CN108188390A - A kind of method for preparing pure tungsten metal part - Google Patents
A kind of method for preparing pure tungsten metal part Download PDFInfo
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- CN108188390A CN108188390A CN201810107384.5A CN201810107384A CN108188390A CN 108188390 A CN108188390 A CN 108188390A CN 201810107384 A CN201810107384 A CN 201810107384A CN 108188390 A CN108188390 A CN 108188390A
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- tungsten
- tungsten powder
- vibration
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- tungsten metal
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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
- B22F3/02—Compacting only
- B22F3/093—Compacting only using vibrations or friction
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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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F3/02—Compacting only
- B22F2003/026—Mold wall lubrication or article surface lubrication
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to a kind of methods of standby pure tungsten metal part, this method first applies vibration using the tungsten powder of certain particle size, improve its initial relative density and then be molded and low temperature sintering method the more highdensity ultra-high purity metal part of high-temperature sintering method has been made.Low energy consumption for the method for the present invention, and the tungsten metal parts of preparation is finer and close, performance higher.
Description
Technical field
The present invention relates to a kind of methods for preparing pure tungsten metal part, belong to intermetallic composite coating preparing technical field.
Background technology
Tungsten is a kind of refractory metal, have fusing point is high, technology is high, density is high, thermal conductivity is high, intensity is high, the coefficient of expansion is low,
The characteristics such as resistance to corrosion height are widely used in the necks such as aerospace, electronic information, the energy, chemical industry, metallurgy and nuclear industry
Domain.But due to its hardness is big, poor toughness, be easily broken off the shortcomings that cause pure tungsten metal be difficult to fine and close forming, forming after defect it is more.
From the point of view of the existing method for preparing pure tungsten metal part, mostly using forming agent is added in powder metallurgy, first unidirectionally
After die forming, prepared by the method being sintered again after degumming, but the sintering temperature used by it is high, as at 2300 DEG C into
Row high temperature sintering wastes a large amount of energy and cost；The single way stempressing of use is directly to be suppressed with pine dress accumulation, is obtained
Pressure embryo relative density it is small, easily generate defect；In order to make the crystal grain of pure tungsten part more tiny, as used in most of method
Tiny powder is suppressed and is sintered, but reduces the consistency of pure tungsten metal so as to cause under the quality of pure tungsten metal
Drop.In addition, preparing pure tungsten metal using tungsten powder sintering, there is bottleneck in the pure tungsten metal for how obtaining high densification, current
Processing method is not broken through always.
Invention content
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of method for preparing tungsten metal parts, this method
Energy consumption and cost waste are reduced, improves the consistency of pure tungsten metal.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
A kind of method for preparing tungsten metal parts, includes the following steps：
S1, feeding：Average grain diameter is referred to as 10~25 μm of tungsten powder, adds in absolute ethyl alcohol and is uniformly mixed, makes the tungsten powder table
Face generates the state moistened slightly；
S2, vibration：It is vibrated after the step S1 tungsten powders obtained are put into molding die；
S3, single way stempressing：Molding die after step S2 is vibrated carries out single way stempressing, takes out briquetting later；
S4, sintering：Briquetting described in step S3 is sintered, leads to Ar gas shieldeds, is first warming up to 80 DEG C of heat preservation removal nothings
Water-ethanol, then be warming up to 1600~1800 DEG C and be sintered；To obtain pure tungsten metal part.
Method as described above, it is preferable that in step sl, the addition of the absolute ethyl alcohol, which is pressed in every gram of tungsten powder, to be added
The absolute ethyl alcohol of 0.4~0.7ml adds in.
Method as described above, it is preferable that in step s 2, the molding die inner wall is first coated into zinc stearate lubrication
Agent adds tungsten powder.
Zinc stearate lubricant is coated in molding die inner wall, to reduce the frictional force of tungsten powder and mold wall, facilitates pressure
Briquetting is taken out after system.
Method as described above, it is preferable that in step s 2, the amplitude of the vibration is 0.1~0.2mm, frequency 150
After~250rad/s, time of vibration is 2~5min.
Method as described above, it is preferable that in step s3, the pressure of the single way stempressing pressing force 200MPa per minute
After rising to 400~500MPa, 2~10min of pressurize is carried out.
Method as described above, it is preferable that in step s 4, the times of 80 DEG C of heat preservations for 15~25min, the burning
The knot time is 1.5~3h.
(3) advantageous effect
The beneficial effects of the invention are as follows：
The method that the present invention prepares tungsten metal parts using vibration, can improve the initial bulk density of tungsten powder, make product
It is finer and close；Using relatively low sintering temperature, the temperature being sintered than in the prior art reduces about 500-600 DEG C, substantially reduces
Energy consumption, makes cost reduction；The product of preparation has low cost, and high-compactness, relative density compares the prior art up to 98.7%
In raising 3.9%, available for preparing high performance part.
Description of the drawings
Fig. 1 is the preceding influence result with to pressing process after vibration of tungsten powder vibration that granularity is 10 μm；
Fig. 2 is the end face SEM figures in the pressed vibrationless pressure embryos of pressure 480MPa；
Fig. 3 is in the pressed end face SEM figures for pressing embryo for having vibration of pressure 480MPa；
Fig. 4 is influence result of the grain graininess to relative density in pressing process；
Fig. 5 is the influence result of grain graininess and sintering temperature to sintered density.
Specific embodiment
The present invention invention mechanism be：It using 10~25 μm of tungsten powder, can subtract the intermolecular force between tungsten powder
It is small, so as to obtain finer and close structure；Vibrating step is added in, the initial bulk density of tungsten powder can be improved, so as to make compacting
Pressure embryo and sintered product or part afterwards is finer and close；Pressure can be improved by being sintered using 1600-1800 DEG C of temperature
The intensity of embryo reduces the residual stress of pressure embryo.The method of the present invention reduces the energy consumption needed for reaction, reduces cost, and technique is broken through
It is insoluble always to prepare pure tungsten metal using tungsten powder sintering, obtain high fine and close pure tungsten metal problem.
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by specific embodiment, to this hair
It is bright to be described in detail.
Embodiment 1
A kind of method for preparing tungsten metal parts, the present embodiment mainly illustrate apply vibration influence using following steps into
Row：
(1) 10 μm of tungsten powder of the quality such as 12 parts is taken, the amount that 5ml absolute ethyl alcohols are added in by every 10g tungsten powders adds in, and mixing is equal
State even, that tungsten powder surface generation is made to moisten slightly；
(2) by after above-mentioned 12 parts of tungsten powders mixing absolute ethyl alcohol, it is respectively put into the cylinder that inner wall is coated with zinc stearate lubricant
In shape mold (a diameter of 20mm of mold).Wherein 6 parts do not apply vibration and are directly suppressed, and suppress, shake after 6 parts of application vibrations
Dynamic condition is that adjusting amplitude is 0.15mm, after frequency is 200rad/s, adds the 3min that shakes；It is shaken using three-dimensional vibrating equipment
Dynamic, which can be found in CN102950789A.Do not applied using tape measure vibrations and apply vibrations after tungsten powder in mold
In height after, calculate its relative density in 0MPa.Calculation formula is：ρ=m/ (π r2hρ0).Wherein, ρ --- relative density；
M --- the powder quality weighed；The radius of r --- mold；The height of h --- powder in a mold；ρ0--- briquetting after compacting
Density.
(3) apply vibration and do not apply 6 parts of tungsten powders of braking, the pressing pressure in compacting is respectively with 200MPa per minute
Pressure rise to pressurize 5min after 80MPa, 160MPa, 240MPa, 320MPa, 400MPa, 480MPa, then surveyed using drainage
The density of pressure embryo every time is measured, and is seen under scanning electron microscope after the tabletting that pressing pressure is 480MPa is carried out grind away, polished
It examines.Influence before tungsten powder vibration and after vibration to pressing process, the results are shown in Figure 1 for relative density, is pressed in pressure 480MPa
(Fig. 2) without friction after system and have vibration (Fig. 3) pressure embryo end face SEM figures as shown in Figures 2 and 3, as a result illustrate to apply and shake
It is dynamic, the relative density of pressure embryo can be effectively improved.
Embodiment 2
A kind of method for preparing tungsten metal parts, the present embodiment mainly illustrates the influence of particle size and temperature, including such as
Lower step：
(1) granularity for taking phase homogenous quantities is respectively 1 μm, 10 μm and 20 μm of tungsten powder, and it is anhydrous to add in 5ml by every 10g tungsten powders
The amount of ethyl alcohol adds in absolute ethyl alcohol, is uniformly mixed, the state that tungsten powder surface generation is made to moisten slightly；
(2) it vibrates：Zinc stearate lubricant is coated in molding die inner wall to reduce the frictional force side of tungsten powder and mold wall
Just briquetting is taken out after suppressing, tungsten powder is put into mold, is put on three dimensional vibration table fixed, adjusting amplitude 0.2mm, frequency is
After 250rad/s, add the 5min that shakes, the height of tungsten powder in a mold is measured using scale after vibrations, calculates it in no pressure
Relative density；
(3) single way stempressing：It is suppressed after applying vibration, the pressing pressure in compacting is respectively with 200MPa's per minute
Pressure rises to pressurize 5min after 100MPa, 200MPa, 300MPa, 400MPa, 500MPa, then measures pressure every time using drainage
The density of embryo, influence of the observation grain graininess to pressing process.
(4) it is sintered：The pressure embryo of 500MPa is put into sintering furnace and is passed through argon gas and is sintered, a sample is taken every 100 DEG C,
Measure relative density, the temperature range of sintering is 25-2300 DEG C, the sintering time of each sample for 1.5h observe grain graininess and
Influence of the sintering temperature to pure tungsten part.As a result as shown in Figure 4, Figure 5.Figure 4, it can be seen that the pressure embryo that granularity is 20 μm can be with
Obtain higher relative density.
As can be seen from Figure 5, when calcination temperature be 1500 DEG C after, just have very high consistency, particle is bigger, consistency with
Particle increases and increases.Can be obtained after 20 μm of particle compacting sintering relative density be 98.6% pure tungsten part, and 1 μm and
The pure tungsten part relative density that 10 μm of tungsten powder obtains is 98.1% and 98.3%, while when being sintered, when temperature is higher than 1700 DEG C
Consistency is almost unchanged afterwards, therefore selects 1700 DEG C of temperature.
Embodiment 3
(1) feeding：The tungsten powder that average grain diameter is 20 μm is weighed, the amount that 5ml absolute ethyl alcohols are added in by every 10g tungsten powders adds in)
Absolute ethyl alcohol is uniformly mixed, and surface is made to generate the state moistened slightly；
(2) it vibrates：Zinc stearate lubricant is coated in molding die inner wall to reduce the frictional force side of tungsten powder and mold wall
Just briquetting is taken out after suppressing, tungsten powder is put into mold, is put on three dimensional vibration table fixed, adjusting amplitude 0.15mm, frequency is
After 200rad/s, add the 3min that shakes；
(3) single way stempressing：The mold equipped with powder is put under forcing press after the completion of vibration, by the pressure of forcing press with every
After the pressure of minute 200MPa rises to 500MPa, briquetting is taken out after carrying out pressurize 5min；Wherein, 5min herein refers to
5min is kept under the pressure of 500MPa；
(4) it is sintered：The briquetting of taking-up is put into sintering furnace and is sintered, Ar gas shieldeds are led in sintering furnace, are first warming up to
80 DEG C of heat preservation 20min removal absolute ethyl alcohols, then it is warming up to 1700 DEG C of heat preservation 2h；So far pure tungsten metal part is obtained.It measures opposite
Density is 98.7%.
Comparative example
Using the prior art, specifically,
(1) feeding：The tungsten powder that average grain diameter is 1 μm is weighed, weighs 8% kerosene-rubber molding agent of tungsten powder quality, it will
Tungsten powder is uniformly mixed with binder；
(2) single way stempressing：Zinc stearate lubricant is coated in molding die inner wall to reduce the friction of tungsten powder and mold wall
Power takes out briquetting after facilitating compacting, uniformly mixed powder is put into after mold, mold is put under forcing press, by forcing press
After pressure rises to 500MPa with the pressure of 200MPa per minute, briquetting is taken out after carrying out pressurize 5min；
(4) it is sintered：The briquetting of taking-up is put into sintering furnace and is sintered, Ar gas shieldeds are led in sintering furnace, are first warming up to
800 DEG C of heat preservation 1h carry out degumming process, then are warming up to 2300 DEG C of heat preservation 2h；So far pure tungsten metal part is obtained.It measures relatively close
Spend is 94.8%.
The above described is only a preferred embodiment of the present invention, being not the limitation that other forms are done to the present invention, appoint
What those skilled in the art can be changed or be modified as the equivalence enforcement of equivalent variations using technology contents disclosed above
Example.But it is every without departing from technical solution of the present invention content, technical spirit according to the present invention is appointed to what above example was made
What simple modification, equivalent variations and remodeling still falls within the protection domain of technical solution of the present invention.
Claims (6)
- A kind of 1. method for preparing tungsten metal parts, which is characterized in that it includes the following steps：S1, feeding：Average grain diameter is referred to as 10~25 μm of tungsten powder, adds in absolute ethyl alcohol and is uniformly mixed, produces the tungsten powder surface The raw state moistened slightly；S2, vibration：It is vibrated after the step S1 tungsten powders obtained are put into molding die；S3, single way stempressing：Molding die after step S2 is vibrated carries out single way stempressing, takes out briquetting later；S4, sintering：Briquetting described in step S3 is sintered, leads to Ar gas shieldeds, 80 DEG C of heat preservations is first warming up to and removes anhydrous second Alcohol, then be warming up to 1600~1800 DEG C and be sintered；To obtain pure tungsten metal part.
- 2. the method as described in claim 1, which is characterized in that in step sl, the addition of the absolute ethyl alcohol presses every gram In tungsten powder plus the absolute ethyl alcohol of 0.5ml adds in.
- 3. the method as described in claim 1, which is characterized in that in step s 2, first coat the molding die inner wall firmly Resin acid zinc lubricant, adds tungsten powder.
- 4. the method as described in claim 1, which is characterized in that in step s 2, the amplitude of the vibration is 0.1~0.2mm, After frequency is 150~250rad/s, time of vibration is 2~5min.
- 5. the method as described in claim 1, which is characterized in that in step s3, the single way stempressing pressing force is per minute After the pressure of 200MPa rises to 400~500MPa, 2~10min of pressurize is carried out.
- 6. the method as described in any one of claim 1-5, which is characterized in that in step s 4, it is described 80 DEG C heat preservation when Between for 15~25min, the sintering time is 1~3h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810107384.5A CN108188390B (en) | 2018-02-02 | 2018-02-02 | Method for preparing pure tungsten metal part |
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| CN201810107384.5A CN108188390B (en) | 2018-02-02 | 2018-02-02 | Method for preparing pure tungsten metal part |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105163A (en) * | 1985-07-04 | 1986-12-31 | 中南工业大学 | The production method of compacting and sintered tungsten goods |
| JPS62196302A (en) * | 1986-02-21 | 1987-08-29 | Nippon Mining Co Ltd | Press molding method for high-purity tungsten powder |
| CN104785781A (en) * | 2014-01-22 | 2015-07-22 | 株洲佳邦难熔金属有限公司 | Method for manufacturing thin tungsten sheet blank capable of being rolled |
| CN106683914A (en) * | 2017-02-25 | 2017-05-17 | 河北工业大学 | Copper-based electrical contact material used for low-voltage electric appliance and preparation method for copper-based electrical contact material |
| CN106984808A (en) * | 2017-04-10 | 2017-07-28 | 四川理工学院 | A kind of localization strengthens the method for preparing powder metallurgy of composite |
| CN107008905A (en) * | 2017-02-25 | 2017-08-04 | 河北工业大学 | The preparation method of TiNiCu marmem based damping composite materials |
-
2018
- 2018-02-02 CN CN201810107384.5A patent/CN108188390B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105163A (en) * | 1985-07-04 | 1986-12-31 | 中南工业大学 | The production method of compacting and sintered tungsten goods |
| JPS62196302A (en) * | 1986-02-21 | 1987-08-29 | Nippon Mining Co Ltd | Press molding method for high-purity tungsten powder |
| CN104785781A (en) * | 2014-01-22 | 2015-07-22 | 株洲佳邦难熔金属有限公司 | Method for manufacturing thin tungsten sheet blank capable of being rolled |
| CN106683914A (en) * | 2017-02-25 | 2017-05-17 | 河北工业大学 | Copper-based electrical contact material used for low-voltage electric appliance and preparation method for copper-based electrical contact material |
| CN107008905A (en) * | 2017-02-25 | 2017-08-04 | 河北工业大学 | The preparation method of TiNiCu marmem based damping composite materials |
| CN106984808A (en) * | 2017-04-10 | 2017-07-28 | 四川理工学院 | A kind of localization strengthens the method for preparing powder metallurgy of composite |
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