CN107190194B - A kind of preparation method of boride ceramic particles enhancing niobium molybdenum-base composite material - Google Patents

A kind of preparation method of boride ceramic particles enhancing niobium molybdenum-base composite material Download PDF

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CN107190194B
CN107190194B CN201710457857.XA CN201710457857A CN107190194B CN 107190194 B CN107190194 B CN 107190194B CN 201710457857 A CN201710457857 A CN 201710457857A CN 107190194 B CN107190194 B CN 107190194B
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powder
temperature
mixed
sintering
composite material
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CN107190194A (en
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刘宗德
王�琦
王永田
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Beijing Huadian Hi Tech Co Ltd
Jiangsu Kehuan New Materials Co Ltd
North China Electric Power University
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Beijing Huadian Hi Tech Co Ltd
Jiangsu Kehuan New Materials Co Ltd
North China Electric Power University
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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
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • 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
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/14—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on borides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • C22C32/0073—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 only borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention discloses a kind of method that vacuum heating-press sintering prepares boride ceramic particles enhancing niobium molybdenum-base composite material, this method includes the following steps：1) mixed-powder, is prepared, the powder includes ZrB215 50wt%, Nb25 51wt% and Mo surpluses；The weight ratio of wherein Nb powder and Mo powder is 1 1.5；By the powder dry mixed；2) it, by the mixed-powder vacuum heating-press sintering, is as follows：(1) it is pressed into tire base；(2) it dries；(3) it is sintered in dynamic vacuum；(4) for maximum sintering temperature up to 2600 DEG C, heating rate is 40 95 DEG C/min；(5) it pressurizes in sintering process to mixed-powder；(6) speed adjust is will heat up after the pressurizing as 40 50 DEG C/min, is increased in-furnace temperature, is made pressure rise；(7) forcing press is closed, closes heating power supply, the temperature of sintering furnace is down to room temperature by natural Slow cooling, and rate of temperature fall is 10 50 DEG C/min.

Description

A kind of preparation method of boride ceramic particles enhancing niobium molybdenum-base composite material
Technical field
The invention belongs to technical field of composite materials, and boride ceramics is prepared more particularly to a kind of vacuum heating-press sintering The method of grain enhancing niobium molybdenum-base composite material utilizes vacuum heating-press sintering synthesis boride ceramic particles enhancing niobium molybdenum base composite wood Material.
Background technology
Particles reiforced metal-base composition is due to high specific stiffness, specific strength, specific modulus, wearability and resistance to height The excellent performance such as temperature is a kind of high-performance advanced material.
Ceramic material has many advantages, such as that corrosion resistance is good, wear-resisting, but brittleness is larger and not easy to be processed；Metal material has excellent Ductility, but it is wear-resisting, anti-corrosion, heat-resisting quantity is poor.Particles reiforced metal-base composition has taken into account the heat-resisting quantity of ceramics With the good toughness of metal, there are single ceramic or incomparable metal material excellent properties, in Aeronautics and Astronautics, automobile etc. Field has a good application prospect.
In ceramic material system, compound (such as ZrB of refractory metal and B, C composition2、ZrC、TaC、 HfB2Etc. superelevation Warm ceramics) fusing point more than 3000 DEG C, the excellent thermo-chemical stability of these compounds is allowed them to as extreme environment The lower candidate material used.Carbide and nitride ceramics there are antioxygenic property it is poor the problem of, so oxidation resistant Boride ceramics and its composite material become research emphasis.Since the last century 60's, just carry out both at home and abroad ZrB2The research of based ultra-high temperature ceramics (its target temperature in use is up to 2000 DEG C or more).Due to ZrB2Ceramics fusing point it is high with And Zr is low with the self-diffusion coefficient of B atoms, so as to pass through the ZrB of direct sintering densification2It is more difficult.Research shows that by mixing Comparatively dense ZrB can be prepared by entering the sintering aids such as carbide, silicide, nitride and rare metal oxide2Base superelevation Warm ceramics.ZrB2Antioxygenic property (the ZrB that ceramics have had at 1100 DEG C2B is formed after oxidation2O3Protective film), and temperature is high When 1100 DEG C, B2O3It volatilizees and loses protective effect.The method of comparative maturity is by ZrB at present2It is compound with SiC, make its 1200 DEG C and when temperatures above, form SiO2Protective film, thus by ZrB2The antioxygenic property of-SiC composite ceramics is increased to 1800 ℃。
Although having been carried out years of researches both at home and abroad, ZrB2The fracture toughnesses of based ultra-high temperature ceramics is poor, heat resistanceheat resistant punching It hits the problem of performance is weaker never effectively to be solved, which greatly limits ZrB2Based ultra-high temperature ceramics are answered Use range.
Refractory metal and its alloy have many advantages, such as that fusing point is high, elevated temperature strength is high, and temperature in use >=1100 DEG C are important Space flight high-temperature structural material.The temperature in use of refractory metal and its alloy is directly related with their fusing point, uses at present Most alloys is niobium alloy and molybdenum alloy.Even if niobium alloy also has preferable plasticity in low temperature (- 196 DEG C), but it is main Shortcoming is poor for high-temperature creep resistance and inoxidizability.Nb-Mo, Nb-W, Nb-Ta etc. are unlimited solid solution alloy, and there is no high-temperature-phases Become or generation brittlement phase the problems such as, therefore, added in Nb a certain proportion of W, Mo, Ta be improve niobium-base alloy high temperature it is strong One of degree and the effective way of croop property.
Due to molybdenum alloy there are black brittleness, welding brittleness, processing difficulties and high temperature oxidation resistance are poor the shortcomings of, application Range is restricted.
Ceramic particle enhancing refractory metal based composites are directed to introduce suitable second phase increasing in refractory metal basal body Strong particle, advantage are：(1) superhigh temperature intensity, the superhigh temperature croop property of ceramic particle enhancing refractory metal based composites It is significantly higher than refractory alloy；(2) high temperature of ceramic particle enhancing refractory metal based composites and superhigh temperature fracture toughness are notable Higher than the value of ceramic material.
Boride ceramics and refractory alloy are respectively provided with high fusing point, such as prepare pottery using traditional high temperature hot pressing sintering method Porcelain particle enhances refractory metal based composites, then there are problems that composite material consistency is low low with elevated temperature strength etc..State at present The inside and outside research to boride ceramic particles enhancing refractory metal based composites is also extremely limited.Therefore, it is equal to prepare tissue Even, high-compactness boride ceramic particles enhancing niobium molybdenum-base composite material is technological difficulties at this stage.
Invention content
It is an object of the present invention to propose a kind of ingredient and system of boride ceramic particles enhancing niobium molybdenum-base composite material Preparation Method solves the problems, such as that niobium-base alloy, molybdenum-base alloy acutely decline in 1100 DEG C of temperatures above intensity, the composite material≤ Under 1800 DEG C of hyperthermal environments there is higher intensity, be a kind of ceramic particle that can be used under hyperthermal environments enhancing Refractory metal based composites.Technical scheme is as follows：
A kind of preparation method of boride ceramic particles enhancing niobium molybdenum-base composite material, includes the following steps：
1) mixed-powder, is prepared
The powder includes ZrB215-50wt%, Nb25-51wt% and Mo surplus；Wherein the weight of Nb powder and Mo powder it Than for 1-1.5；By the powder dry mixed；Further, in the powder, ZrB2600 mesh of powder, purity >=99.95%：Nb powder 500-800 mesh, purity >=99.95%：Mo powder 500-800 mesh, purity >=99.95%.
It is 3 hours dry under the conditions of 110 DEG C that the powder of said ratio, which is put into drying box in temperature, is then placed in planet It is mixed in formula ball mill, drum's speed of rotation 180-220rpm, powder mixing is obtained ingredient after 10-15 hours uniformly mixes Powder.
2), vacuum heating-press sintering
Boride ceramic particles enhancing niobium molybdenum-base composite material is prepared using vacuum super high sintering temperature stove, the specific steps are：
(1) mixed-powder is placed in pre-fabricated mold, using the Y32-50T forcing presses that pressure is 50 tons in room temperature It is lower that mixed-powder is pressed into tire base；The pressure that forcing press is applied on mixed-powder is 25-30MPa；
(2) the tire base suppressed is put into dryer and dried, drying temperature is 250-300 DEG C, drying time 45-60 Minute；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vacuum pump, when vacuum pump registration is -0.15~-0.1MPa, is passed through argon gas, air pressure in stove is kept In the dynamic vacuum of -0.09~-0.07MPa, and until being continued until that stove is cooled to room temperature；
(5) start maximum sintering temperature up to 2600 DEG C, tonnage up to 15 tons of vacuum superhigh temperature hot-pressed sintering furnace to mixed The heating of powder tire base is closed, the heating rate of mixed-powder tire base is 40-95 DEG C/min；In-furnace temperature is detected using thermocouple, when When in-furnace temperature rises to 1700-1900 DEG C, start the pressure that mechanical press applies tire base pressure sintering, press ram It it is 15-30 minutes to the soaking time of tire base at a temperature of 1700-1900 DEG C for 25-30MPa；
(6) continue to high temperature stove heat, heating ramp rate is 40-50 DEG C/min, and measuring point temperature in stove is made to rise to 2400- 2600℃；Mechanical press is adjusted, pressure rise is made to keep the temperature 10-15 minutes to 50MPa；
(7) forcing press is closed, closes heating power supply, the temperature of sintering furnace is down to room temperature, cooling speed by natural Slow cooling Rate is 10-50 DEG C/min.
Compared with prior art, the present invention its remarkable advantage is：(1) it is prepared using vacuum high-frequency sensing super high sintering temperature method Boride ceramic particles enhance niobium molybdenum-base composite material, and the experiment condition of high temperature and pressure can melt whole metal phases and part Ceramic phase passes through composition design and preparation process, the ZrB of addition2It reacts to have synthesized with Nb, Mo and contains Nb3B2With NbB complex phase boron The composite material of compound ceramics enhancing；(2) compression strength of the composite material at room temperature is 1400-1700MPa, at 1300 DEG C Compression strength is 200-700MPa, is 130-160MPa in 1700 DEG C of compression strength, far above pure niobium base and the pottery of pure molybdenum base Porcelain mutually enhances the intensity of composite material at the same temperature；(3) the highest consistency of the composite material is more than 99%, wherein Nb3B2 Microhardness with NbB complex phase borides is 14-15GPa.
Description of the drawings
Fig. 1 is the high-frequency induction heating sintering furnace schematic diagram that the present invention uses.In figure：1- cylinder bodies, 2- pistons, 3- fire resistings Plate, 4- fire resisting heating units, 5- molds, 6- furnace bodies, 7- workbench, 8- argon gas pump, 9- thermocouples, 10- vacuum pumps, 11- high frequencies Induction coil, 12- power supplys.
Fig. 2 is ZrB of the present invention2Mass fraction is 22% niobium molybdenum-base composite material stereoscan photograph.13 are in figure ZrO phases, 14 be Nb3B2Phase, 15 be rich molybdenum phase niobium molybdenum solid solution.
Fig. 3 is ZrB of the present invention2Mass fraction is 35% niobium molybdenum-base composite material stereoscan photograph.16 are in figure ZrB2Phase, 17 be Nb3B2Phase, 18 be rich molybdenum phase niobium molybdenum solid solution.
Fig. 4 is ZrB of the present invention2Mass fraction is 50% niobium molybdenum-base composite material stereoscan photograph.19 are in figure ZrB2Phase, 20 be Mo2Zr phases, 21 be Nb3B2It is mutually rich molybdenum phase niobium molybdenum solid solution with the mixture of NbB phases, 22.
Fig. 5 is compressive stress strain curve figure of the material of the present invention at 1300 DEG C.23 be ZrB in figure2Mass fraction is 35% niobium molybdenum-base composite material, 24 be ZrB2Mass fraction is 50% niobium molybdenum-base composite material.
Fig. 6 is compressive stress strain curve figure of the material of the present invention at 1700 DEG C.25 be ZrB in figure2Mass fraction is 35% niobium molybdenum-base composite material, 26 be ZrB2Mass fraction is 50% niobium molybdenum-base composite material.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples.
Embodiment 1
Prepare ZrB2The boride ceramic particles that mass fraction is 22% enhance niobium molybdenum-base composite material：
Alloy powder and ceramic powder are weighed, boride is prepared using vacuum high-frequency induction heating ultra-temperature hot-pressed sintering furnace Ceramic particle enhances niobium molybdenum-base composite material.Dusty material is by ZrB2, the compositions such as Nb, Mo.In selected powder, ZrB2Powder (600 mesh, purity >=99.95%)：22wt.%；Nb powder (500-800 mesh, purity >=99.95%)：38wt.%；Mo powder (500- 800 mesh, purity >=99.95%)：Surplus.
The specific steps are：
(1) mixed-powder is placed in pre-fabricated mold, using Y32-50T forcing presses at room temperature by mixed-powder It is pressed into tire base；The pressure that forcing press is applied on mixed-powder is 25MPa；
(2) the tire base suppressed is put into dryer and dried, drying temperature is 250 DEG C, and drying time is 45 minutes；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vacuum pump, when vacuum pump registration is -0.1MPa, be passed through argon gas, air pressure in stove is maintained at - In the dynamic vacuum of 0.08MPa, and until being continued until that stove is cooled to room temperature；
(5) start high-frequency induction heating superhigh temperature hot-pressed sintering furnace to heat up to mixed-powder tire base, heating power is 160kW, the heating rate of mixed-powder tire base is 95 DEG C/min；In-furnace temperature is detected using thermocouple, when in-furnace temperature rises to At 1800 DEG C, starting mechanical press to mixed-powder pressure sintering, the pressure that press ram applies is 25MPa, It it is 30 minutes to the soaking time of powder at a temperature of 1800 DEG C；
(6) continuing to high temperature stove heat, heating ramp rate is 47 DEG C/min, and measuring point temperature in stove is made to rise to 2500 DEG C, Mechanical press pressure rise is made to keep the temperature 10 minutes to 50MPa；
(7) forcing press is closed, closes heating power supply, the temperature of sintering furnace is down to room temperature, cooling speed by natural Slow cooling Rate is 10-50 DEG C/min.
The material being prepared is high cylindrical shape, is highly a diameter of 14mm, 100mm.Fig. 2 is ZrB2Mass fraction For the stereoscan photograph of 22% niobium molybdenum-base composite material, apparent element segregation, even tissue and crystal grain are not present in figure Tiny, ZrO phases play the role of dispersion-strengtherning, Nb in figure3B2The hardness of phase can reach 6.5GPa, the presence card of niobium molybdenum solid solution Real solution strengthening effect.Due to the collective effect of the solution strengthening effect of the dispersion-strengthened action and metallic atom of ZrO phases, The compressive strength at room temperature of composite material may be up to 1403MPa, far above pure niobium base or the ceramic particle reinforcing material of pure molybdenum base.
Embodiment 2
Prepare ZrB2The boride ceramic particles that mass fraction is 35% enhance niobium molybdenum-base composite material：
Alloy powder and ceramic powder are weighed, boride is prepared using vacuum high-frequency induction heating ultra-temperature hot-pressed sintering furnace Ceramic particle enhances niobium molybdenum-base composite material.Dusty material is by ZrB2, the compositions such as Nb, Mo.In selected powder, ZrB2Powder (600 mesh, purity >=99.95%)：35wt.%, Nb powder (500-800 mesh, purity >=99.95%)：32wt.%, Mo powder (500- 800 mesh, purity >=99.95%)：Surplus.
The specific steps are：
(1) mixed-powder is placed in pre-fabricated mold, using Y32-50T forcing presses at room temperature by mixed-powder It is pressed into tire base；The pressure that forcing press is applied on mixed-powder is 28MPa；
(2) the tire base suppressed is put into dryer and dried, drying temperature is 280 DEG C, and drying time is 55 minutes；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vacuum pump, when vacuum pump registration is -0.15MPa, be passed through argon gas, air pressure in stove is maintained at - In the dynamic vacuum of 0.07MPa, and until being continued until that stove is cooled to room temperature；
(5) start high-frequency induction heating superhigh temperature hot-pressed sintering furnace to heat up to mixed-powder tire base, heating power is 200kW, the heating rate of mixed-powder tire base is 65 DEG C/min；In-furnace temperature is detected using thermocouple, when in-furnace temperature rises to At 1900 DEG C, starting mechanical press to mixed-powder pressure sintering, the pressure that press ram applies is 28MPa, It it is 15 minutes to the soaking time of powder at a temperature of 1900 DEG C；
(6) continuing to high temperature stove heat, heating ramp rate is 47 DEG C/min, and measuring point temperature in stove is made to rise to 2600 DEG C, Mechanical press pressure rise is made to keep the temperature 15 minutes to 50MPa；
(7) forcing press is closed, closes heating power supply, the temperature of sintering furnace is down to room temperature, cooling speed by natural Slow cooling Rate is 10-50 DEG C/min.
The material being prepared is short cylindrical shape, and a diameter of 50mm is highly 20mm.Fig. 3 is ZrB2Mass fraction For the stereoscan photograph of 35% niobium molybdenum-base composite material, ZrB in figure2Mutually play the role of dispersion-strengtherning, Nb3B2Phase it is hard Degree can reach 11.4GPa, helpful to the intensity for improving composite material, and the presence of niobium molybdenum solid solution confirms that solution strengthening is imitated It answers, can further promote the intensity of composite material.Due to ZrB2The dispersion-strengthened action of phase and metallic atom solution strengthening effect The collective effect answered, the compressive strength at room temperature of composite material are 1202MPa, and the compression strength at 1300 DEG C is 207MPa, 1700 Compression strength at DEG C is 171MPa, far above pure niobium base or the ceramic particle reinforcing material of pure molybdenum base.
Embodiment 3
Prepare ZrB2The boride ceramic particles that mass fraction is 50% enhance niobium molybdenum-base composite material：
Alloy powder and ceramic powder are weighed, boride is prepared using vacuum high-frequency induction heating ultra-temperature hot-pressed sintering furnace Ceramic particle enhances niobium molybdenum-base composite material.Dusty material is by ZrB2, the compositions such as Nb, Mo.In selected powder, ZrB2Powder (600 mesh, purity >=99.95%)：50wt.%, Nb powder (500-800 mesh, purity >=99.95%)：25wt.%, Mo powder (500- 800 mesh, purity >=99.95%)：Surplus.
The specific steps are：
(1) mixed-powder is placed in pre-fabricated mold, using Y32-50T forcing presses at room temperature by mixed-powder It is pressed into tire base；The pressure that forcing press is applied on mixed-powder is 30MPa；
(2) the tire base suppressed is put into dryer and dried, drying temperature is 300 DEG C, and drying time is 60 minutes；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vacuum pump, when vacuum pump registration is -0.12MPa, be passed through argon gas, air pressure in stove is maintained at - In the dynamic vacuum of 0.09MPa, and until being continued until that stove is cooled to room temperature；
(5) start high-frequency induction heating superhigh temperature hot-pressed sintering furnace to heat up to mixed-powder tire base, heating power is 250kW, the heating rate of mixed-powder tire base is 40 DEG C/min；In-furnace temperature is detected using thermocouple, when in-furnace temperature rises to At 1700 DEG C, starting mechanical press to mixed-powder pressure sintering, the pressure that press ram applies is 30MPa, It it is 20 minutes to the soaking time of powder at a temperature of 1700 DEG C；
(6) continuing to high temperature stove heat, heating ramp rate is 40 DEG C/min, and measuring point temperature in stove is made to rise to 2400 DEG C, Mechanical press pressure rise is made to keep the temperature 10 minutes to 50MPa；
(7) forcing press is closed, closes heating power supply, the temperature of sintering furnace is down to room temperature, cooling speed by natural Slow cooling Rate is 10-50 DEG C/min.
The material being prepared is short cylindrical shape, and a diameter of 50mm is highly 60mm.Fig. 4 is ZrB2Mass fraction For the stereoscan photograph of 50% niobium molybdenum-base composite material, ZrB in figure2Mutually play the role of dispersion-strengtherning, Nb3B2It is answered with NbB The hardness of boride phase can reach 14.3GPa, and the presence of niobium molybdenum solid solution confirms solution strengthening effect.Due to ZrB2Phase is more The collective effect of invigoration effect and metallic atom solution strengthening effect is dissipated, the compressive strength at room temperature of composite material is 1636MPa, Compression strength at 1300 DEG C is 642MPa, and the compression strength at 1700 DEG C is 144MPa, far above pure niobium base or pure molybdenum base Ceramic particle reinforcing material.
Technical scheme of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited it is retouched The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.

Claims (4)

1. a kind of preparation method of boride ceramic particles enhancing niobium molybdenum-base composite material, which is characterized in that step is as follows：
1）, prepare mixed-powder
The powder includes ZrB250wt%, Nb25-51wt% and Mo surplus；The weight ratio of wherein Nb powder and Mo powder is 1-1.5, The sum of content of three kinds of components is 100wt%；By the powder dry mixed；
2）, vacuum heating-press sintering, be as follows：
（1）The mixed-powder is placed in prefabricated mould, is pressed into tire base；
（2）The tire base suppressed is dried；
（3）Tire base after drying is placed in carbon fiber crucible, is sintered in dynamic vacuum；
（4）For maximum sintering temperature up to 2600 DEG C, heating rate is 40-95 DEG C/min；
（5）It pressurizes in sintering process to mixed-powder；
（6）Speed adjust be will heat up after the pressurizing as 40-50 DEG C/min, in-furnace temperature is increased, make pressure rise；
（7）Forcing press is closed, closes heating power supply, the temperature of sintering furnace is down to room temperature by natural Slow cooling, and rate of temperature fall is 10-50℃/min；
Wherein, step 2）Described in sintering process, when temperature rises to 1700-1900 DEG C, pressurize to tire base, pressure 25- 30MPa, and keep the temperature 15-30 minutes at this temperature；Subsequent temperature of continuing rising of pressurizeing makes pressure rise to 50MPa, at 2400-2600 DEG C Heat preservation 10-15 minutes.
2. method according to claim 1, which is characterized in that step 1）Described in powder, ZrB2600 mesh of powder, purity >= 99.95%：Nb powder 500-800 mesh, purity >=99.95%：Mo powder 500-800 mesh, purity >=99.95%.
3. method according to claim 1, which is characterized in that step 2）Described in drying temperature be 250-300 DEG C, during drying Between be 45-60 minutes.
4. method according to claim 1, which is characterized in that step 2）Described in dynamic vacuum be -0.09~-0.07MPa, When vacuum pump registration is -0.15~-0.1MPa, it is passed through argon gas.
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