CN101284734A - Molybdenum disilicide matrix composite and method for making same - Google Patents
Molybdenum disilicide matrix composite and method for making same Download PDFInfo
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- CN101284734A CN101284734A CNA2008100313585A CN200810031358A CN101284734A CN 101284734 A CN101284734 A CN 101284734A CN A2008100313585 A CNA2008100313585 A CN A2008100313585A CN 200810031358 A CN200810031358 A CN 200810031358A CN 101284734 A CN101284734 A CN 101284734A
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Abstract
The invention discloses a high-temperature structural material which takes MoSi2 as the matrix and takes Si3N4 particles and SiC whiskers as the strengthening phases, as well as the preparation process thereof. The preparation process adds the mixed strengthening phases of the Si3N4 particles with the volume fraction being 20 vol% to 50 vol% and the SiC whiskers into the MoSi2 powder so as to be subjected to hot pressing for 30 to 45 minutes at 1,500 DEG C to 1,700 DEG C, thereby obtaining the MoSi2-Si3N4/SiC composite high-temperature structural material. The addition of the mixed strengthening phase inhibits the expansion of the MoSi2 grains during the process of sintering, and the crack deflection of Si3N4 and SiC enables the strength and the toughness of the material to be improved. Si3N4 and SiC can serve a function of grapping grains and inhibiting the glass phase generation of SiO, thereby enabling the anti-creeping performance at the high temperature to be improved. The high-temperature structural material overcomes the defects that the prior molybdenum disilicide material is easy to be broken at the room temperature, and the anticreeping performance at the high temperature is bad, and provides the method for preparing the molybdenum disilicide composite high-temperature structural material.
Description
Technical field
The invention belongs to the high-temperature structural material field, relate generally to a kind of take molybdenum disilicide as matrix, Si
3N
4Particle and SiC whisker are high-temperature structural material and the preparation method of hardening constituent.
Background technology
The development of modern aerospace technology, key parts such as engine are had higher requirement with high-temperature structural material---higher intensity and working temperature (greater than 1200 ℃) and lower density.Widespread use at present the aircraft engine structured material---the maximum operation (service) temperature of nickel base superalloy is 1150 ℃, near 90% of its fusing point, the space that does not promote again almost, though with γ-TiAl is that the Intermatallic Ti-Al compound of representative is applied in aircraft industry as high-temperature structural material, but its maximum operating temperature is 900-1000 ℃, still can't surpass nickel base superalloy, be difficult to satisfy the requirement of following high-performance gas turbine engine.Over past ten years, having more dystectic refractory metal silicide becomes the up-to-date focus of high-temperature structural material with the intermetallic compound area research, as MoSi
2, WSi
2, Mo
5Si
3, Ti
5Si
3And Nb
5Si
3Deng, wherein the Mo-Si series intermetallic compound becomes the high-temperature structural material of future generation of tool DEVELOPMENT PROSPECT with its better comprehensive performance.
MoSi
2With its high melt point (2030 ℃), excellent resistance of oxidation, moderate density and good advantages such as thermal conductivity, become the high-temperature structural material that has development potentiality.Late 1940s, American Studies MoSi
2The high-temperature mechanical property of sill has been inquired into the possibility of making high-temperature structural material with it.The fifties, the research MoSi such as Sweden, Germany and Austria
2Sill is made the heater element of electric furnace.At the beginning of the seventies, the U.S. is with MoSi
2The base coating is used for the protection of gas turbine parts and succeeds.Since the eighties, the famous research institutions such as Marx's Planck institute of the metallic substance institute of U.S. Los Alamos National Laboratories, northeastern Japan university and Germany drop into great amount of manpower and material resources, carry out MoSi
2The research of base high temperature structural material and application thereof makes it become the research focus in high-temperature structural material field once more
MoSi
2Use the problem that needs to solve two aspects as high-temperature structural material: the one, its room temperature toughness and hot strength deficiency, especially high-temperature creep resistance need further to improve; The 2nd, " pest " oxidation can take place in it in the time of 450-550 ℃.
Therefore, from the angle that high-temperature structural material is used, the technology of Strengthening and Toughening be must adopt, its Toughness and elevated temperature strength improved simultaneously; And the raising oxidation resistance, avoid " pest " oxidation to take place.At present, for MoSi
2Strengthening and Toughening carried out a large amount of research work, main method is alloying and Composite.
Alloying is to MoSi
2The fracture toughness of material improves certain limitation, so the research of Composite is significant.Compoundization strengthening phase generally is to select ceramic particle, whisker or fibers such as a kind of oxide compound, carbide, boride, nitride, selects the research work of two kinds of strengthening phases also day by day to increase simultaneously at present.
Summary of the invention
It is good to the purpose of this invention is to provide a kind of fracture toughness property, the bending strength height, and the molybdenum disilicide-base combined high temperature structured material that " pest " oxidation does not take place is mentioned its preparation method.
Molybdenum disilicide-base combined high temperature structural material provided by the invention, its raw material is with MoSi
2Be matrix, add Si
3N
4Particle and SiC whisker be Strengthening and Toughening mutually.Si
3N
4Particle and SiC Whisker Content account for respectively 10～30vol% of material, Si
3N
4The total content of particle and SiC whisker accounts for 20～50vol% of material, MoSi
2Be surplus.Si
3N
4Grain diameter is less than 2 μ m, and the SiC diameter of whiskers is less than 0.5 μ m, and its draw ratio must be greater than 10: 1.
For preparing this combined high temperature structured material, the present invention implements by following steps:
(1) with Si
3N
4Granule content is 10～30vol%, Si
3N
4The total content of particle and SiC whisker was that the molybdenum disilicide mixed-powder of 20～50vol% is put into ball grinder, adds alcohol, with 1: 1～10: 1 ball mill mixings of ratio of grinding media to material 8～24 hours.
(2) with the mixed-powder drying behind the ball milling, cross 200 mesh sieves.
(3) mixed powder after will sieving is put into high purity graphite hot pressing grinding tool, puts into hot-pressed sintering furnace and carries out hot pressed sintering.Concrete technology is: the temperature rise rate with 15～25 ℃/min is heated to 1000～1300 ℃, is heated to 1600～1800 ℃, insulation 30～60min, furnace cooling then with 5～15 ℃ heat-up rate again.Institute's plus-pressure is 20～25MPa during this time.Furnace atmosphere is non-oxidizing atmosphere, i.e. vacuum or inert atmosphere.
Characteristics of the present invention be good with high high-temp stability, intensity is high, with the matrix chemical compatibility good Si
3N
4Particle SiC whisker can play crystal grain thinning as its composite toughening phase, gains in strength and the effect of fracture toughness.Si wherein
3N
4The Si that produces during particle high-temperature
2ON protectiveness film can significantly improve its oxidation resistance.Although Si
3N
4The thermal coefficient of expansion of particle SiC whisker and matrix differs bigger, but its particle diameter and diameter are very little, can overcome this with shortcoming.
As mentioned above, the present invention has made the bending strength height by above-mentioned technology, and fracture toughness property is good, the combined high temperature structured material that resistance toheat is good.The invention is characterized in and add Si
3N
4Particle SiC whisker with crystal grain thinning, strengthens toughness reinforcingly as its composite toughening, finally obtains the molybdenum disilicide-base combined high temperature structural material of function admirable.
Description of drawings
Fig. 1 is heat pressing process figure.
Below by specific embodiment and comparative example marked improvement of the present invention is described.
Embodiment
Embodiment 1 molybdenum disilicide-base combined high temperature structural material, its raw material is with MoSi
2Be matrix, add Si
3N
4Particle and SiC whisker be Strengthening and Toughening mutually, play crystal grain thinning, strengthen toughness reinforcing, and the effect that improves antioxygenic property.Si wherein
3N
4That granule content accounts for material is 10～30vol%, Si
3N
4The total content of particle and SiC whisker accounts for 20～50vol% of material.
The present invention implements by following steps:
(1) with Si
3N
4Granule content is 10～30vol%, Si
3N
4The total content of particle and SiC whisker was that the molybdenum disilicide mixed-powder of 20～50vol% is put into ball grinder, adds alcohol, with 1: 1～10: 1 ball mill mixings of ratio of grinding media to material 8～24 hours.
(2) with the mixed-powder drying behind the ball milling, cross 200 mesh sieves.
(3) mixed powder after will sieving is put into graphite hot pressing grinding tool, puts into hot-pressed sintering furnace and carries out hot pressed sintering.Concrete technology is: the temperature rise rate with 15～25 ℃/min is heated to 1000～1300 ℃, is heated to 1600～1800 ℃, insulation 30～60min, furnace cooling then with 5～15 ℃ heat-up rate again.Institute's plus-pressure is 20～25MPa during this time.
Table 1 is the essential characteristic of embodiment and comparative example.
The essential characteristic of table 1 embodiment and comparative example
| The sample code name | MoSi 2(vol%) | Si 3N 4(vol%) | SiC (vol%) |
| B1 | 100 | 0 | 0 |
| B2 | 80 | 20 | 0 |
| B3 | 80 | 0 | 20 |
| S1 | 70 | 20 | 10 |
| S2 | 70 | 10 | 20 |
| S3 | 60 | 20 | 20 |
| |
50 | 20 | 30 |
| |
50 | 30 | 20 |
| B4 | 40 | 30 | 30 |
Annotate: B represents comparative example, and S represents embodiment.
Prepare B1, S1, S2, S3, S4 after the S5, compares its grain fineness number, ambient temperature mechanical properties and resistance toheat, the result is shown in table 2～4.
The grain size of table 2 embodiment and comparative example relatively
| Sample type | B1 | S1 | S2 | S3 | S4 | S5 |
| Grain size (m) | ＞40 | ＜25 | ＜15 | ＜15 | ＜10 | ＜10 |
As can be seen from Table 2, add Si
3N
4The sample grain size of particle and SiC whisker reduces greatly, and the hardening constituent that adds is more many, and crystal grain is more tiny.Find that by displaing microstructure observing the strengthening phase of disperse is with MoSi
2" cut apart " to become tiny island, the adding of visible tiny strengthening phase has hindered MoSi
2Thereby growing up of crystal grain makes grain refining.Refined crystalline strengthening is important strengthening mechanism, and the crystal grain crystallization also is to improve the flexible important channel simultaneously.
The mechanical performance compare of table 3 embodiment and comparative example
| Sample type | B1 | S1 | S2 | S3 | S4 | S5 |
| Bending strength (MPa) | 252 | 400 | 384 | 389 | 419 | 427 |
| Fracture toughness (MPam 1/2) | 2.9 | 6.06 | 9.72 | 10.48 | 8.1 | 10.01 |
| Vickers hardness (GPa) | 9.56 | 11.35 | 10.89 | 10.24 | 11.83 | 11.82 |
Can find out obviously that from table 3 the sample mechanical property that adds hardening constituent has had significantly raising.Wherein, bending strength is the highest has improved 70%.This is that intensity rises thereupon because dispersion-strengthened promotes the refinement of crystal grain mutually, and simultaneously, the strengthening phase of disperse has played the effect that second-phase dispersion is strengthened.
The adding of hardening constituent improves significantly the toughness of sample.Observation by S1～S5 fracture surface of sample finds that its fracture mode is by pure MoSi
2Transgranular fracture be converted into transgranular fracture with along brilliant fracture coexistence, and the hardening constituent particle that exists is extracted phenomenon; Observe the trend of specimen surface crackle, can find crack deflection and the phenomenon of cutting the hardening constituent particle.This explanation: 1) grain refining has changed fracture mode to a certain extent, has improved toughness; 2) crackle cutting strengthening phase particle reduces energy, and crackle runs into strengthening phase deflection and then prolonged the fracture approach, has reduced crack tip stress; 3) particle is extracted with the bridge linking effect of whisker has great role to consuming energy-to-break, has improved toughness.
The improve effect of hardness of strengthening phase.The abrasion resistance properties of material is determined jointly that by hardness and the fracture toughness of material therefore, this material also has the potentiality as high-abrasive material.
The resistance toheat of table 4 embodiment and comparative example
| The test kind | B1 | S1 | S2 | S3 | S4 | S5 |
| Heat resisting temperature | 1700 |
1800 |
1800 ℃ | 1780 ℃ | 1780 ℃ | 1750 ℃ |
As can be seen from Table 4, the sample that adds hardening constituent all can using more than 1700 ℃, be considered pure MoSi
2Exist more than 1400 ℃ the time intensity characteristic that descends suddenly, and Si
3N
4Do not have this characteristic with SiC, therefore, under the hot conditions, the material that adds hardening constituent has preferably strength advantage.
Prepare B2, B3, behind the B4, with B1, S2, S3, S4, S5 compares, shown in its mechanical property table 5.
The mechanical performance compare of table 5 embodiment and comparative example
| Sample type | Bending strength (MPa) | Fracture toughness (MPam 1/2) | Vickers hardness (GPa) |
| B1 | 252 | 2.9 | 9.56 |
| B2 | 310 | 4.81 | 11.66 |
| B3 | 303 | 5.12 | 10.74 |
| B4 | 205 | 3.71 | 10.23 |
| S2 | 384 | 9.72 | 10.89 |
| S3 | 389 | 10.48 | 10.24 |
| S4 | 419 | 8.1 | 11.83 |
| S5 | 427 | 10.01 | 11.82 |
As can be seen from Table 5, add the B2 of single hardening constituent, B3 sample bending strength and fracture toughness and interpolation Si
3N
4Particle has bigger gap with SiC whisker complex intensifying S2～S5 mutually, and this explanation particle and whisker complex intensifying want to have the effect of obvious raising intensity and toughness.From B4 and S5 more as can be seen, when the content of strengthening phase reached 60vol%, its bending strength and fracture toughness property declined to a great extent.This is because Si
3N
4Thermal coefficient of expansion and MoSi with SiC
2Gap is bigger, when two of hardening constituent reaches a critical point, does not just display because thermal coefficient of expansion does not mate the negative effect that causes.In addition, the fragility impurity that inevitably exists in the hardening constituent has also caused the decline of mechanical property.
Claims (4)
1, a kind of molybdenum disilicide matrix composite is with MoSi
2Be matrix, it is characterized in that: Si
3N
4Particle and SiC Whisker Content account for respectively 10～30vol% of material, Si
3N
4The total content of particle and SiC whisker accounts for 20～50vol% of material, MoSi
2Be surplus.
2, according to the described molybdenum disilicide matrix composite of claim 1, its feature of raw material is: Si
3N
4Grain diameter is less than 2 μ m, and the SiC diameter of whiskers is less than 0.5 μ m, and its draw ratio must be greater than 10: 1.
3, a kind of preparation method of molybdenum disilicide matrix composite according to claim 1 is characterized in that may further comprise the steps:
(1) with Si
3N
4Granule content is 10～40vol%, Si
3N
4The total content of particle and SiC whisker was that the molybdenum disilicide mixed-powder of 20～50vol% is put into ball grinder, adds alcohol, with 1: 1～10: 1 ball mill mixings of ratio of grinding media to material 8～24 hours;
(2) with the mixed-powder drying behind the ball milling, cross 200 mesh sieves;
(3) mixed powder after will sieving is put into graphite hot pressing grinding tool, put into hot-pressed sintering furnace and carry out hot pressed sintering, concrete technology is: the temperature rise rate with 15～25 ℃/min is heated to 1000～1300 ℃, be heated to 1600～1800 ℃ with 5～15 ℃ heat-up rate again, insulation 30～60min, furnace cooling then, institute's plus-pressure is 20～25MPa.
4, according to the preparation method of the described molybdenum disilicide matrix composite of claim 3, it is characterized in that: the atmosphere during hot pressed sintering is vacuum or inert atmosphere.
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|---|---|---|---|
| CNA2008100313585A CN101284734A (en) | 2008-05-22 | 2008-05-22 | Molybdenum disilicide matrix composite and method for making same |
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|---|---|---|---|
| CNA2008100313585A CN101284734A (en) | 2008-05-22 | 2008-05-22 | Molybdenum disilicide matrix composite and method for making same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674919A (en) * | 2012-05-14 | 2012-09-19 | 中国科学院地理科学与资源研究所 | Deodorizing material for compost, as well as preparation method and application thereof |
| CN110183233A (en) * | 2019-06-12 | 2019-08-30 | 万细凤 | A kind of novel Si3N4Enhance MoSi2Based composites and preparation method |
| CN116178023A (en) * | 2023-02-21 | 2023-05-30 | 中钢集团洛阳耐火材料研究院有限公司 | Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material |
-
2008
- 2008-05-22 CN CNA2008100313585A patent/CN101284734A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674919A (en) * | 2012-05-14 | 2012-09-19 | 中国科学院地理科学与资源研究所 | Deodorizing material for compost, as well as preparation method and application thereof |
| CN102674919B (en) * | 2012-05-14 | 2014-01-29 | 中国科学院地理科学与资源研究所 | Deodorizing material for compost, as well as preparation method and application thereof |
| CN110183233A (en) * | 2019-06-12 | 2019-08-30 | 万细凤 | A kind of novel Si3N4Enhance MoSi2Based composites and preparation method |
| CN116178023A (en) * | 2023-02-21 | 2023-05-30 | 中钢集团洛阳耐火材料研究院有限公司 | Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material |
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Open date: 20081015 |