CN107190194A - A kind of boride ceramic particles strengthen the preparation method of niobium molybdenum-base composite material - Google Patents
A kind of boride ceramic particles strengthen the preparation method of niobium molybdenum-base composite material Download PDFInfo
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- CN107190194A CN107190194A CN201710457857.XA CN201710457857A CN107190194A CN 107190194 A CN107190194 A CN 107190194A CN 201710457857 A CN201710457857 A CN 201710457857A CN 107190194 A CN107190194 A CN 107190194A
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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
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- 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
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
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- B22—CASTING; POWDER METALLURGY
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Abstract
Preparing boride ceramic particles the invention discloses a kind of vacuum heating-press sintering strengthens the method for niobium molybdenum-base composite material, and this method comprises 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), by the mixed-powder vacuum heating-press sintering, comprise the following steps that：(1) it is pressed into tire base；(2) dry；(3) sintered in dynamic vacuum；(4) maximum sintering temperature is up to 2600 DEG C, and heating rate is 40 95 DEG C/min；(5) mixed-powder is pressurizeed in sintering process；(6) speed adjust is will heat up after the pressurizing for 40 50 DEG C/min, is raised in-furnace temperature, is made pressure rise；(7) closing presure machine, closes heating power supply, and 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
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of vacuum heating-press sintering prepares boride ceramics
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 class high-performance advanced material.
Ceramic material has the advantages that corrosion resistance is good, wear-resisting, but fragility is larger and not easy processing；Metal material has excellent
Ductility, but wear-resisting, anti-corrosion, heat-resisting quantity is poor.Particles reiforced metal-base composition has taken into account the heat-resisting quantity of ceramics
The good toughness with metal, with single ceramics or the incomparable excellent properties of metal material, in Aeronautics and Astronautics, automobile etc.
Field has a good application prospect.
In ceramic material system, compound (such as ZrB that refractory metal is constituted with B, C2、ZrC、TaC、HfB2Etc. superhigh temperature
Ceramics) fusing point more than 3000 DEG C, the excellent thermo-chemical stability of these compounds is allowed them to as extreme environment
The candidate material used.There is the problem of antioxygenic property is poor in carbide and nitride ceramics, so oxidation resistant
Boride ceramics and its composite turn into the emphasis of research.Since eighties of last century sixties, ZrB is just carried out both at home and abroad2
The research of based ultra-high temperature ceramics (its target temperature in use is up to more than 2000 DEG C).Due to ZrB2Ceramics fusing point is high and Zr
Self-diffusion coefficient with B atoms is low, so as to pass through the fine and close ZrB of direct sintering2It is more difficult.Research shows, by mixing carbon
The sintering aids such as compound, silicide, nitride and rare metal oxide can prepare comparatively dense ZrB2Based ultra-high temperature is made pottery
Porcelain.ZrB2Antioxygenic property (the ZrB that ceramics have had at 1100 DEG C2B is formed after oxidation2O3Diaphragm), and temperature is higher than
At 1100 DEG C, B2O3Volatilize and lose protective effect.The method of current comparative maturity is by ZrB2It is compound with SiC, make it 1200
DEG C and form SiO during temperatures above2Diaphragm, so that by ZrB2The antioxygenic property of-SiC composite ceramicses brings up to 1800 DEG C.
Although having been carried out years of researches both at home and abroad, ZrB2The ceramic fracture toughness of based ultra-high temperature is poor, heat resistanceheat resistant punching
Hit the problem of performance is weaker and never have and effectively solved, which greatly limits ZrB2Based ultra-high temperature is ceramic to answer
Use scope.
Refractory metal and its alloy have the advantages that fusing point height, elevated temperature strength are high, and its temperature in use >=1100 DEG C is 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 its is main
Shortcoming is that high-temperature creep resistance and inoxidizability are poor.Nb-Mo, Nb-W, Nb-Ta etc. are unlimited solid solution alloy, in the absence of high-temperature-phase
The problems such as becoming or generate brittlement phase, therefore, it is the elevated temperature strength for improving niobium-base alloy that a certain proportion of W, Mo, Ta are added in Nb
One of with the effective way of croop property.
The shortcomings of there is black brittleness, welding fragility, processing difficulties and poor high temperature oxidation resistance due to molybdenum alloy, it is applied
Scope is restricted.
Ceramic particle enhancing refractory metal based composites, which are directed to introduce appropriate second in refractory metal basal body, mutually to be increased
Strong particle, its advantage is：(1) ceramic particle strengthens superhigh temperature intensity, the superhigh temperature croop property of refractory metal based composites
It is significantly higher than refractory alloy；(2) high temperature and superhigh temperature fracture toughness of ceramic particle enhancing refractory metal based composites 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 strengthens refractory metal based composites, then has that composite consistency is low and the low problem of elevated temperature strength.Current state
The inside and outside research for strengthening refractory metal based composites to boride ceramic particles is also extremely limited.Therefore, tissue is prepared equal
Even, high-compactness boride ceramic particles enhancing niobium molybdenum-base composite material is technological difficulties at this stage.
The content of the invention
It is an object of the present invention to which proposing a kind of new boride ceramic particles strengthens the composition of niobium molybdenum-base composite material
And preparation method, solve niobium-base alloy, molybdenum-base alloy and acutely decline problem in 1100 DEG C of temperatures above intensity, the composite
There is higher intensity under≤1800 DEG C of hyperthermal environments, be a kind of new ceramics that can be used under hyperthermal environments
Particle strengthens refractory metal based composites.Technical scheme is as follows：
A kind of boride ceramic particles strengthen the preparation method of niobium molybdenum-base composite material, comprise 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, ZrB2The mesh of powder 600, purity >=99.95%：Nb powder
500-800 mesh, purity >=99.95%：Mo powder 500-800 mesh, purity >=99.95%.
The powder of said ratio is put into drying box and dried 3 hours under the conditions of temperature is 110 DEG C, planet is then placed in
Mixed in formula ball mill, drum's speed of rotation is 180-220rpm, powder mixing is obtained into composition 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, is concretely comprised the following steps：
(1) mixed-powder is placed in pre-fabricated mould, 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, and drying time is 45-60
Minute；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vavuum pump, when vavuum pump registration is -0.15~-0.1MPa, is passed through argon gas, air pressure in stove is kept
In -0.09~-0.07MPa dynamic vacuum, and untill 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 to tire base pressure sintering, press ram
For 25-30MPa, the soaking time to tire base at a temperature of 1700-1900 DEG C is 15-30 minutes；
(6) continue to high temperature stove heat, heating ramp rate is 40-50 DEG C/min, measuring point temperature in stove is risen to 2400-
2600℃；Mechanical press is adjusted, makes pressure rise to 50MPa, is incubated 10-15 minutes；
(7) closing presure machine, closes heating power supply, and 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, its remarkable advantage is the present invention：(1) prepared using vacuum high-frequency sensing super high sintering temperature method
Boride ceramic particles strengthen niobium molybdenum-base composite material, and the experiment condition of HTHP can melt whole metal phase and part
Ceramic phase, passes through composition design and preparation technology, the ZrB of addition2Synthesized with Nb, Mo reaction and contained Nb3B2With NbB complex phase boron
The enhanced composite of compound ceramics；(2) compression strength of the composite 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 strengthens the intensity of composite at the same temperature；(3) the highest consistency of the composite is more than 99%, wherein Nb3B2
Microhardness with NbB complex phase borides is 14-15GPa.
Brief description of the drawings
The high-frequency induction heating sintering furnace schematic diagram that Fig. 1 uses for the present invention.In figure：1- cylinder bodies, 2- pistons, 3- fire resistings
Plate, 4- fire resisting heaters, 5- moulds, 6- bodies of heater, 7- workbench, 8- argon gas pumps, 9- thermocouples, 10- vavuum 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 be ZrO in figure
Phase, 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 be ZrB in figure2
Phase, 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 be ZrB in figure2
Phase, 20 be Mo2Zr phases, 21 be Nb3B2It is 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.
Embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples.
Embodiment 1
Prepare ZrB2Mass fraction strengthens niobium molybdenum-base composite material for 22% boride ceramic particles：
Alloy powder and ceramic powder are weighed, boride is prepared using vacuum high-frequency induction heating ultra-temperature hot-pressed sintering furnace
Ceramic particle strengthens niobium molybdenum-base composite material.Dusty material is by ZrB2, the composition 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.
Concretely comprise the following steps：
(1) mixed-powder is placed in pre-fabricated mould, 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, drying time is 45 minutes；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vavuum pump, when vavuum pump registration is -0.1MPa, be passed through argon gas, air pressure in stove is maintained at -
In 0.08MPa dynamic vacuum, and untill 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, start 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) continue to high temperature stove heat, heating ramp rate is 47 DEG C/min, measuring point temperature in stove is risen to 2500 DEG C,
Make mechanical press pressure rise to 50MPa, be incubated 10 minutes；
(7) closing presure machine, closes heating power supply, and 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 prepared be high cylindrical shape, its a diameter of 14mm, highly be 100mm.Fig. 2 is ZrB2Mass fraction
For the stereoscan photograph of 22% niobium molybdenum-base composite material, obvious element segregation, even tissue and crystal grain are not present in figure
Tiny, ZrO phases play a part 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 ZrO phases dispersion-strengthened action and metallic atom solution strengthening effect collective effect,
The compressive strength at room temperature of composite may be up to 1403MPa, far above pure niobium base or the ceramic particle reinforcing material of pure molybdenum base.
Embodiment 2
Prepare ZrB2Mass fraction strengthens niobium molybdenum-base composite material for 35% boride ceramic particles：
Alloy powder and ceramic powder are weighed, boride is prepared using vacuum high-frequency induction heating ultra-temperature hot-pressed sintering furnace
Ceramic particle strengthens niobium molybdenum-base composite material.Dusty material is by ZrB2, the composition 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.
Concretely comprise the following steps：
(1) mixed-powder is placed in pre-fabricated mould, 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, drying time is 55 minutes；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vavuum pump, when vavuum pump registration is -0.15MPa, be passed through argon gas, air pressure in stove is maintained at -
In 0.07MPa dynamic vacuum, and untill 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, start 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) continue to high temperature stove heat, heating ramp rate is 47 DEG C/min, measuring point temperature in stove is risen to 2600 DEG C,
Make mechanical press pressure rise to 50MPa, be incubated 15 minutes；
(7) closing presure machine, closes heating power supply, and 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 prepared is short cylindrical shape, and its 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 a part of dispersion-strengtherning, Nb3B2Phase it is hard
Degree can reach 11.4GPa, and the intensity to raising composite is helpful, and the presence of niobium molybdenum solid solution confirms that solution strengthening is imitated
Should, it can further lift the intensity of composite.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 is that the compression strength at 1202MPa, 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 ZrB2Mass fraction strengthens niobium molybdenum-base composite material for 50% boride ceramic particles：
Alloy powder and ceramic powder are weighed, boride is prepared using vacuum high-frequency induction heating ultra-temperature hot-pressed sintering furnace
Ceramic particle strengthens niobium molybdenum-base composite material.Dusty material is by ZrB2, the composition 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.
Concretely comprise the following steps：
(1) mixed-powder is placed in pre-fabricated mould, 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, drying time is 60 minutes；
(3) the tire base after drying is placed in carbon fiber crucible, prepares to fire；
(4) start vavuum pump, when vavuum pump registration is -0.12MPa, be passed through argon gas, air pressure in stove is maintained at -
In 0.09MPa dynamic vacuum, and untill 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, start 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) continue to high temperature stove heat, heating ramp rate is 40 DEG C/min, measuring point temperature in stove is risen to 2400 DEG C,
Make mechanical press pressure rise to 50MPa, be incubated 10 minutes；
(7) closing presure machine, closes heating power supply, and 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 prepared is short cylindrical shape, and its 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 a part of dispersion-strengtherning, Nb3B2It is multiple 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 is 1636MPa,
Compression strength at 1300 DEG C is that the compression strength at 642MPa, 1700 DEG C is 144MPa, far above pure niobium base or pure molybdenum base
Ceramic particle reinforcing material.
Technical scheme is described in detail above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiment in the present invention, those skilled in the art can also make a variety of changes accordingly, but appoint
What is equal with the present invention or similar change belongs to the scope of protection of the invention.
Claims (7)
1. a kind of boride ceramic particles strengthen the preparation method of niobium molybdenum-base composite material, it is characterised in that step is as follows：
1) mixed-powder, is prepared
The powder includes ZrB215-50wt%, Nb25-51wt% and Mo surplus；The weight ratio of wherein Nb powder and Mo powder is 1-
1.5；By the powder dry mixed；
2), vacuum heating-press sintering, is comprised the following steps that：
(1) mixed-powder is placed in prefabricated mould, is pressed into tire base；
(2) the tire base suppressed is dried；
(3) the tire base after drying is placed in carbon fiber crucible, sintered in dynamic vacuum；
(4) maximum sintering temperature is up to 2600 DEG C, and heating rate is 40-95 DEG C/min；
(5) mixed-powder is pressurizeed in sintering process；
(6) speed adjust is will heat up after the pressurizing for 40-50 DEG C/min, is raised in-furnace temperature, is made pressure rise；
(7) closing presure machine, closes heating power supply, and the temperature of sintering furnace is down to room temperature by natural Slow cooling, and rate of temperature fall is
10-50℃/min。
2. method according to claim 1, it is characterised in that step 1) described in powder, ZrB2The mesh of powder 600, 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, it is characterised in that step 2) described in the pressure of compacting tire base be 25-30MPa.
4. method according to claim 1, it is characterised in that step 2) described in drying temperature be 250-300 DEG C, during drying
Between be 45-60 minutes.
5. method according to claim 1, it is characterised in that step 2) described in dynamic vacuum be -0.09~-0.07MPa,
When vavuum pump registration is -0.15~-0.1MPa, argon gas is passed through.
6. method according to claim 1, it is characterised in that step 2) described in sintering process, temperature rises to 1700-
At 1900 DEG C, tire base is pressurizeed, pressure is 25-30MPa, and be incubated 15-30 minutes at this temperature.
7. method according to claim 1, it is characterised in that step 2) in the follow-up temperature of continuing rising of pressurization make pressure rise extremely
50MPa, 10-15 minutes are incubated at 2400-2600 DEG C.
Priority Applications (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111979464A (en) * | 2020-08-28 | 2020-11-24 | 南京航空航天大学 | Mo with dual-scale dual-form hard phase crystal grains2FeB2Base cermet and method for preparing same |
| CN116179883A (en) * | 2022-12-28 | 2023-05-30 | 吉林大学 | Nanometer NbB 2 Preparation method of particle reinforced NiAl alloy |
| CN116179884A (en) * | 2022-12-28 | 2023-05-30 | 吉林大学 | Vacuum induction smelting method for preparing titanium-coated NbB 2 Method for reinforcing TiAl alloy by nano particles |
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| WO2005047181A2 (en) * | 2003-06-03 | 2005-05-26 | Seldon Technologies, Llc | Fused nanostructure material |
| CN103981385A (en) * | 2014-05-29 | 2014-08-13 | 西北有色金属研究院 | Method for preparing molybdenum-chromium-zirconium boride composite material |
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| JPS5451465A (en) * | 1977-09-30 | 1979-04-23 | Denki Kagaku Kogyo Kk | Method of producing thermionic emission material |
| WO2005047181A2 (en) * | 2003-06-03 | 2005-05-26 | Seldon Technologies, Llc | Fused nanostructure material |
| CN103981385A (en) * | 2014-05-29 | 2014-08-13 | 西北有色金属研究院 | Method for preparing molybdenum-chromium-zirconium boride composite material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111979464A (en) * | 2020-08-28 | 2020-11-24 | 南京航空航天大学 | Mo with dual-scale dual-form hard phase crystal grains2FeB2Base cermet and method for preparing same |
| CN111979464B (en) * | 2020-08-28 | 2021-11-05 | 南京航空航天大学 | Mo with dual-scale dual-form hard phase crystal grains2FeB2Base cermet and method for preparing same |
| CN116179883A (en) * | 2022-12-28 | 2023-05-30 | 吉林大学 | Nanometer NbB 2 Preparation method of particle reinforced NiAl alloy |
| CN116179884A (en) * | 2022-12-28 | 2023-05-30 | 吉林大学 | Vacuum induction smelting method for preparing titanium-coated NbB 2 Method for reinforcing TiAl alloy by nano particles |
| CN116179883B (en) * | 2022-12-28 | 2024-06-25 | 吉林大学 | Nanometer NbB2Preparation method of particle reinforced NiAl alloy |
| CN116179884B (en) * | 2022-12-28 | 2024-06-25 | 吉林大学 | Vacuum induction smelting method for preparing titanium-coated NbB2Method for reinforcing TiAl alloy by nano particles |
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