CN105908043A - Mo-ZrB2-SiC-AlN composite material and preparation method thereof - Google Patents
Mo-ZrB2-SiC-AlN composite material and preparation method thereof Download PDFInfo
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- CN105908043A CN105908043A CN201610273312.9A CN201610273312A CN105908043A CN 105908043 A CN105908043 A CN 105908043A CN 201610273312 A CN201610273312 A CN 201610273312A CN 105908043 A CN105908043 A CN 105908043A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
Abstract
The invention provides a Mo-ZrB2-SiC-AlN composite material. The Mo-ZrB2-SiC-AlN composite material is composed of, by mass, 3%-25% of zirconium boride, 2%-10% of silicon carbide, 2%-8% of aluminum nitride and the balance molybdenum and inevitable impurities. The invention further provides a preparation method of the Mo-ZrB2-SiC-AlN composite material. The preparation method comprises the following steps that 1, zirconium boride powder, silicon carbide powder, aluminum nitride powder and molybdenum powder are uniformly mixed through a wet ball grinding method and are crushed after being subjected to vacuum drying, so that mixed powder is obtained; and 2, the mixed powder is placed in a discharge plasma sintering furnace to be subjected to discharge plasma sintering, and thus the Mo-ZrB2-SiC-AlN composite material is obtained. According to the Mo-ZrB2-SiC-AlN composite material and the preparation method thereof, energy consumption is low, the cycle is short, the prepared Mo-ZrB2-SiC-AlN composite material is fine and uniform in microstructure, and the ideal microstructure enables the Mo-ZrB2-SiC-AlN composite material to have the unique performances of being low in density, high in strength and toughness, resistant to oxidation and the like.
Description
Technical field
The invention belongs to technical field of composite preparation, be specifically related to a kind of Mo-ZrB2-SiC-AlN
Composite and preparation method thereof.
Background technology
Along with the development of aeronautical and space technology, develop the hyperthermal material gesture substituting existing nickel based super alloy
Must go.Elevated temperature strength and antioxygenic property that hyperthermal material is had allow them to be competent in
Superhigh temperature extreme environment, including supersonic vehicle, air reenters and rocket propulsion system.Superhigh temperature
Material plays the most important effect in Aero-Space and national defense industry.Refractory metal molybdenum and
Alloy has fusing point thermal shock resistance high, preferable and Room-Temperature Fracture Toughness, it is possible to as superhigh temperature
The candidate material used under environment, but they are easy to oxidation in atmosphere, and high temperature creep property is poor
And be restricted；It addition, molybdenum and alloy thereof have the highest density, during this application in terms of space flight
Totally unfavorable.Boride, carbide and nitride ceramics composite have high-melting-point, low-density,
At high temperature can keep good elevated temperature strength, excellent antioxygenic property, excellent heat stability and
Chemical stability has good future as superhigh temperature structural material.But, ceramic material has one
Total feature is exactly that toughness limits its use not, and it is strong that superhigh temperature ceramics also shows low high temperature
Degree, this inferior performance owing to granule reunion, uneven, granule boundary is the purest, do not have
Prepare the dense ceramic material with intact microstructure.It addition, boride, carbide and nitridation
Thing ceramic material is because they the lowest caking powers limit their use.The chemistry of themselves
Even if the character of key makes them also be difficult to obtain fine and close material at 2000 DEG C of sintering carried out above.?
So it is sintered causing the abnormal growth of crystal grain at a temperature of height, is easily formed fine fisssure simultaneously
Stricture of vagina, this is very harmful to the mechanical property of material.Therefore, send out to meet space flight and aviation technology
Exhibition and the needs of national defense construction, it is necessary to develop new hyperthermal material.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that a kind of
Mo-ZrB2-SiC-AlN composite.The microstructure fine uniform of this composite, density is
7.9g/cm3～8.6g/cm3, solid density is 98.7%～99.5%, and Room-Temperature Fracture Toughness is
7MPa·m1/2～13MPa m1/2, the tensile strength under the conditions of 1400 DEG C is 329MPa～523MPa,
Aoxidizing material unaccounted-for (MUF) after 100h in 1400 DEG C of air ambients is 12 μm～37 μm, have low-density,
The features such as high intensity, high tenacity and antioxidation, it is possible to use in 1400 DEG C of air.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of
Mo-ZrB2-SiC-AlN composite, it is characterised in that be grouped into by the one-tenth of following mass percent:
Zirconium boride 3%～25%, carborundum 2%～10%, aluminium nitride 2%～8%, surplus is that molybdenum is with inevitable
Impurity.
Above-mentioned a kind of Mo-ZrB2-SiC-AlN composite, it is characterised in that by following quality hundred
The raw material of proportion by subtraction is made: zirconium boride 5%～20%, carborundum 3%～8%, and aluminium nitride 4%～7% is remaining
Amount is molybdenum and inevitable impurity.
Above-mentioned a kind of Mo-ZrB2-SiC-AlN composite, it is characterised in that by following quality hundred
The raw material of proportion by subtraction is made: zirconium boride 15%, carborundum 6%, aluminium nitride 7%, and surplus is molybdenum and can not
The impurity avoided.
It addition, present invention also offers one to prepare above-mentioned Mo-ZrB2The side of-SiC-AlN composite
Method, it is characterised in that the method comprises the following steps:
Step one, use wet ball grinding method by boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum
Powder mix homogeneously, pulverizes after vacuum drying, obtains mixed powder；
Step 2, mixed powder described in step one is placed in discharge plasma sintering stove, in vacuum
Degree is not more than 5 × 10-2Pa, temperature is 1700 DEG C～1800 DEG C, and pressure is the bar of 30MPa～40MPa
Discharge plasma sintering 3min～7min under part, obtains Mo-ZrB after furnace cooling2-SiC-AlN is combined
Material.
Above-mentioned method, it is characterised in that boronation zirconium powder described in step one, carborundum powder and nitridation
The quality purity of aluminium powder is all not less than 99%, and the quality purity of described molybdenum powder is not less than 99.9%.
Above-mentioned method, it is characterised in that boronation zirconium powder described in step one, carborundum powder and nitridation
The particle diameter of aluminium powder is not more than 0.5 μm no more than 100nm, the particle diameter of described molybdenum powder.
Above-mentioned method, it is characterised in that use anhydrous second described in step one during wet ball grinding
Alcohol is dispersant, and the volume of described dehydrated alcohol is zirconium boride, carborundum powder, aluminium nitride and molybdenum powder matter
1.5～3 times of amount sum, wherein the unit of volume is mL, and the unit of quality is g.
Above-mentioned method, it is characterised in that the speed of wet ball grinding described in step one is
200rpm～300rpm, ball material mass ratio is (10～16): 1, and Ball-milling Time is 20h～30h.
Above-mentioned method, it is characterised in that the temperature dried described in step one is 90 DEG C～100 DEG C.
The present invention compared with prior art has the advantage that
1, the present invention is by nanometer zirconium boride (ZrB2) and carborundum (SiC) be incorporated in refractory metal molybdenum, pole
Improve greatly elevated temperature strength and the antioxygenic property of refractory metal molybdenum；Nano aluminum nitride (AlN) is added
To Mo-ZrB2In-SiC ceramic matrix composite material, improve the sintering character of material, contribute to obtaining high densification
Spend thin crystal composite material.
2, to use the technical process of mechanical alloying+discharge plasma sintering to be prepared for the completeest for the present invention
Fully dense Mo-ZrB2-SiC-AlN composite, the method not only has that energy consumption is low, the cycle is short
Advantage, and the Mo-ZrB prepared2-SiC-AlN composite microstructure fine uniform.Tiny
Nano ceramics is evenly distributed in Mo substrate mutually, and this preferable microstructure makes
Mo-ZrB2-SiC-AlN composite has the performance of uniqueness, such as low-density, high intensity, high tenacity
With features such as antioxidation.
3, Mo-ZrB of the present invention2-SiC-AlN composite density is 7.9g/cm3～8.6g/cm3, reason
Opinion density is 98.7%～99.5%, and Room-Temperature Fracture Toughness is 7MPa m1/2～13MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 329MPa～523MPa, in 1400 DEG C of air ambients aoxidize 100h
Rear material unaccounted-for (MUF) is 12 μm～37 μm.
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention 1Mo-ZrB2The micro-organization chart of-SiC-AlN composite.
Detailed description of the invention
Embodiment 1
The present embodiment Mo-ZrB2-SiC-AlN composite is grouped into by the one-tenth of following mass percent:
Zirconium boride (ZrB2) 15%, carborundum (SiC) 6%, aluminium nitride (AlN) 7%, surplus is molybdenum (Mo) and not
Evitable impurity.
The present embodiment Mo-ZrB2The preparation method of-SiC-AlN composite comprises the following steps:
Step one, boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder are placed in ball mill, adopt
With the mode mix homogeneously of wet ball grinding, dry the most under vacuum, pulverize after drying and mixed
Close powder；The quality purity of described boronation zirconium powder, carborundum powder and aluminum nitride powder all not less than 99%,
The particle diameter of described expanded zirconium powder, carborundum powder and aluminum nitride powder no more than 100nm, described molybdenum powder
Particle diameter is not more than 0.5 μm；The dispersant used during described wet ball grinding is dehydrated alcohol, described
The volume of dehydrated alcohol is zirconium boride, carborundum, aluminium nitride and 1.5 times of molybdenum powder quality sum, its
The unit of middle volume is mL, and the unit of quality is g；Described ball mill is planetary ball mill, institute
The rotating speed stating ball mill is 250rpm, and the ball material mass ratio of wet ball grinding is 13: 1, and Ball-milling Time is
25h；The temperature of described drying is 95 DEG C；
Step 2, mixed powder described in rapid are placed in discharge plasma sintering stove, little in vacuum
In 5 × 10-2Pa, temperature is 1750 DEG C, and pressure is discharge plasma sintering 5min under conditions of 40MPa,
Mo-ZrB is obtained after furnace cooling2-SiC-AlN composite.
The present embodiment Mo-ZrB2The microscopic structure of-SiC-AlN composite is as shown in Figure 1.From Fig. 1
In it can be seen that the Mo-ZrB for preparing of the present embodiment2The microscopic structure of-SiC-AlN composite does not has
Observing the defect such as micro-crack and hole, material is almost the finest and close.This is owing to the present invention uses
Mechanical alloying+discharge plasma sintering method prepares Mo-ZrB2-SiC-AlN composite, passes through
Mechanical alloying makes boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder mix homogeneously, and refines
Powder and improve sintering activity；Discharge plasma sintering not only has similar discharge plasma sintering
Joule heat and pressurization cause plastic deformation acceleration of sintering process, and be unique in that electric discharge wait from
Sub-sintering process can produce between powder particle DC pulse voltage, make electric discharge between powder particle be produced from
Heating；The intergranular contact portion of energetic particle hits produced by electric discharge, makes material produce evaporation and makees
With and purify particle surface, improve sintering activity, reduce atom diffusion free energy, help speed up
The diffusion of atom.Analyze Mo-ZrB prepared by the present embodiment further2-SiC-AlN composite micro-
See tissue to find, AlN, Al2O3It is distributed in ZrB with BN2Three corner nodes at, these products
Formation can use AlN and B2O3Between chemical reaction explain:
2AlN+B2O3=Al2O3+2BN (1)
B2O3It is ZrB2The pollutant that particle surface aoxidizes and formed, B2O3Oxide layer reduces material
Sintering activity, prevents the densification of material.(1) formula reaction Gibbs free energy at room temperature is
-270kJ/mol, this is highly beneficial to reaction.The Main Function of AlN additive is to consume ZrB2Granule
The oxide skin(coating) of outside, improves ZrB2Sintering activity, contributes to obtaining the material of high-compactness.
Therefore, the present invention uses mechanical alloying+discharge plasma sintering method to prepare Mo-ZrB2-SiC-AlN
Composite not only reduces sintering temperature, and be obtained in that microstructure fine uniform, densification and
There is no the Mo-ZrB of the defect such as hole and micro-crack2-SiC-AlN composite.Molybdenum phase average crystal grain chi
Very little be about 2 μm, granule boundary is pure, and in etc. shaft-like；Ceramic phase average grain size is about
100nm, nano-ceramic particle is evenly distributed in continuous print Mo substrate, this preferable microstructure
Make Mo-ZrB2-SiC-AlN composite has good comprehensive mechanical property.
ZrB2Ceramic phase has good protectiveness below 1200 DEG C, but along with the rising of temperature, thus
Make original protective layer lose efficacy, can occur to react further with oxygen.This is because B2O3When 1400K
Show significantly evaporation, at more than 1700K, not there is protective effect.By adding SiC, Ke Yigai
Become its oxidation kinetics, and limit B2O3Volatilization.Silicon-boron forms borosilicate more effectively to be stoped
Oxygen spreads to the inside.ZrB2In B be dissolved in SiO2In, define borosilicate glass layer.At oxygen
The initial stage changed, because this glassy layer and pure SiO2Comparing, viscosity is low, so the hole on surface
Gap can be sealed by this layer very fast, prevents B2O3Evaporation.The protection of higher temperature, gives the credit to
ZrO2With SiO2Between react the ZrSiO of formation4。ZrSiO4Until 1949K is stable, fine and close
Stable ZrSiO4Oxygen outside oxide-film prevention invades and causes continuation oxidation, is effectively protected material.
Therefore, the present invention is by nanometer ZrB2, SiC and AlN superhigh temperature ceramics be incorporated in refractory metal molybdenum,
Not only increase the elevated temperature strength of refractory metal molybdenum, reduce density, the most also there is good antioxygen
Change performance.
Mo-ZrB prepared by the present embodiment2-SiC-AlN composite microstructure fine uniform, density
For 8.3g/cm3, solid density is 99.5%, and Room-Temperature Fracture Toughness is 13MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 523MPa, 1400 DEG C of air ambients aoxidize material after 100h and damage
Mistake is 12 μm, has the features such as low-density, high intensity, high tenacity and antioxidation, it is possible at 1400 DEG C
Air uses.
Embodiment 2
The present embodiment Mo-ZrB2-SiC-AlN composite is grouped into by the one-tenth of following mass percent:
Zirconium boride (ZrB2) 5%, carborundum (SiC) 3%, aluminium nitride (AlN) 4%, surplus is molybdenum (Mo) and not
Evitable impurity.
The present embodiment Mo-ZrB2The preparation method of-SiC-AlN composite comprises the following steps:
Step one, boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder are placed in ball mill, adopt
With the mode mix homogeneously of wet ball grinding, dry the most under vacuum, pulverize after drying and mixed
Close powder；The quality purity of described boronation zirconium powder, carborundum powder and aluminum nitride powder all not less than 99%,
The particle diameter of described expanded zirconium powder, carborundum powder and aluminum nitride powder no more than 100nm, described molybdenum powder
Particle diameter is not more than 0.5 μm；The dispersant used during described wet ball grinding is dehydrated alcohol, described
The volume of dehydrated alcohol is zirconium boride, carborundum, aluminium nitride and 2 times of molybdenum powder quality sum, wherein
The unit of volume is mL, and the unit of quality is g；Described ball mill is planetary ball mill, described
The rotating speed of ball mill is 200rpm, and the ball material mass ratio of wet ball grinding is 10: 1, and Ball-milling Time is
20h；The temperature of described drying is 90 DEG C；
Step 2, mixed powder described in rapid are placed in discharge plasma sintering stove, little in vacuum
In 5 × 10-2Pa, temperature is 1700 DEG C, and pressure is discharge plasma sintering 3min under conditions of 30MPa,
Mo-ZrB is obtained after furnace cooling2-SiC-AlN composite.
Mo-ZrB prepared by the present embodiment2-SiC-AlN composite microstructure fine uniform, close
Degree is 8.4g/cm3, solid density is 99.2%, and Room-Temperature Fracture Toughness is 11MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 369MPa, 1400 DEG C of air ambients aoxidize material after 100h and damage
Mistake is 32 μm, has the features such as low-density, high intensity, high tenacity and antioxidation, it is possible at 1400 DEG C
Air uses.
Embodiment 3
The present embodiment Mo-ZrB2-SiC-AlN composite is grouped into by the one-tenth of following mass percent:
Zirconium boride (ZrB2) 20%, carborundum (SiC) 8%, aluminium nitride (AlN) 6%, surplus be molybdenum (Mo) and
Inevitably impurity.
The present embodiment Mo-ZrB2The preparation method of-SiC-AlN composite comprises the following steps:
Step one, boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder are placed in ball mill, adopt
With the mode mix homogeneously of wet ball grinding, dry the most under vacuum, pulverize after drying and mixed
Close powder；The quality purity of described boronation zirconium powder, carborundum powder and aluminum nitride powder all not less than 99%,
The particle diameter of described expanded zirconium powder, carborundum powder and aluminum nitride powder no more than 100nm, described molybdenum powder
Particle diameter is not more than 0.5 μm；The dispersant used during described wet ball grinding is dehydrated alcohol, described
The volume of dehydrated alcohol is zirconium boride, carborundum, aluminium nitride and 3 times of molybdenum powder quality sum, wherein
The unit of volume is mL, and the unit of quality is g；Described ball mill is planetary ball mill, described
The rotating speed of ball mill is 300rpm, and the ball material mass ratio of wet ball grinding is 16: 1, and Ball-milling Time is
30h；The temperature of described drying is 100 DEG C；
Step 2, mixed powder described in rapid are placed in discharge plasma sintering stove, little in vacuum
In 5 × 10-2Pa, temperature is 1800 DEG C, and pressure is discharge plasma sintering 7min under conditions of 30MPa,
Mo-ZrB is obtained after furnace cooling2-SiC-AlN composite.
Mo-ZrB prepared by the present embodiment2-SiC-AlN composite microstructure fine uniform, density
For 8.1g/cm3, solid density is 99.5%, and Room-Temperature Fracture Toughness is 9MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 479MPa, 1400 DEG C of air ambients aoxidize material after 100h and damage
Mistake is 16 μm, has the features such as low-density, high intensity, high tenacity and antioxidation, it is possible at 1400 DEG C
Air uses.
Embodiment 4
The present embodiment Mo-ZrB2-SiC-AlN composite is grouped into by the one-tenth of following mass percent:
Zirconium boride (ZrB2) 3%, carborundum (SiC) 2%, aluminium nitride (AlN) 2%, surplus is molybdenum (Mo) and not
Evitable impurity.
The present embodiment Mo-ZrB2The preparation method of-SiC-AlN composite comprises the following steps:
Step one, boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder are placed in ball mill, adopt
With the mode mix homogeneously of wet ball grinding, dry the most under vacuum, pulverize after drying and mixed
Close powder；The quality purity of described boronation zirconium powder, carborundum powder and aluminum nitride powder all not less than 99%,
The particle diameter of described expanded zirconium powder, carborundum powder and aluminum nitride powder no more than 100nm, described molybdenum powder
Particle diameter is not more than 0.5 μm；The dispersant used during described wet ball grinding is dehydrated alcohol, described
The volume of dehydrated alcohol is zirconium boride, carborundum, aluminium nitride and 2.2 times of molybdenum powder quality sum, its
The unit of middle volume is mL, and the unit of quality is g；Described ball mill is planetary ball mill, institute
The rotating speed stating ball mill is 230rpm, and the ball material mass ratio of wet ball grinding is 11: 1, and Ball-milling Time is
22h；The temperature of described drying is 93 DEG C；
Step 2, mixed powder described in rapid are placed in discharge plasma sintering stove, little in vacuum
In 5 × 10-2Pa, temperature is 1730 DEG C, and pressure is discharge plasma sintering 4min under conditions of 35MPa,
Mo-ZrB is obtained after furnace cooling2-SiC-AlN composite.
Mo-ZrB prepared by the present embodiment2-SiC-AlN composite microstructure fine uniform, density
For 8.6g/cm3, solid density is 98.7%, and Room-Temperature Fracture Toughness is 13MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 329MPa, 1400 DEG C of air ambients aoxidize material after 100h and damage
Mistake is 37 μm, has the features such as low-density, high intensity, high tenacity and antioxidation, it is possible at 1400 DEG C
Air uses.
Embodiment 5
The present embodiment Mo-ZrB2-SiC-AlN composite is grouped into by the one-tenth of following mass percent:
Zirconium boride (ZrB2) 25%, carborundum (SiC) 10%, aluminium nitride (AlN) 8%, surplus be molybdenum (Mo) and
Inevitably impurity.
The present embodiment Mo-ZrB2The preparation method of-SiC-AlN composite comprises the following steps:
Step one, boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder are placed in ball mill, adopt
With the mode mix homogeneously of wet ball grinding, dry the most under vacuum, pulverize after drying and mixed
Close powder；The quality purity of described boronation zirconium powder, carborundum powder and aluminum nitride powder all not less than 99%,
The particle diameter of described expanded zirconium powder, carborundum powder and aluminum nitride powder no more than 100nm, described molybdenum powder
Particle diameter is not more than 0.5 μm；The dispersant used during described wet ball grinding is dehydrated alcohol, described
The volume of dehydrated alcohol is zirconium boride, carborundum, aluminium nitride and 2.8 times of molybdenum powder quality sum, its
The unit of middle volume is mL, and the unit of quality is g；Described ball mill is planetary ball mill, institute
The rotating speed stating ball mill is 230rpm, and the ball material mass ratio of wet ball grinding is 15: 1, and Ball-milling Time is
22h；The temperature of described drying is 98 DEG C；
Step 2, mixed powder described in rapid are placed in discharge plasma sintering stove, little in vacuum
In 5 × 10-2Pa, temperature is 1730 DEG C, and pressure is discharge plasma sintering 6min under conditions of 37MPa,
Mo-ZrB is obtained after furnace cooling2-SiC-AlN composite.
Mo-ZrB prepared by the present embodiment2-SiC-AlN composite microstructure fine uniform, density
For 7.9g/cm3, solid density is 98.7%, and Room-Temperature Fracture Toughness is 7MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 523MPa, 1400 DEG C of air ambients aoxidize material after 100h and damage
Mistake is 12 μm, has the features such as low-density, high intensity, high tenacity and antioxidation, it is possible at 1400 DEG C
Air uses.
Embodiment 6
The present embodiment Mo-ZrB2-SiC-AlN composite is grouped into by the one-tenth of following mass percent:
Zirconium boride (ZrB2) 25%, carborundum (SiC) 10%, aluminium nitride (AlN) 5%, surplus be molybdenum (Mo) and
Inevitably impurity.
The present embodiment Mo-ZrB2The preparation method of-SiC-AlN composite comprises the following steps:
Step one, boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum powder are placed in ball mill, adopt
With the mode mix homogeneously of wet ball grinding, dry the most under vacuum, pulverize after drying and mixed
Close powder；The quality purity of described boronation zirconium powder, carborundum powder and aluminum nitride powder all not less than 99%,
The particle diameter of described expanded zirconium powder, carborundum powder and aluminum nitride powder no more than 100nm, described molybdenum powder
Particle diameter is not more than 0.5 μm；The dispersant used during described wet ball grinding is dehydrated alcohol, described
The volume of dehydrated alcohol is zirconium boride, carborundum, aluminium nitride and 2.5 times of molybdenum powder quality sum, its
The unit of middle volume is mL, and the unit of quality is g；Described ball mill is planetary ball mill, institute
The rotating speed stating ball mill is 250rpm, and the ball material mass ratio of wet ball grinding is 16: 1, and Ball-milling Time is
20h；The temperature of described drying is 100 DEG C；
Step 2, mixed powder described in rapid are placed in discharge plasma sintering stove, little in vacuum
In 5 × 10-2Pa, temperature is 1750 DEG C, and pressure is discharge plasma sintering 5min under conditions of 40MPa,
Mo-ZrB is obtained after furnace cooling2-SiC-AlN composite.
Mo-ZrB prepared by the present embodiment2-SiC-AlN composite microstructure fine uniform, density
For 8.0g/cm3, solid density is 99.5%, and Room-Temperature Fracture Toughness is 10MPa m1/2, at 1400 DEG C
Under the conditions of tensile strength be 501MPa, 1400 DEG C of air ambients aoxidize material after 100h and damage
Mistake is 12 μm μm, has the features such as low-density, high intensity, high tenacity and antioxidation, it is possible at 1400 DEG C
Air uses.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention.All
It is that any simple modification, change and the equivalence made above example according to inventive technique essence becomes
Change, all still fall within the protection domain of technical solution of the present invention.
Claims (9)
1. a Mo-ZrB2-SiC-AlN composite, it is characterised in that by following percent mass
The one-tenth of ratio is grouped into: zirconium boride 3%～25%, carborundum 2%～10%, aluminium nitride 2%～8%, surplus
For molybdenum and inevitable impurity.
A kind of Mo-ZrB the most according to claim 12-SiC-AlN composite, its feature
It is, is made up of the raw material of following mass percent: zirconium boride 5%～20%, carborundum 3%～8%,
Aluminium nitride 4%～7%, surplus is molybdenum and inevitable impurity.
A kind of Mo-ZrB the most according to claim 22-SiC-AlN composite, its feature
It is, is made up of the raw material of following mass percent: zirconium boride 15%, carborundum 6%, aluminium nitride
7%, surplus is molybdenum and inevitable impurity.
4. prepare Mo-ZrB as described in claim 1,2 or 3 for one kind2-SiC-AlN composite
Method, it is characterised in that the method comprises the following steps:
Step one, use wet ball grinding method by boronation zirconium powder, carborundum powder, aluminum nitride powder and molybdenum
Powder mix homogeneously, pulverizes after vacuum drying, obtains mixed powder；
Step 2, mixed powder described in step one is placed in discharge plasma sintering stove, in vacuum
Degree is not more than 5 × 10-2Pa, temperature is 1700 DEG C～1800 DEG C, and pressure is the bar of 30MPa～40MPa
Discharge plasma sintering 3min～7min under part, obtains Mo-ZrB after furnace cooling2-SiC-AlN is combined
Material.
Method the most according to claim 4, it is characterised in that zirconium boride described in step one
The quality purity of powder, carborundum powder and aluminum nitride powder all not less than 99%, the quality purity of described molybdenum powder
Not less than 99.9%.
Method the most according to claim 4, it is characterised in that zirconium boride described in step one
The particle diameter of powder, carborundum powder and aluminum nitride powder is not more than no more than 100nm, the particle diameter of described molybdenum powder
0.5μm。
Method the most according to claim 4, it is characterised in that wet method ball described in step one
Using dehydrated alcohol during mill is dispersant, and the volume of described dehydrated alcohol is zirconium boride, carbonization
Silica flour, aluminium nitride and 1.5～3 times of molybdenum powder quality sum, wherein the unit of volume is mL, quality
Unit be g.
Method the most according to claim 4, it is characterised in that wet method ball described in step one
The speed of mill is 200rpm～300rpm, and ball material mass ratio is (10～16): 1, and Ball-milling Time is
20h～30h.
Method the most according to claim 4, it is characterised in that dry described in step one
Temperature is 90 DEG C～100 DEG C.
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| CN107760952A (en) * | 2017-11-08 | 2018-03-06 | 西北有色金属研究院 | A kind of Mo Si C alloy bars and preparation method thereof |
| CN109231973A (en) * | 2018-10-31 | 2019-01-18 | 广州供电局有限公司 | Complex phase ceramic insulating part and preparation method thereof |
| CN115612904A (en) * | 2022-08-26 | 2023-01-17 | 洛阳科威钨钼有限公司 | High-hardness TZM alloy and preparation method thereof |
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| CN105177385A (en) * | 2015-10-26 | 2015-12-23 | 西北有色金属研究院 | Nb-Si-Ti-W-Hf composite material and preparation method thereof |
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| CN105177385A (en) * | 2015-10-26 | 2015-12-23 | 西北有色金属研究院 | Nb-Si-Ti-W-Hf composite material and preparation method thereof |
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| CN107760952A (en) * | 2017-11-08 | 2018-03-06 | 西北有色金属研究院 | A kind of Mo Si C alloy bars and preparation method thereof |
| CN107760952B (en) * | 2017-11-08 | 2018-11-02 | 西北有色金属研究院 | A kind of Mo-Si-C alloy bar materials and preparation method thereof |
| CN109231973A (en) * | 2018-10-31 | 2019-01-18 | 广州供电局有限公司 | Complex phase ceramic insulating part and preparation method thereof |
| CN109231973B (en) * | 2018-10-31 | 2022-02-01 | 广东电网有限责任公司广州供电局 | Complex phase ceramic insulator and preparation method thereof |
| CN115612904A (en) * | 2022-08-26 | 2023-01-17 | 洛阳科威钨钼有限公司 | High-hardness TZM alloy and preparation method thereof |
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