CN1283825C - Preparation process for integrated enhancing hardness and breaking toughness of omposite material with MoSi2 base by addiing multi-element - Google Patents
Preparation process for integrated enhancing hardness and breaking toughness of omposite material with MoSi2 base by addiing multi-element Download PDFInfo
- Publication number
- CN1283825C CN1283825C CN 200410022942 CN200410022942A CN1283825C CN 1283825 C CN1283825 C CN 1283825C CN 200410022942 CN200410022942 CN 200410022942 CN 200410022942 A CN200410022942 A CN 200410022942A CN 1283825 C CN1283825 C CN 1283825C
- Authority
- CN
- China
- Prior art keywords
- mosi2
- fracture toughness
- mosi
- fracture
- hardness
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Ceramic Products (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention discloses a preparing method for comprehensively improving the hardness and the fracture toughness of MoSi2-based composite material by adding various elements, which is characterized in that various elements such as W, La, etc. are simultaneously introduced in the technological process that MoSi2 is mechanically alloyed or is synthesized at high temperature by a self-propagating method, solid solution and second phase particles dispersively distributed are generated in situ, and a tissue structure whose average grain size is smaller than 1 mu m is obtained, the mode of combining fine grain brittle fracture with coarse grain transgranular fracture of pure MoSi2 is converted into a transgranular fracture mode by strengthening and toughening mechanisms such as a mechanism for strengthening particles and solid solution, a mechanism for toughening fine grains, a crack deflecting and bridging mechanism, etc. The method solves the problem that the increased range of the room-temperature fracture toughness of the MoSi2-base composite material is limited. Thus, the hardness and the fracture toughness of MoSi2 are synthetically increased, particularly, the value of fracture toughness is greatly increased, and the value is increased by 89.36 to 178.26%. The present invention can also be applied to the preparation of other intermetallic compounds and ceramic material.
Description
Technical field
The present invention relates to a kind of MoSi
2The preparation method of (molybdenum disilicide) based composites, the multiple element of particularly a kind of interpolation comprehensively improves MoSi
2The preparation method of based composites hardness and fracture toughness property.
Background technology
At present, because MoSi
2Its distinctive C of Intermetallic compound
11bType crystal structure has caused the low inherent defect of room temperature fracture toughness property.Existing method is at MoSi
2Add single toughness element such as Nb etc. in the matrix, or introduce high-melting-point, the high elastic coefficient second phase particle or fiber such as SiC, ZrO
2, C, TiC, Al
2O
3, WSi
2, Mo
5Si
3Deng, improve the flexible purpose to reach, but aforesaid method is to MoSi
2The raising effect of room temperature fracture toughness property is limited, and general fracture toughness property value only is 6～8.5MPam
1/2Disclosed among the Chinese patent publication number CN1448461A and utilized doped with rare-earth oxide to carry out modification, improved fracture toughness property of molybdenum silicide base composite exothermic body and preparation method thereof.But this preparation method's technological process is still complicated, and will select the higher aluminosilicate of quality as the binding agent in moulding, the drying process, thereby has increased the cost in the preparation process greatly.
Summary of the invention
At above-mentioned situation, the object of the present invention is to provide and a kind ofly comprehensively improve MoSi by adding multiple element
2The preparation method that based composites hardness and fracture toughness property and technology are simple, cost does not increase.
To achieve these goals, the multiple element of a kind of interpolation comprehensively improves MoSi
2The preparation method of (molybdenum disilicide) based composites hardness and fracture toughness property is at MoSi
2The granularity of introducing at least two kinds of polynary additive W and La element in mechanical alloying or the self-propagating high-temperature building-up process simultaneously is 200 orders～400 orders, and the molar fraction of W element is 10～25%, and the weight ratio of La element is 0.1～2.0%, and original position generates sosoloid WSi
2The second particle La mutually that (two tungsten silicides) and disperse distribute
2O
3(lanthanum sesquioxide), and the adopting process flow process is: Mo powder+Si powder+polynary additive → mixing → mechanical alloying or self-propagating high-temperature synthesize → sieve → die mould → sintering or hot pressing.
Above-mentioned technical process medium-pressure type pressure is that 100～500Mpa, dwell time are 1～2 minute; Sintering temperature is 1600～1800 ℃, and soaking time is 1～2 hour; Hot pressing temperature is 1500～1700 ℃, and soaking time is 1～2 hour, exerts pressure to be 〉=20Mpa.
The present invention is owing to adopt the multiple element of interpolation to introduce two or more highly malleablized phase simultaneously, original position generates sosoloid and disperse second particle mutually that distributes, obtain the weave construction of average grain size＜1 μ m, utilize highly malleablized mechanism such as particle strengthening and solution strengthening, thin brilliant malleableize, crack deflection and bridge joint, with pure MoSi
2Thin brilliantly be converted into the scheme of transgranular fracture form along brilliant fracture and coarse-grain transgranular fracture array configuration, solved MoSi
2The limited difficult problem of based composites room temperature fracture toughness property increase rate, thus MoSi comprehensively improved
2Hardness and fracture toughness property, particularly improved the fracture toughness value significantly, make this value be up to 18MPam
1/2Can be suitable for the use temperature environment is 1000～1600 ℃.The present invention also can be applicable among the preparation of other intermetallic compound and stupalith.
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the typical grain structure structure iron that adopts the product of the present invention's preparation.
Fig. 2 is pure MoSi
2The organization chart of product.
Fig. 3 is the typical fracture apperance structure iron that adopts the product of the present invention's preparation.
Embodiment
Mechanism of the present invention: synthetic by polynary additive W, La element and Mo powder+Si powder alloying or self-propagating high-temperature under the high-energy ball milling effect, original position generate sosoloid and disperse second mutually, in the sinter molding process, obtain the weave construction of average grain size＜1 μ m.
Fig. 1 represents the product that adopts the present invention to prepare, can obtain the typical grain structure structure iron of average grain size＜1 μ m, and second is evenly distributed mutually.Fig. 2 is pure MoSi
2The organization chart of product.Fig. 3 represents to adopt the typical fracture apperance structure iron that can obtain the transgranular fracture form behind the present invention.
Adopting process flow process of the present invention is: in Mo powder and Si powder, add simultaneously under two kinds of element powders → mixing of W and La → high energy ball mill ball action alloying or self-propagating high-temperature synthetic → original position generates sosoloid WSi
2The second particle La mutually that distributes with disperse
2O
3→ sieve → die mould → sintering or hot pressing.
Embodiment 1: choose in 400 purpose Mo powder and the Si powder and add 200 purpose 10mol.%W simultaneously and two kinds of element powders of 0.2wt.%La mix, alloying mode under the ball action of high energy ball mill makes its original position generate sosoloid WSi
2The second particle La mutually that distributes with disperse
2O
3, 200 orders that sieve then, with synthetic composite powder die mould, pressure is 100Mpa, pressurize 2 minutes; Pressed compact is inserted in the sintering oven under hydrogen atmosphere in 1600 ℃ of sintering, be incubated 2 hours, furnace cooling gets product, and product is the silver gray solid.
Embodiment 2: choose in 200 purpose Mo powder and the Si powder and add 400 purpose 15mol.%W simultaneously and two kinds of element powders of 0.5wt.%La mix; in the self-propagating high-temperature device, utilize the tungsten filament igniting under the vacuum; cause self-propagating reaction to take place; the synthetic composite powder is carried out hot pressing, and hot pressing temperature is 1700 ℃, and soaking time is 1 hour; exert pressure and be 25Mpa; all the time feed the mobile hydrogen shield in the hot pressing, furnace cooling gets product, and product is the silver gray solid.
Embodiment 3: choose in 300 purpose Mo powder and the Si powder and add 300 purpose 20mol.%W simultaneously and two kinds of element powders of 2.0wt.%La mix, in the self-propagating high-temperature device, utilize the tungsten filament igniting under the vacuum, cause self-propagating reaction to take place, with synthetic composite powder die mould, pressure is 500Mpa, pressurize 1 minute; Pressed compact is inserted in the sintering oven under hydrogen atmosphere in 1800 ℃ of sintering, be incubated 1 hour, furnace cooling gets product, and product is the silver gray solid.
Embodiment 4: choose in 300 purpose Mo powder and the Si powder and add 300 purpose 25mol.%W simultaneously and two kinds of element powders of 0.8wt.%La mix; in the self-propagating high-temperature device, utilize the tungsten filament igniting under the vacuum; cause self-propagating reaction to take place; the synthetic composite powder is carried out hot pressing, and hot pressing temperature is 1500 ℃, and soaking time is 2 hours; exert pressure and be 20Mpa; all the time feed the mobile hydrogen shield in the hot pressing, furnace cooling gets product, and product is the silver gray solid.
MoSi in above-mentioned technological process
2Original position has generated WSi in the matrix
2The rare earth oxide second of solid solution phase and disperse distribution is particle La mutually
2O
3, MoSi then
2The over-all properties of based composites hardness and fracture toughness property significantly improves and improves, and sees Table 1, and the hardness of material has improved 2.54～4.0HRA, fracture toughness property and then improved 89.36～178.26%, and maximum reaches 18.56MPam
1/2, product is suitable for temperature fully 1000～1600 ℃ environmental applications.
Table 1 is MoSi
2And rare earth-WSi
2/ MoSi
2Performance of composites
| Material | Density ρ/g·cm -3 | Hardness HRA | Fracture toughness K IC/MPa·m 1/2 |
| MoSi 2Embodiment 1 embodiment 2 embodiment 3 embodiment 4 | 5.99 7.77 7.79 7.75 7.89 | 81.12 83.66 84.01 84.34 85.12 | 6.67 15.09 16.23 12.63 18.56 |
It is worthy of note: the present invention also can be applicable among the preparation of other intermetallic compound and stupalith.
Claims (3)
1, the multiple element of a kind of interpolation comprehensively improves MoSi
2The preparation method of based composites hardness and fracture toughness property is at MoSi
2Introduce W and two kinds of elements of La at least in mechanical alloying or the self-propagating high-temperature building-up process simultaneously, original position generates sosoloid WSi
2The second particle La mutually that distributes with disperse
2O
3, and the adopting process flow process is: add two kinds of element powders → mixing → mechanical alloyings of W and La or self-propagating high-temperature in Mo powder and the Si powder simultaneously and synthesize → sieve → die mould → sintering or hot pressing; The granularity of described W and La powder is 200 orders～400 orders, and the molar fraction of W element is 10～25%, and the weight ratio of La element is 0.1～2.0%.
2, the multiple element of a kind of interpolation according to claim 1 comprehensively improves MoSi
2The preparation method of based composites hardness and fracture toughness property, described die mould pressure is that 100～500Mpa, dwell time are 1～2 minute.
3, the multiple element of a kind of interpolation according to claim 1 comprehensively improves MoSi
2The preparation method of based composites hardness and fracture toughness property, described sintering temperature are 1600～1800 ℃, and soaking time is 1～2 hour; Described hot pressing temperature is 1500～1700 ℃, and soaking time is 1～2 hour, exerts pressure 〉=20Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410022942 CN1283825C (en) | 2004-03-02 | 2004-03-02 | Preparation process for integrated enhancing hardness and breaking toughness of omposite material with MoSi2 base by addiing multi-element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410022942 CN1283825C (en) | 2004-03-02 | 2004-03-02 | Preparation process for integrated enhancing hardness and breaking toughness of omposite material with MoSi2 base by addiing multi-element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1560303A CN1560303A (en) | 2005-01-05 |
| CN1283825C true CN1283825C (en) | 2006-11-08 |
Family
ID=34441026
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410022942 Expired - Fee Related CN1283825C (en) | 2004-03-02 | 2004-03-02 | Preparation process for integrated enhancing hardness and breaking toughness of omposite material with MoSi2 base by addiing multi-element |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1283825C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441345C (en) * | 2007-01-04 | 2008-12-10 | 北京科技大学 | Method of preparing tunsten and aluminium-doped molybdenum silicide powder |
| CN101255056B (en) * | 2008-04-03 | 2010-12-08 | 燕山大学 | Superplastic nano AlN ceramic material and preparation method thereof |
| CN101812622B (en) * | 2010-02-08 | 2011-07-20 | 吉林大学 | Ceramic-intermetallic compound composite material containing binder and preparation method thereof |
| CN103231058B (en) * | 2013-05-13 | 2015-03-18 | 中原工学院 | Preparation method of high temperature silicon molybdenum rods |
| CN104962857B (en) * | 2015-07-24 | 2017-09-29 | 厦门理工学院 | A kind of coating molybdenum heater that can be used in an atmosphere and preparation method thereof |
| CN112374894B (en) * | 2020-04-11 | 2022-06-10 | 湖北中烟工业有限责任公司 | Metal silicide based heating material and preparation method thereof |
| CN114591088B (en) * | 2020-12-07 | 2022-12-16 | 中南大学 | TiC reinforcing MoSi 2 Base composite material and preparation method thereof |
-
2004
- 2004-03-02 CN CN 200410022942 patent/CN1283825C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1560303A (en) | 2005-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101798217B (en) | Composite rare earth-stabilized zirconia-based multielement nano/micro composite ceramic tool and die material and preparation method thereof | |
| CN109608203B (en) | High-entropy disilicide and preparation method thereof | |
| JP5302965B2 (en) | Hard powder, method for producing hard powder, and sintered hard alloy | |
| CN102161594B (en) | SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof | |
| CN109072360A (en) | The adhesive composition of four tungsten borides and that grinding method | |
| CN1283825C (en) | Preparation process for integrated enhancing hardness and breaking toughness of omposite material with MoSi2 base by addiing multi-element | |
| CN111533560A (en) | Boron carbide-based composite ceramic material and preparation method thereof | |
| CN108611539B (en) | A kind of complex intensifying hard alloy and preparation method thereof | |
| CN113373363B (en) | Refractory high-entropy composite material and preparation method thereof | |
| CN110655404A (en) | Titanium silicon carbide based composite ceramic material and preparation process thereof | |
| CN1789463A (en) | Method for improving property of TiAI intermetallic compound based composite material | |
| CN111943702B (en) | In-situ synthesized beta-SIALON whisker toughened tungsten carbide composite material and preparation method and application thereof | |
| CN101343183A (en) | Zirconium titanium carbide particle reinforced silicon aluminum titanium carbide zirconium based composite material and preparation thereof | |
| CN101417879B (en) | Nb4AlC3 block ceramic synthesized by hot pressing at in-situ reaction and preparation method thereof | |
| CN102249682B (en) | Titanium carbide ceramic composite material reinforced with ferrum and aluminium intermetallic compound and preparation method thereof | |
| CN114538930A (en) | Crack self-healing gradient functional ceramic cutter material and preparation method thereof | |
| US5773733A (en) | Alumina-aluminum nitride-nickel composites | |
| CN110438384B (en) | Iron-nickel-based ultrafine-grained hard alloy and preparation method thereof | |
| CN100422113C (en) | Silicon-aluminium titanium carbonate solid-solution material and preparing method | |
| CN101701305B (en) | TiAl intermetallic compound composite material and preparation method thereof | |
| CN100422109C (en) | Aluminium oxide silicon titanium carbonate/aluminium oxide lamina composite material and preparing method | |
| CN101092301A (en) | Composite material of aluminum titanium carbide / titanium diboride, and preparation method | |
| CN116730723B (en) | Al (aluminum) alloy 3 BC ceramic material and preparation method and application thereof | |
| CN105543535A (en) | Al4SiC4 and Cr cooperative reinforcement net-shaped/globular copper material and preparation method | |
| CN1053173C (en) | Complex-phase ceramic cutting-tool material and processing technology thereof |
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: 20061108 |