CN107363258A - A kind of preparation method of high compactness tungsten-copper functional gradient material - Google Patents
A kind of preparation method of high compactness tungsten-copper functional gradient material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high compactness tungsten-copper functional gradient material, belong to material engineering field.The present invention mixes after peach gum ball milling is sieved first with deionized water, coagulant liquid must be disperseed, copper powder, tungsten powder and dispersion gel liquid are mixed again, ultrasonic disperse obtains dispersion liquid, is placed in after dispersion liquid is spray-dried in mould, and cold pressing treatment must be cold-pressed blank, calcining is incubated after pre-burning, standing is cooled to room temperature, obtains sintering feed and ball milling sieving, obtains combining powder；Weigh the powder such as 200 mesh tungsten powders, 300 mesh tungsten powders, 500 mesh tungsten powders, combining powder respectively again, each powder is laid into graphite hot pressing die, is placed in hot-pressed sintering furnace, is calcined after pre-burning, cooling.Tungsten-copper functional gradient material densification degree prepared by the present invention is high, and microstructure is uniform, can be widely applied in the high-tech areas such as Aero-Space, nuclear industry and electronics industry.
Description
Technical field
The present invention relates to a kind of preparation method of high compactness tungsten-copper functional gradient material, belong to material engineering field.
Background technology
The equally distributed neither solid solution of two-phase that tungsten-copper composite material is made up of tungsten and copper does not form compound again
A kind of composite, have high-melting-point, electrical erosion resistance, resistance fusion welding and the elevated temperature strength of tungsten and high conductivity, the high heat conduction of copper concurrently
Property, plasticity and workability, and can absorb a large amount of arc energies when copper evaporates under high arc temperature, reduce arc temperature, change
Kind use condition and reduction galvanic action.Because tungsten-carbon/carbon-copper composite material has the above advantage, therefore, touched earliest as electricity
Head and electrode material application, and more and more as jet pipe throat lining, electron beam target etc. be applied to Aero-Space, nuclear industry and
In the high-tech areas such as electronics industry.With the expansion of application, while the also Burning corrosion resistance to Tungsten-copper Composites, thermal shock resistance
Requirements at the higher level are proposed etc. performance.Especially in some special occasions, it is desirable to the one side of material will can bear very high temperature with
And the bombardment of particle, and another side needs to force cooling.Current this kind of material is mainly combined by W and Cu directly welding.But
It is due to that the physical property of tungsten and copper has a long way to go, usually causes due to thermal stress the knot in tungsten side or W and Cu in use
Cracked on conjunction face, simple tungsten-carbon/carbon-copper composite material can not meet to apply, and the concept of functionally gradient material (FGM) is considered as to solve
One of best approach of this problem.
The preparation of tungsten copper functionally gradient material (FGM) mostly be based on sintering technology, one of which using successively laying heterogeneity than
Tungsten copper powder, at a temperature of less than copper fusing point pressure sintering obtain tungsten/copper gradient material, composition discontinuous gradient be present in the method
The problem of distribution, while the problems such as densification degree is low, microstructure is uneven also be present.
It would therefore be highly desirable to find a kind of densification degree height, the uniform tungsten-copper functional gradient material of microstructure.
The content of the invention
The technical problems to be solved by the invention：It is low for traditional tungsten-copper functional gradient material densification degree, it is microcosmic
A kind of the problem of uneven microstructure, there is provided preparation method of high compactness tungsten-copper functional gradient material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Peach gum ball milling is taken to sieve to obtain peach gum ball-milled powder, in mass ratio 1:10, peach gum ball-milled powder is mixed with deionized water
Close, obtain scattered coagulant liquid, in mass ratio 1:5:5,100 mesh copper powders, 200 mesh tungsten powders and dispersion gel liquid are mixed, ultrasonic disperse
Obtain dispersion liquid；
（2）Dispersion liquid is placed in spray-drying installation, be spray-dried dried powder is placed in mould, cold pressing treatment obtains cold
Pressed compact material, calcining is incubated after pre-burning, standing is cooled to room temperature, obtains sintering feed and ball milling sieving, obtains combining powder；
（3）Count in parts by weight, weigh 45~50 part of 200 mesh tungsten powder, 45~50 part of 300 mesh tungsten powder, 45~50 part of 500 mesh respectively
Tungsten powder, 15~20 part of 200 mesh copper powder, 15~20 part of 300 mesh copper powder, 15~20 part of 500 mesh copper powder and 40~45 parts of combining powders,
Each powder is laid into graphite hot pressing die, waited after the completion of laying, graphite hot pressing die is placed in hot-pressed sintering furnace, pre-burning
After calcine, a kind of high compactness tungsten-copper functional gradient material can be prepared into after cooling.
Step（2）Described spray drying inlet temperature is 110~115 DEG C, and outlet temperature is 55~65 DEG C, charging rate
For 2mL/min, air mass flow 350L/h.
Step（2）Described cold pressing treatment is that 25~30s is suppressed in the case where pressure is 25~30MPa.
Step（2）Described calcined temperature is 200~210 DEG C.
Step（2）Described insulation calcining heat is 1100~1200 DEG C.
Step（3）Described each powder lays into graphite hot pressing die concrete operation step：200 mesh tungsten powders are laid
Lay to 200 mesh tungsten powder layer surfaces to graphite hot pressing die bottom, then by combining powder, finally lay 200 mesh copper powders to knot
Powder layer surface is closed, then presses laying order, then respectively by 300 mesh, 500 mesh tungsten powders and 300 mesh, 500 mesh copper powders and with reference to powder
End is laid into mould successively, controls every layer of combining powder to lay consistency of thickness.
Step（3）Described calcination condition is：Nitrogen atmosphere, pressure be 15~20MPa, temperature be 1100~1200 DEG C
Under the conditions of calcine 2~3h.
Step（3）It is described to be cooled to be cooled to room temperature by 15 DEG C/min.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is glutinous by the way that tungsten powder is glued through peach gum, after being supported on copper powder particle surface, through high temperature sintering and is incubated calcining,
Charing peach gum simultaneously sinters removal peach gum charcoal matrix, tungsten powder is had cladding to Copper Powder Surface, forms the aggregate of fine and close cladding, pass through
This aggregate improves the compactness of FGM；
（2）The present invention is mixed by powders at different levels and carries out pre-burning modification, is tying metal ion in powder stable under normal temperature
The amplitude of thermal vibration on point, metal ion is departed from node and be subjected to displacement, diffuse into and reduce material sintering stress, while by
Acted in pre-sintering, improve the constraint of lattice suffered by metal ion, improve thermal vibration frequency, it is microcosmic so as to be effectively improved material
Institutional framework, improve material compactness.
Embodiment
Peach gum and ball milling are taken, 200 mesh sieves is crossed and obtains peach gum ball-milled powder, in mass ratio 1:10, by peach gum ball-milled powder with going
Ionized water mixes, and 10~15min of ultrasonic disperse under 200~300W, is prepared into dispersion gel liquid, tungsten powder and copper powder are put respectively
In ball grinder, ball milling simultaneously sieves, and obtains 100 mesh copper powders and 200 mesh tungsten powders, and in mass ratio 1:5:5, by copper powder, tungsten powder and disperse
Coagulant liquid mixes, then ultrasonic disperse obtains dispersion liquid under 200~300W, and then dispersion liquid is placed in spray-drying installation, control
System spray drying inlet temperature is 110~115 DEG C, and outlet temperature is 55~65 DEG C, charging rate 2mL/min, air mass flow
For 350L/h, after the completion of to be spray dried, obtain dried powder and be placed in mould, 25~30s of cold pressing treatment under 25~30MPa
Afterwards, blank must be cold-pressed and be placed in 1~2h of pre-burning at 200~210 DEG C, be then warming up to 1100~1200 DEG C by 10 DEG C/min, protected
After 3~5h of temperature calcining, standing is cooled to room temperature, obtains sintering feed and is placed in 3~5h of ball milling under 350~400r/min, crosses 150 mesh sieves
Obtain combining powder；Count in parts by weight, respectively weigh 45~50 part of 200 mesh tungsten powder, 45~50 part of 300 mesh tungsten powder, 45~50 parts
500 mesh tungsten powders, 15~20 part of 200 mesh copper powder, 15~20 part of 300 mesh copper powder, 15~20 part of 500 mesh copper powder and 40~45 parts of combinations
Powder, 200 mesh tungsten powders are laid to graphite hot pressing die bottom, then combining powder is laid to 200 mesh tungsten powder layer surfaces, finally
200 mesh copper powders are laid to combining powder layer surface, then press laying order, then respectively by 300 mesh, 500 mesh tungsten powders and 300
Mesh, 500 mesh copper powders and combining powder are laid into mould successively, are controlled every layer of combining powder to lay consistency of thickness, are waited to have laid
Cheng Hou, graphite hot pressing die is placed in hot-pressed sintering furnace, leads to nitrogen and exclude air, in nitrogen atmosphere, 15~20MPa conditions
Under, be warming up to 950~1000 DEG C of 25~30min of pre-burning by 10 DEG C/min, after insulation, pressurize sinter 25~30min, then by 5 DEG C/
Min is warming up to 1150~1200 DEG C, after 2~3h is calcined in insulation, pressurize, then is cooled to room temperature by 15 DEG C/min, you can is prepared into
A kind of high compactness tungsten-copper functional gradient material.
Example 1
Peach gum and ball milling are taken, 200 mesh sieves is crossed and obtains peach gum ball-milled powder, in mass ratio 1:10, by peach gum ball-milled powder and deionization
Water mixes, and the ultrasonic disperse 15min under 300W, is prepared into dispersion gel liquid, tungsten powder and copper powder are respectively placed in ball grinder, ball
Grind and sieve, obtain 100 mesh copper powders and 200 mesh tungsten powders, in mass ratio 1:5:5, copper powder, tungsten powder and dispersion gel liquid are mixed, then
Ultrasonic disperse obtains dispersion liquid under 300W, and then dispersion liquid is placed in spray-drying installation, control spray drying inlet temperature
For 115 DEG C, outlet temperature is 65 DEG C, charging rate 2mL/min, air mass flow 350L/h, after the completion of to be spray dried, is obtained
Dried powder is placed in mould, under 30MPa after cold pressing treatment 30s, must be cold-pressed blank and is placed in pre-burning 2h at 210 DEG C, with
1200 DEG C, after 5h is calcined in insulation are warming up to by 10 DEG C/min afterwards, standing is cooled to room temperature, obtains sintering feed and is placed under 400r/min
Ball milling 5h, cross 150 mesh sieves and obtain combining powder；Count in parts by weight, respectively weigh 50 part of 200 mesh tungsten powder, 50 part of 300 mesh tungsten powder,
50 part of 500 mesh tungsten powder, 20 part of 200 mesh copper powder, 20 part of 300 mesh copper powder, 20 part of 500 mesh copper powder and 45 parts of combining powders, by 200 mesh
Tungsten powder is laid to graphite hot pressing die bottom, then combining powder is laid to 200 mesh tungsten powder layer surfaces, finally by 200 mesh copper powders
Lay to combining powder layer surface, then press laying order, then respectively by 300 mesh, 500 mesh tungsten powders and 300 mesh, 500 mesh copper powders
Laid successively into mould with combining powder, control every layer of combining powder to lay consistency of thickness, wait after the completion of laying, by graphite thermal
Compression mould is placed in hot-pressed sintering furnace, is led to nitrogen and is excluded air, under the conditions of nitrogen atmosphere, 20MPa, is warming up to by 10 DEG C/min
1000 DEG C of pre-burning 30min, it is incubated, after pressurize sintering 30min, then 1200 DEG C is warming up to by 5 DEG C/min, insulation, pressurize calcining 3h
Afterwards, then by 15 DEG C/min it is cooled to room temperature, you can be prepared into a kind of high compactness tungsten-copper functional gradient material.
Example 2
Peach gum and ball milling are taken, 200 mesh sieves is crossed and obtains peach gum ball-milled powder, in mass ratio 1:10, by peach gum ball-milled powder and deionization
Water mixes, and the ultrasonic disperse 10min under 200W, is prepared into dispersion gel liquid, tungsten powder and copper powder are respectively placed in ball grinder, ball
Grind and sieve, obtain 100 mesh copper powders and 200 mesh tungsten powders, in mass ratio 1:5:5, copper powder, tungsten powder and dispersion gel liquid are mixed, then
Ultrasonic disperse obtains dispersion liquid under 200W, and then dispersion liquid is placed in spray-drying installation, control spray drying inlet temperature
For 110 DEG C, outlet temperature is 55 DEG C, charging rate 2mL/min, air mass flow 350L/h, after the completion of to be spray dried, is obtained
Dried powder is placed in mould, under 25MPa after cold pressing treatment 25s, must be cold-pressed blank and is placed in pre-burning 1h at 200 DEG C, with
1100 DEG C, after 3h is calcined in insulation are warming up to by 10 DEG C/min afterwards, standing is cooled to room temperature, obtains sintering feed and is placed under 350r/min
Ball milling 3h, cross 150 mesh sieves and obtain combining powder；Count in parts by weight, respectively weigh 45 part of 200 mesh tungsten powder, 45 part of 300 mesh tungsten powder,
45 part of 500 mesh tungsten powder, 15 part of 200 mesh copper powder, 15 part of 300 mesh copper powder, 15 part of 500 mesh copper powder and 40 parts of combining powders, by 200 mesh
Tungsten powder is laid to graphite hot pressing die bottom, then combining powder is laid to 200 mesh tungsten powder layer surfaces, finally by 200 mesh copper powders
Lay to combining powder layer surface, then press laying order, then respectively by 300 mesh, 500 mesh tungsten powders and 300 mesh, 500 mesh copper powders
Laid successively into mould with combining powder, control every layer of combining powder to lay consistency of thickness, wait after the completion of laying, by graphite thermal
Compression mould is placed in hot-pressed sintering furnace, is led to nitrogen and is excluded air, under the conditions of nitrogen atmosphere, 15MPa, is warming up to by 10 DEG C/min
950 DEG C of pre-burning 25min, it is incubated, after pressurize sintering 25min, then 1150 DEG C is warming up to by 5 DEG C/min, insulation, pressurize calcining 2h
Afterwards, then by 15 DEG C/min it is cooled to room temperature, you can be prepared into a kind of high compactness tungsten-copper functional gradient material.
Example 3
Peach gum and ball milling are taken, 200 mesh sieves is crossed and obtains peach gum ball-milled powder, in mass ratio 1:10, by peach gum ball-milled powder and deionization
Water mixes, and the ultrasonic disperse 12min under 250W, is prepared into dispersion gel liquid, tungsten powder and copper powder are respectively placed in ball grinder, ball
Grind and sieve, obtain 100 mesh copper powders and 200 mesh tungsten powders, in mass ratio 1:5:5, copper powder, tungsten powder and dispersion gel liquid are mixed, then
Ultrasonic disperse obtains dispersion liquid under 250W, and then dispersion liquid is placed in spray-drying installation, control spray drying inlet temperature
For 112 DEG C, outlet temperature is 60 DEG C, charging rate 2mL/min, air mass flow 350L/h, after the completion of to be spray dried, is obtained
Dried powder is placed in mould, under 27MPa after cold pressing treatment 27s, must be cold-pressed blank and is placed in pre-burning 1h at 205 DEG C, with
1150 DEG C, after 4h is calcined in insulation are warming up to by 10 DEG C/min afterwards, standing is cooled to room temperature, obtains sintering feed and is placed under 370r/min
Ball milling 4h, cross 150 mesh sieves and obtain combining powder；Count in parts by weight, respectively weigh 47 part of 200 mesh tungsten powder, 47 part of 300 mesh tungsten powder,
47 part of 500 mesh tungsten powder, 18 part of 200 mesh copper powder, 16 part of 300 mesh copper powder, 17 part of 500 mesh copper powder and 42 parts of combining powders, by 200 mesh
Tungsten powder is laid to graphite hot pressing die bottom, then combining powder is laid to 200 mesh tungsten powder layer surfaces, finally by 200 mesh copper powders
Lay to combining powder layer surface, then press laying order, then respectively by 300 mesh, 500 mesh tungsten powders and 300 mesh, 500 mesh copper powders
Laid successively into mould with combining powder, control every layer of combining powder to lay consistency of thickness, wait after the completion of laying, by graphite thermal
Compression mould is placed in hot-pressed sintering furnace, is led to nitrogen and is excluded air, under the conditions of nitrogen atmosphere, 17MPa, is warming up to by 10 DEG C/min
970 DEG C of pre-burning 27min, it is incubated, after pressurize sintering 27min, then 1170 DEG C is warming up to by 5 DEG C/min, insulation, pressurize calcining 3h
Afterwards, then by 15 DEG C/min it is cooled to room temperature, you can be prepared into a kind of high compactness tungsten-copper functional gradient material.
Reference examples：The tungsten-copper functional gradient material of metal Co., Ltd of Shenzhen production.
The FGM that example and reference examples are obtained cut into ф 18mm × 16mm test specimen, carries out
Detection, specific detection are as follows：
1. shock resistance：Tested using laser thermal shock experiment, it is 200mW/m to control laser power density2, beam spot is straight
Footpath is 2~4mm, is impacted 1000 times.
2. tensile property is tested：Tested using universal testing machine.
Specific testing result such as table 1.
Table 1
| Example 1 | Example 2 | Example 3 | Reference examples | |
| Compared to density（%） | 98.6 | 98.5 | 99.0 | 82.6 |
| Tensile strength（MPa） | 235 | 240 | 245 | 198 |
| Elongation after fracture（%） | 33.6 | 34.8 | 35.9 | 20.8 |
| Shock resistance | Surface nondestructive does harm to | Surface nondestructive does harm to | Surface nondestructive does harm to | Surface starts cracked |
As shown in Table 1, the tungsten-copper functional gradient material densification degree that prepared by the present invention is high, and intensity is high, has preferable anti-impact
Hit performance.
Claims (8)
1. a kind of preparation method of high compactness tungsten-copper functional gradient material, it is characterised in that specifically preparation process is：
（1）Peach gum ball milling is taken to sieve to obtain peach gum ball-milled powder, in mass ratio 1:10, peach gum ball-milled powder is mixed with deionized water
Close, obtain scattered coagulant liquid, in mass ratio 1:5:5,100 mesh copper powders, 200 mesh tungsten powders and dispersion gel liquid are mixed, ultrasonic disperse
Obtain dispersion liquid；
（2）Dispersion liquid is placed in spray-drying installation, be spray-dried dried powder is placed in mould, cold pressing treatment obtains cold
Pressed compact material, calcining is incubated after pre-burning, standing is cooled to room temperature, obtains sintering feed and ball milling sieving, obtains combining powder；
（3）Count in parts by weight, weigh 45~50 part of 200 mesh tungsten powder, 45~50 part of 300 mesh tungsten powder, 45~50 part of 500 mesh respectively
Tungsten powder, 15~20 part of 200 mesh copper powder, 15~20 part of 300 mesh copper powder, 15~20 part of 500 mesh copper powder and 40~45 parts of combining powders,
Each powder is laid into graphite hot pressing die, waited after the completion of laying, graphite hot pressing die is placed in hot-pressed sintering furnace, pre-burning
After calcine, a kind of high compactness tungsten-copper functional gradient material can be prepared into after cooling.
A kind of 2. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that：Step
Suddenly（2）Described spray drying inlet temperature is 110~115 DEG C, and outlet temperature is 55~65 DEG C, charging rate 2mL/min,
Air mass flow is 350L/h.
A kind of 3. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that：Step
Suddenly（2）Described cold pressing treatment is that 25~30s is suppressed in the case where pressure is 25~30MPa.
A kind of 4. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that：Step
Suddenly（2）Described calcined temperature is 200~210 DEG C.
A kind of 5. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that：Step
Suddenly（2）Described insulation calcining heat is 1100~1200 DEG C.
A kind of 6. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that step
Suddenly（3）Described each powder lays into graphite hot pressing die concrete operation step：200 mesh tungsten powders are laid to graphite hot pressing
Mold bottom, then combining powder is laid to 200 mesh tungsten powder layer surfaces, finally 200 mesh copper powders are laid to combining powder layer table
Face, laying order then is pressed, then respectively lay 300 mesh, 500 mesh tungsten powders and 300 mesh, 500 mesh copper powders and combining powder successively
Into mould, every layer of combining powder is controlled to lay consistency of thickness.
A kind of 7. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that：Step
Suddenly（3）Described calcination condition is：Calcined under the conditions of nitrogen atmosphere, pressure are 15~20MPa, temperature is 1100~1200 DEG C
2~3h.
A kind of 8. preparation method of high compactness tungsten-copper functional gradient material according to claim 1, it is characterised in that：Step
Suddenly（3）It is described to be cooled to be cooled to room temperature by 15 DEG C/min.
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| CN110877103A (en) * | 2019-10-10 | 2020-03-13 | 温州中希电工合金有限公司 | Silver tungsten carbide graphite composite spherical powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110877103A (en) * | 2019-10-10 | 2020-03-13 | 温州中希电工合金有限公司 | Silver tungsten carbide graphite composite spherical powder and preparation method thereof |
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Application publication date: 20171121 |