase disperse equably are distributed in the zirconium-aluminum-silicon-carbon matrix, and zirconium-aluminum-silicon-carbon-composite material of silicon carbide size is at Φ 50mm * 24mm.
Embodiment 2.
It is Zr powder 100.0 grams, Al powder 54.3 grams, Si powder 30.2 grams and C powder 42.6 grams about 300 orders that raw material adopts granularity; Ball milling is 10 hours in the alcohol medium; Under the pressure of 15MPa, be cold-pressed into pie, cold pressing 10 minutes time, in the graphite jig of packing into; Temperature rise rate with 10 ℃/min in the hot pressing furnace that is connected with rare gas element (argon gas) conduct protection gas rises to 2000 ℃ of reaction in hot pressing 1 hour, and hot pressing pressure is 30MPa.That obtain is Zr
3[Al (Si)]
4C
6-20vol.%SiC matrix material, silicon-carbide particle wild phase disperse equably are distributed in the zirconium-aluminum-silicon-carbon matrix, and zirconium-aluminum-silicon-carbon-composite material of silicon carbide size is at Φ 60mm * 18.8mm.Corresponding X-ray diffracting spectrum is listed on the accompanying drawing 1.
Embodiment 3.
It is Zr powder 100.0 grams, Al powder 52.1 grams, Si powder 50.3 grams and C powder 47.8 grams about 400 orders that raw material adopts granularity; Ball milling is 15 hours in the alcohol medium, under the pressure of 20MPa, is cold-pressed into pie, colds pressing 5 minutes time; Pack in the graphite jig, (vacuum tightness is 10 under vacuum
-2Pa) temperature rise rate with 15 ℃/min in the hot pressing furnace rises to 1900 ℃ of reaction in hot pressing 0.5 hour, and hot pressing pressure is 35MPa.That obtain is Zr
3[Al (Si)]
4C
6-30vol.%SiC matrix material, silicon-carbide particle wild phase disperse equably are distributed in the zirconium-aluminum-silicon-carbon matrix, and zirconium-aluminum-silicon-carbon-composite material of silicon carbide size is at Φ 70mm * 15.8mm.Corresponding X-ray diffracting spectrum, the grain morphology stereoscan photograph is listed in respectively on the accompanying drawing 2-3.The kinetic Young's modulus of this matrix material and shearing modulus are respectively 386 and 163GPa; Vickers' hardness is 16.4GPa; Bending strength is 353MPa; Fracture toughness property is 6.62MPam
1/2From the relation curve (accompanying drawing 4) of kinetic Young's modulus and temperature, it can also be seen that this matrix material still can keep very high high temperature rigid (323GPa) at 1600 ℃.
Comparative example
The single-phase Zr that adopted the prepared identical with embodiment 3
2[Al (Si)]
4C
5Vickers' hardness be 11.7GPa; Kinetic Young's modulus and shearing modulus are respectively 361 and 153GPa; Bending strength is 302MPa, and fracture toughness is 3.88MPam
1/2From the relation curve (accompanying drawing 4) of kinetic Young's modulus and temperature, in whole Range of measuring temp, Young's modulus all is lower than Zr
3[Al (Si)]
4C
6-30vol.%SiC matrix material.This shows single-phase Zr
2[Al (Si)]
4C
5Each item mechanical performance index all far below Zr
2[Al (Si)]
4C
5-SiC matrix material.
Claims (6)
1. zirconium-aluminum-silicon-carbon-composite material of silicon carbide, it is characterized in that: be made up of silicon-carbide particle wild phase and zirconium-aluminum-silicon-carbon matrix, wherein the percent by volume of silicon-carbide particle wild phase is 5～30%; This matrix material prepares through following method:
With simple substance Zr powder, Al powder, Si powder and C powder as raw material; Wherein the mol ratio of Zr: Al: Si: C is 2: (3～4): (0.5～3.5): (4～8); Raw material powder was mixed 5～50 hours through physical mechanical method; The coldmoulding in the graphite jig of packing into, the pressure that applies is 5～20MPa, colds pressing 1～30 minute time; Sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere or vacuum, temperature rise rate are 2～50 ℃/minute, and sintering temperature is that 1600～2400 ℃, sintering time are that 0.1～4 hour, sintering pressure are 20～40MPa.
2. according to the preparation method of the described zirconium-aluminum-silicon-carbon-composite material of silicon carbide of claim 1; It is characterized in that: with simple substance Zr powder, Al powder, Si powder and C powder as raw material; Wherein the mol ratio of Zr: Al: Si: C is 2: (3～4): (0.5～3.5): (4～8), and raw material powder was mixed 5～50 hours through physical mechanical method, coldmoulding in the graphite jig of packing into; The pressure that applies is 5～20MPa, colds pressing 1～30 minute time; Sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere or vacuum, temperature rise rate are 2～50 ℃/minute, and sintering temperature is that 1600～2400 ℃, sintering time are that 0.1～4 hour, sintering pressure are 20～40MPa; The volume percent of said silicon-carbide particle wild phase is 5～30%.
3. according to the preparation method of the described zirconium-aluminum-silicon-carbon-composite material of silicon carbide of claim 2, it is characterized in that: the Zr powder of said adding, Al powder, Si powder and C powder degree scope are 200～400 orders.
4. according to the preparation method of the described zirconium-aluminum-silicon-carbon-composite material of silicon carbide of claim 2, it is characterized in that: said agglomerating mode is hot pressed sintering or HIP sintering.
5. according to the preparation method of the described zirconium-aluminum-silicon-carbon-composite material of silicon carbide of claim 2, it is characterized in that: said rare gas element is argon gas, helium or neon.
6. according to the preparation method of the described zirconium-aluminum-silicon-carbon-composite material of silicon carbide of claim 2, it is characterized in that: said physical mechanical method is employed in ball milling in the alcohol medium.
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| CN102718488A (en) * | 2011-05-27 | 2012-10-10 | 中国科学院金属研究所 | Hf-Al-Si-C-silicon carbide composite material and preparation method thereof |
| CN102745992B (en) * | 2012-07-25 | 2014-04-09 | 南京工业大学 | (ZrB2+ZrC)/(Zr3[Al(Si)]4C6 complex-phase ceramic material and preparation method thereof |
| CN102745993B (en) * | 2012-07-25 | 2014-02-26 | 南京工业大学 | Zr2[Al(Si)]4C5-ZrB2-SiC composite material and preparation method thereof |
| CN103451463B (en) * | 2013-08-27 | 2015-11-25 | 朱育盼 | A kind of Mg 2si strengthens the preparation method of Mg alloy composite materials |
| CN104060173B (en) * | 2014-07-02 | 2016-08-24 | 北京交通大学 | A kind of Ti3alC2strengthen Fe based composites and in-situ heat extruding production thereof |
| CN109608200B (en) * | 2018-12-10 | 2021-06-29 | 武汉科技大学 | Carbon-silicon-aluminum-bonded SiC refractory material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4915903A (en) * | 1984-10-19 | 1990-04-10 | Martin Marietta Corporation | Process for forming composites having an intermetallic containing matrix |
| CN101343183A (en) * | 2007-07-13 | 2009-01-14 | 中国科学院金属研究所 | Zirconium titanium carbide particle reinforced silicon aluminum titanium carbide zirconium based composite material and preparation thereof |
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2009
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4915903A (en) * | 1984-10-19 | 1990-04-10 | Martin Marietta Corporation | Process for forming composites having an intermetallic containing matrix |
| CN101343183A (en) * | 2007-07-13 | 2009-01-14 | 中国科学院金属研究所 | Zirconium titanium carbide particle reinforced silicon aluminum titanium carbide zirconium based composite material and preparation thereof |
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