CN105886821B - A kind of gradient of porosity consecutive variations POROUS TUNGSTEN base and preparation method - Google Patents
A kind of gradient of porosity consecutive variations POROUS TUNGSTEN base and preparation method Download PDFInfo
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- CN105886821B CN105886821B CN201610381906.1A CN201610381906A CN105886821B CN 105886821 B CN105886821 B CN 105886821B CN 201610381906 A CN201610381906 A CN 201610381906A CN 105886821 B CN105886821 B CN 105886821B
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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
- C22C1/08—Alloys with open or closed pores
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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
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1143—Making porous workpieces or articles involving an oxidation, reduction or reaction step
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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
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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
Abstract
A kind of gradient of porosity consecutive variations POROUS TUNGSTEN base and preparation method, belong to powder metallurgical technology.In the POROUS TUNGSTEN base, porosity is from high to low from surface to internal distribution gradient, porosity consecutive variations.Its preparation method, it is to be placed in relative density in the inert atmosphere containing steam for 55 85% POROUS TUNGSTEN blank, pass through high-temperature oxydation gasification process of the steam to tungsten constituent element, by tungsten constituent element volatilization effusion POROUS TUNGSTEN blank, pore-creating is realized, the POROUS TUNGSTEN crude green body of gradient of porosity consecutive variations is obtained, after cooling, high temperature reduction is carried out again, obtains the POROUS TUNGSTEN base of gradient of porosity consecutive variations.Present invention process is simple and convenient to operate, flow is short, environment-friendly；It is expected to solve the problems, such as the preparation of the more complicated continuous gradient tungsten copper tungsten alloy part of space geometry feature, is created conditions for manufacture continuous gradient tungsten-copper composite material.Suitable for industrial applications.
Description
Technical field
The present invention relates to a kind of POROUS TUNGSTEN base of gradient of porosity consecutive variations and preparation method, belong to PM technique
Field.
Background technology
Tungsten-copper composite material collects the highly thermally conductive and excellent machinability of high rigidity, high-melting-point and the copper of tungsten in one
Body, has wide application in electrical contact, machined electrode, Electronic Packaging and superhigh temperature (such as guided missile throat liner material) field.
For the tungsten-copper alloy of tungstenic amount (mass percent) more than 45% generally based on porous W skeleton, using the copper technology system of oozing
The tungsten-copper composite material of standby homogeneous.With the development of science and technology, such as the operating temperature of solid propellant engine of new generation
And pressure increase, high-temperature fuel gas washes away to rocket larynx lining with the increase of ablation ability, the amount of copper that existing tungsten copper throat liner material is carried compared with
Low, copper is greatly shortened from the sweating cooling effect working time, and service life is only the 2/3 of target life objective；With extensive collection
Into the development of circuit engineering, the power density of electronic device is increasingly improved, it is necessary to develop highly thermally conductive property, the tungsten of low thermal coefficient of expansion
Carbon/carbon-copper composite material；The nuclear fusion system of future source of energy demand effective way is solved as the mankind, towards high-temperature plasma
Layer material is adapted between plasma facing material pure tungsten and water cooling system copper alloy, should have excellent thermal conductivity and thermal expansion system
The tungsten-copper alloy of consecutive variations is counted to alleviate thermal stress therein.In above demand, answered using the tungsten copper of composition consecutive variations
Condensation material is optimal solution route.Particularly, served as a contrast as rocket larynx and be adapted to layer material with nuclear fusion system, due to space geometry
The complexity of shape, prior art, which builds composition continuous gradient, becomes very difficult.
At present, the tungsten copper gradient composites reported mostly use layered structure method-powder laying method, will difference contain
The tungsten copper powder mixture of amount of copper be successively seated in it is repressed in mould obtain tungsten copper powder pressed compact, then pass through different sintering
Technology prepares gradient tungsten-copper composite material.University of Science ＆ Technology, Beijing, Central South University, Wuhan University of Technology, HeFei University of Technology etc. are single
Position generally prepares block formula gradient tungsten-copper composite material using this kind of method.But the structure of this kind of composite is step gradient
Structure, it is difficult to meet the application needs for effectively alleviating high thermal stress under superhigh temperature service condition.Effectively alleviate hyperpyrexia to meet
The application demand of stress, composition is best-of-breed technology approach in continuously varying gradient tungsten-copper composite material.In order to manufacture continuous ladder
Tungsten-copper composite material is spent, hypergravity casting makes tungsten particle component in single side using the density variation between tungsten particle and copper liquid
Copper content continuously varying gradient tungsten-copper alloy is built to (i.e. gravity field direction).Freely filled out because tungsten particle component is nearly at
State is filled, the high continuous gradient tungsten-copper composite material of copper content, engineering application value very little can only be prepared.Profit has been invented by Germany
The POROUS TUNGSTEN base of porosity consecutive variations is prepared with the electrolytic attack method based on porous W skeleton, recycling oozes copper technology preparation
The technology of continuous gradient tungsten-copper composite material, but the efficiency of the technique construction gradient of porosity is very low, and generally time-consuming 180-240 is small
When.Meanwhile, the technology is there is also environmental pollution problem and the continuously distributed POROUS TUNGSTEN base of porosity can only be built in single direction.
The content of the invention
It is an object of the invention to the deficiency for overcoming prior art is simple and convenient to operate there is provided a kind of technique, flow is short,
The POROUS TUNGSTEN base and preparation method of environment-friendly gradient of porosity consecutive variations.Gradient of porosity prepared by the present invention continuously becomes
The POROUS TUNGSTEN base of change is from material surface to wood interior porosity consecutive variations, it is expected to solve the more complicated continuous ladder of space geometry feature
The preparation problem of tungsten copper tungsten alloy part is spent, is created conditions for manufacture continuous gradient tungsten-copper composite material.
During a kind of porosity of the present invention is in the POROUS TUNGSTEN base that continuous gradient changes, the POROUS TUNGSTEN base, porosity is from surface
To internal distribution gradient, porosity consecutive variations.
In the present invention in a kind of POROUS TUNGSTEN base of gradient of porosity change, the POROUS TUNGSTEN base, porosity from high to low, from
Surface is to internal distribution gradient, and porosity highest region is POROUS TUNGSTEN base surface region.
In the present invention in a kind of POROUS TUNGSTEN base of gradient of porosity change, the POROUS TUNGSTEN base, pore-size is at 5-38 μm
Continuous gradient distribution, gradient of porosity distributed areas thickness be 1.5-5mm.
A kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change of the present invention, by the tungsten that relative density is 55-85%
Powder pressed compact is placed in the inert atmosphere containing steam, and by high-temperature oxydation-gasification process of the steam to tungsten constituent element, tungsten constituent element is volatilized
Porous tungsten powder pressed compact is escaped, pore-creating is realized, the POROUS TUNGSTEN crude green body of gradient of porosity consecutive variations is obtained, after cooling, then height is carried out
Temperature reduction, obtains the POROUS TUNGSTEN base of gradient of porosity consecutive variations.
A kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change of the present invention, the gas of inert atmosphere is selected from argon or nitrogen
Gas.
A kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change of the present invention, the high-temperature oxydation-gasification process work
Skill parameter is：870-1100 DEG C of temperature, soaking time 1.5-3 hours.
A kind of preparation method of the POROUS TUNGSTEN base of present invention gradient of porosity change, high temperature reduction technological parameter is：Temperature
870-920 DEG C, soaking time 1-1.5 hours, reducing atmosphere：Hydrogen.
A kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change of the present invention, POROUS TUNGSTEN blank uses granularity for 2-5 μ
The tungsten powder of m tungsten powder and 7-10 μm of m, in mass ratio 1：2.3-1:3 are well mixed, and are pressed into the base that relative density is 55-85%
Material.
In a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change of the present invention, the POROUS TUNGSTEN base prepared, hole
Gap size is distributed in 5-38 μm of continuous gradient, and gradient of porosity distributed areas thickness is 1.5-5mm.
Principle and advantage
The present invention devises the POROUS TUNGSTEN base that porosity is distributed from material surface to inner gradient；By containing the lazy of steam
Property atmosphere (argon gas or nitrogen) under, in 870-1100 DEG C of temperature range, utilize hydrone and tungsten powder particles in POROUS TUNGSTEN pressed compact
The oxide of oxidation reaction generation tungsten and then hydrone react tungsten oxygen of the generation with developability with established tungsten oxide
The hydrate of compound is the gasification of tungsten constituent element, tungsten constituent element is escaped POROUS TUNGSTEN base and pore-creating.Due to the oxidation of above-mentioned tungsten component, tungsten oxygen
The hydrate of compound is progressively promoted from POROUS TUNGSTEN base surface to material internal, therefore, by regulating and controlling tungsten constituent element in POROUS TUNGSTEN blank
Oxidation-volatilization treatment conditions and tungsten powder particles size, can regulate and control the size of porosity, porosity continuously varying gradient,
And the thickness of gradient of porosity distributed areas, it can form that surface region porosity is high effectively in POROUS TUNGSTEN base and material internal
The POROUS TUNGSTEN base for the continuous porosity graded that porosity is gradually reduced.Meanwhile, it is several that the present invention can effectively build space
What more complicated porosity continuously varying gradient POROUS TUNGSTEN base of shape, is combined to prepare the more complicated continuous gradient tungsten copper of shape
Material creates condition.
Brief description of the drawings
Accompanying drawing 1 is the porosity distribution map of the POROUS TUNGSTEN base of gradient of porosity consecutive variations prepared by the embodiment of the present invention 1.
Accompanying drawing 2 is the porosity distribution map of the POROUS TUNGSTEN base of gradient of porosity consecutive variations prepared by the embodiment of the present invention 2.
It can be seen that from accompanying drawing 1：In the space away from surface 3mm, porosity is continuously reduced to from 24.7% in top layer
The 8.05% of core area.
It can be seen that from accompanying drawing 2：In the space away from surface 1.5mm, porosity is from 31.4% continuous reduction in top layer
To the 25.3% of core area.
Embodiment
In the POROUS TUNGSTEN base of gradient of porosity consecutive variations prepared by the embodiment of the present invention, porosity is using quantitative metallography point
Analysis method is determined.Pore size is measured using metallographic wire cutting method.
Embodiment 1：The high temperature preparation of the POROUS TUNGSTEN base of gradient of porosity consecutive variations
The tungsten powder of 5 microns of 10 microns of tungsten powder of 70% (mass fraction) and 30% (mass fraction) is mixed in ball mill
Close 6-8 hours, then mixing tungsten powder is loaded gum cover and carries out isostatic cool pressing processing in 300MPa, pressed compact relative density is
57%.Tungsten powder pressed compact is placed in the electric tube furnace of flowing nitrogen to the oxidation-gasification process for carrying out tungsten.In order to realize tungsten constituent element
Oxidation-gasification process effect, is first passed through in aqueous surge flask before nitrogen enters electric tube furnace and is humidified.In 970 DEG C of tungsten constituent elements
Handled 1.5 hours through " oxidation-gasification ", furnace cooling.Reduced 1 hour in high-purity hydrogen at 900 DEG C again.It is last to lead to hydrogen
Sintered 3 hours in 2200 degrees Celsius in intermediate frequency furnace, furnace cooling.The distribution of POROUS TUNGSTEN base porosity gradient is as shown in Figure 1.
It can be found that the porosity in POROUS TUNGSTEN base is distributed in continuous gradient from Fig. 1, pore-size scope is 12-38 μm.
Embodiment 2：The normal temperature preparation of the POROUS TUNGSTEN base of gradient of porosity consecutive variations
First by 5 microns of tungsten powders of 10 microns of tungsten powder of 60% (mass fraction) and 40% (mass fraction) in ball mill
Mixing 6-8 hours.In 600-650MPa Forming under Pressure bulk samples, pressed compact relative density is 78%.Tungsten powder pressed compact is placed in
Oxidation-gasification process of tungsten is carried out in the electric tube furnace of flowing nitrogen.In order to realize oxidation-gasification process effect of tungsten constituent element,
First it is passed through in aqueous surge flask and is humidified before nitrogen enters electric tube furnace.In 870 DEG C of tungsten constituent elements through " oxidation-gasification " processing 2
Hour, furnace cooling.Reduced 1 hour in high-purity hydrogen at 920 DEG C again.The distribution of POROUS TUNGSTEN base porosity is as shown in Figure 2.From figure
2 as can be seen that POROUS TUNGSTEN base porosity is distributed in continuous gradient, and pore-size scope is 5-30 μm.
Claims (6)
1. a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change, is the POROUS TUNGSTEN blank by relative density for 55-85%
It is placed in the inert atmosphere containing steam, it is by high-temperature oxydation-gasification process of the steam to tungsten constituent element, the volatilization effusion of tungsten constituent element is more
Hole tungsten blank, realizes pore-creating, obtains the POROUS TUNGSTEN crude green body of gradient of porosity consecutive variations, after cooling, then carries out high temperature reduction, obtains
To the POROUS TUNGSTEN base of gradient of porosity consecutive variations.
2. a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change according to claim 1, it is characterised in that：It is lazy
Property atmosphere gas be selected from argon or nitrogen.
3. a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change according to claim 1, it is characterised in that：Institute
Stating high-temperature oxydation-gasification process technological parameter is：870-1100 DEG C of temperature, soaking time 1.5-3 hours.
4. a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change according to claim 1, it is characterised in that：It is high
Warm reducing process parameter is：870-920 DEG C of temperature, soaking time 1-1.5 hours, reducing atmosphere：Hydrogen.
5. a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change according to claim 1, it is characterised in that：It is many
Hole tungsten blank uses granularity for 2-5 μm of tungsten powder and 7-10 μm of tungsten powder, and in mass ratio 1：2.3 -1：3 are well mixed, and are pressed into
Relative density is 55-85% blank.
6. a kind of preparation method of the POROUS TUNGSTEN base of gradient of porosity change according to claim 1-5 any one, its
It is characterised by：In the POROUS TUNGSTEN base prepared, porosity is from high to low, from surface to internal distribution gradient, and porosity connects
Continuous change；Pore-size is distributed in 5-38 μm of continuous gradient, and gradient of porosity distributed areas thickness is 1.5-5mm.
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| CN106475563B (en) * | 2016-10-31 | 2018-05-11 | 西北有色金属研究院 | A kind of gradient tungsten-copper composite material and preparation method thereof |
| CN107200583B (en) * | 2017-05-26 | 2019-11-08 | 哈尔滨工业大学 | A kind of porous material and preparation method thereof with porosity continuous gradient |
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| JP4242716B2 (en) * | 2003-06-30 | 2009-03-25 | 本田技研工業株式会社 | Manufacturing method of inclined composite material |
| CN100451144C (en) * | 2006-12-25 | 2009-01-14 | 华南理工大学 | Method for preparing shape memory nickel titanium alloy with gradient porosity |
| CN100482821C (en) * | 2007-07-13 | 2009-04-29 | 东南大学 | Method for preparing foam aluminum and alloy product with closed gradient pore structure |
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