CN108941541A - A kind of method that diamond surface forms high-temperature stable coating - Google Patents
A kind of method that diamond surface forms high-temperature stable coating Download PDFInfo
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- CN108941541A CN108941541A CN201810827294.3A CN201810827294A CN108941541A CN 108941541 A CN108941541 A CN 108941541A CN 201810827294 A CN201810827294 A CN 201810827294A CN 108941541 A CN108941541 A CN 108941541A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
Abstract
The invention discloses a kind of methods that diamond surface forms high-temperature stable coating, comprising: carries out ball milling after mixing Si powder, Co powder and TiC or WC, obtains metallization mixed-powder；The diadust of coating surface silicon layer and metallization mixed-powder and organic solvent are uniformly mixed, mixed slurry is obtained after drying；Mixed slurry is heated and is reacted, the diamond that surface has high-temperature stable coating is obtained.The method that diamond surface of the present invention forms high-temperature stable coating, by the metalization layer for forming silicon carbide and high-temperature stability on diadust surface, the bond strength between metal alloy coating and diamond can be significantly improved, and can be used in high temperature applicationss.
Description
Technical field
The present invention relates to the technical fields of diamond surface processing more particularly to a kind of diamond surface to form high-temperature stable
The method of coating.
Background technique
Diamond itself also has excellent optics, sound in addition to the excellent properties such as high, anticorrosive, wearability with hardness
The properties such as, calorifics and electricity.Since over half a century, the production of diamond and the development of application technology are advanced by leaps and bounds,
It has reached in quantity, quality and many performances and has been even more than natural diamond.Diamond and its product are not only answered extensively
For mechanical, metallurgy, each industrial technical field such as build work, traffic, national defence, it is extended to high performance heat-resistant piece, anti-corrosion
The key areas such as part, heat conducting element and chip.Superhard material based on diamond etc. has become the basic of Modern Manufacturing Technology
Means play support and facilitation to state-owned pillar industry and national defense industry.It is counted according to external authoritative sources, world's diamond
Demand be just incremented by with average 8% or so annual growth rate, carbonado 50% or so is for manufacturing processing of stone at present
Tool.It is contemplated that the material progress of the mankind will attain a yet higher goal, or even peak after diamond product is universal, into
Enter the eternal diamond epoch.
Performance difference is larger between the material interfaces such as diamond and most of metal, ceramics, and interface can be higher, so that Buddha's warrior attendant
It is difficult to effectively soak between stone and metal or alloy, interface binding power is poor, i.e., is usually between diamond abrasive grain and bonding agent
Cast setting easily falls off under the action of grinding force, reduces the service life of grinding tool.It is estimated that diamond impregnated tools
Middle diamond utilization rate is only 60% or so, has millions of carats of expensive diamond drop-off every year and is lost among scrap,
Loss is in terms of ten million yuan.
For improve diamond tool service life, using Modified Diamond method improve diamond surface with it is intermetallic
Wellability and bond strength become more reasonable method.What country's plating was relatively uniform at present is using magnetron sputtering, chemistry
The methods of plating, plating, PVD, CVD improve diamond and intermetallic knot in diamond surface deposited metal layer or carbide lamella
With joint efforts.However, metal layer or carbide lamella that these diamond surfaces are formed or combining defective tightness or in high temperature item
It is dissociated under part.Therefore, diamond and intermetallic binding performance are significantly improved there is an urgent need in the art to one kind and can guarantee in height
The method that thermal field closes the Modified Diamond used.
Summary of the invention
The problem of based on background technique, the invention proposes a kind of diamond surfaces to form high-temperature stable coating
Method can significantly improve metal conjunction by forming the metalization layer of silicon carbide and high-temperature stability on diadust surface
Bond strength between gold plate and diamond, and can be used in high temperature applicationss.
The method that a kind of diamond surface proposed by the present invention forms high-temperature stable coating, includes the following steps:
S1, by weight percentage by the Si powder of 20-50wt%, the Co powder of 30-60wt% and 10-30wt% TiC or
After WC mixing, dehydrated alcohol is added as medium and carries out ball milling, is dried after ball milling 20-30h, metallization mixed powder is obtained after sieving
End；
S2, the obtained metallization mixed-powder of the diadust of coating surface silicon layer and S1 and organic solvent are mixed
Uniformly, mixed slurry is obtained after drying；
S3, the mixed slurry for obtaining S2 are under vacuum conditions or heating reaction under inert gas protection, heating are reacted
Temperature be 1000-1300 DEG C, time 30-60min, it is cooling after sieving remove extra metallization mixed-powder, obtain table
Face has the diamond of high-temperature stable coating.
Preferably, in S1, granularity≤5um of the Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity
>=99wt%；Granularity≤2um of the TiC, purity >=99wt%；Granularity≤2um of the WC, purity >=99wt%.
Preferably, in S2, the coating surface silicon layer is obtained in diadust coating surface silicon layer by salt bath process
Diadust；Preferably, by partial size be 100-200 μm diadust and calcium chloride powder, partial size be 5-10 μm silicon
Powder 3-6:5-8:1 in mass ratio is added in high speed mixer and is uniformly mixed, in vacuum degree≤10-3It is warming up under conditions of Pa
Insulation reaction 30-60min after 1050-1150 DEG C, after being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then
It using hot-water soak, rinses, is then cleaned by ultrasonic using deionized water, then rinsed using dehydrated alcohol, obtained after vacuum drying
The diadust of the coating surface silicon layer.
Preferably, before high speed mixer is added in diadust and calcium chloride powder, silicon powder, diamond is carried out
Cleaning；Specifically diadust is immersed in dilution heat of sulfuric acid, the insulated and stirred 60-90min at 60-80 DEG C, after filtering
It uses distilled water repeated flushing to cleaning solution pH for 6-7, then 30-60min is cleaned by ultrasonic using acetone, it is then super using distilled water
Sound cleans 10-30min, is rinsed after filtering using dehydrated alcohol, then be dried in vacuo.
Preferably, in S2, diadust, metallization mixed-powder and the metallization mixed powder of the coating surface silicon layer
The weight ratio at end is 6-15:2-10:1-3.
Preferably, in S2, the organic solvent be one of dehydrated alcohol, polyvinyl alcohol, polyethylene glycol, ethylene glycol or
The a variety of combinations with diethy-aceto oxalate of person.
Preferably, in S3, the mixed slurry that S2 is obtained is the lazy of 100-100000Pa under vacuum conditions or in pressure
Heating reaction is carried out in property gas shield.
Preferably, in S3, when extra metallization mixed-powder is removed in sieving, 30 mesh, 80 mesh, 150 mesh are specifically crossed respectively
Sieve removes extra metallization mixed-powder.
The method that a kind of diamond surface proposed by the present invention forms high-temperature stable coating, using by Si powder, Co powder, TiC
Or the metallization mixed-powder of WC composition and the diadust of coating surface silicon layer carry out high-temperature heating treatment, it is on the one hand viscous
The silicon layer and diamond particle surfaces carbon atom for being attached to diamond particle surfaces occur chemical reaction and generate boron carbide, another party
Face, metallize mixed-powder under high-temperature process in melting or slush state, the silicon of diamond particle surfaces will and week
The large quantitative metal liquid phase reaction enclosed forms silicon alloy metal layer in diamond particles outermost layer, wherein in metallization mixed-powder
Si powder can reduce the fusion temperature of metalization layer, be conducive to the metallization reaction of silicon carbide, gold then can be improved in Co powder
The interaction and binding force of categoryization layer and silicon carbide, TiC powder and WC powder Dispersed precipitate play metalization layer in metalization layer
To the effect of reinforcement heatproof.
It follows that in the diamond surface clad that preparation method of the present invention obtains while including nanometer silicon carbide
Layer and metallic nanotubes layer, the nanometer silicon carbide layer are directly combined to diamond particle surfaces, the metallic nanotubes layer
It combines closely in the nanometer silicon carbide layer surface, i.e., diamond and metalization layer is connected to by silicon carbide transition zone, and
It is firmly combined together due to passing through chemical bonds between diamond and metalization layer, significantly improves the interface knot of the two
Conjunction ability, while improving the wetability between diamond and metal, the especially associativity between diamond powder and metal,
Simultaneously with the high-temperature stability of the metalization layer, it ensure that the plating diamond has and use advantage in high temperature applicationss.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the diamond that surface prepared by the present invention has high-temperature stable coating.
Fig. 2 is that the surface that the embodiment of the present invention 1 obtains has the cross sectional scanning electron of the diamond of high-temperature stable coating aobvious
Micro- photo.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of method that diamond surface forms high-temperature stable coating, includes the following steps:
S1, the TiC of the Si powder of 30wt%, the Co powder of 40wt% and 30wt% is added in ball grinder by weight percentage,
Dehydrated alcohol is added as medium and carries out ball milling, is dried after ball milling 25h, obtains metallization mixed-powder after crossing 200 meshes, wherein
Granularity≤5um of the Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity >=99wt%；The grain of the TiC
Degree≤2um, purity >=99wt%；
It S2, is 100 μm of diadust and the silicon powder 4:7:1 in mass ratio that calcium chloride powder, partial size are 8 μm by partial size
It is added in high speed mixer and is uniformly mixed, in vacuum degree≤10-3Insulation reaction 40min after being warming up to 1100 DEG C under conditions of Pa,
After being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then using hot-water soak, rinse, then using go from
Sub- water ultrasonic cleaning, then rinsed using dehydrated alcohol, the diadust of the coating surface silicon layer is obtained after vacuum drying；It presses
Weight ratio 10:6:2 adds the metallization mixed-powder and organic solvent that the diadust of coating surface silicon layer and S1 are obtained
Enter in blender and be uniformly mixed, the organic solvent is the combination of dehydrated alcohol and diethy-aceto oxalate, is mixed after drying
Close slurry；
S3, the mixed slurry that S2 is obtained is heated into reaction under vacuum conditions, the temperature for heating reaction is 1200 DEG C, the time
For 40min, 30 mesh, 80 mesh, 150 mesh sieve are crossed respectively after cooling and remove extra metallization mixed-powder, obtaining surface has
The diamond of high-temperature stable coating.
Surface manufactured in the present embodiment has electron scanning micrograph such as Fig. 2 institute of the diamond of high-temperature stable coating
Show, shows that diamond particle surfaces growth has coating in figure.
Embodiment 2
A kind of method that diamond surface forms high-temperature stable coating, includes the following steps:
S1, the WC of the Si powder of 20wt%, the Co powder of 60wt% and 20wt% is added in ball grinder by weight percentage, added
Enter dehydrated alcohol as medium and carry out ball milling, dried after ball milling 20h, obtains metallization mixed-powder after crossing 200 meshes, wherein institute
State granularity≤5um of Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity >=99wt%；The granularity of the WC
≤ 2um, purity >=99wt%；
S2, it is 100 μm of diadust and the silicon powder 3:8 in mass ratio that calcium chloride powder, partial size are 10 μm by partial size:
It is uniformly mixed in 1 addition high speed mixer, in vacuum degree≤10-3Insulation reaction 60min after being warming up to 1050 DEG C under conditions of Pa,
After being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then using hot-water soak, rinse, then using go from
Sub- water ultrasonic cleaning, then rinsed using dehydrated alcohol, the diadust of the coating surface silicon layer is obtained after vacuum drying；It presses
Weight ratio 6:10:1 adds the metallization mixed-powder and organic solvent that the diadust of coating surface silicon layer and S1 are obtained
Enter in blender and be uniformly mixed, the organic solvent is the combination of polyvinyl alcohol and diethy-aceto oxalate, is mixed after drying
Close slurry；
S3, the mixed slurry that S2 is obtained is heated into reaction under vacuum conditions, the temperature for heating reaction is 100 DEG C, the time
For 60min, 30 mesh, 80 mesh, 150 mesh sieve are crossed respectively after cooling and remove extra metallization mixed-powder, obtaining surface has
The diamond of high-temperature stable coating.
Embodiment 3
A kind of method that diamond surface forms high-temperature stable coating, includes the following steps:
S1, the TiC of the Si powder of 50wt%, the Co powder of 30wt% and 20wt% is added in ball grinder by weight percentage,
Dehydrated alcohol is added as medium and carries out ball milling, is dried after ball milling 30h, obtains metallization mixed-powder after crossing 200 meshes, wherein
Granularity≤5um of the Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity >=99wt%；The grain of the TiC
Degree≤2um, purity >=99wt%；
It S2, is 200 μm of diadust and the silicon powder 6:5:1 in mass ratio that calcium chloride powder, partial size are 5 μm by partial size
It is added in high speed mixer and is uniformly mixed, in vacuum degree≤10-3Insulation reaction 30min after being warming up to 1150 DEG C under conditions of Pa,
After being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then using hot-water soak, rinse, then using go from
Sub- water ultrasonic cleaning, then rinsed using dehydrated alcohol, the diadust of the coating surface silicon layer is obtained after vacuum drying；It presses
Weight ratio 15:2:3 adds the metallization mixed-powder and organic solvent that the diadust of coating surface silicon layer and S1 are obtained
Enter in blender and be uniformly mixed, the organic solvent is the combination of polyethylene glycol and diethy-aceto oxalate, is mixed after drying
Close slurry；
S3, the mixed slurry for obtaining S2 heat reaction in the case where pressure is 100Pa inert gas shielding, heat the temperature of reaction
Degree is 1300 DEG C, time 30min, crosses 30 mesh, 80 mesh, 150 mesh sieve respectively after cooling and removes extra metallization mixed powder
End obtains the diamond that surface has high-temperature stable coating.
Embodiment 4
A kind of method that diamond surface forms high-temperature stable coating, includes the following steps:
S1, the WC of the Si powder of 40wt%, the Co powder of 50wt% and 10wt% is added in ball grinder by weight percentage, added
Enter dehydrated alcohol as medium and carry out ball milling, dried after ball milling 28h, obtains metallization mixed-powder after crossing 200 meshes, wherein institute
State granularity≤5um of Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity >=99wt%；The granularity of the WC
≤ 2um, purity >=99wt%；
It S2, is 150 μm of diadust and the silicon powder 5:6:1 in mass ratio that calcium chloride powder, partial size are 7 μm by partial size
It is added in high speed mixer and is uniformly mixed, in vacuum degree≤10-3Insulation reaction 50min after being warming up to 1100 DEG C under conditions of Pa,
After being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then using hot-water soak, rinse, then using go from
Sub- water ultrasonic cleaning, then rinsed using dehydrated alcohol, the diadust of the coating surface silicon layer is obtained after vacuum drying；It presses
Weight ratio 11:7:2 adds the metallization mixed-powder and organic solvent that the diadust of coating surface silicon layer and S1 are obtained
Enter in blender and be uniformly mixed, the organic solvent is the combination of ethylene glycol and diethy-aceto oxalate, is mixed after drying
Slurry；
S3, the mixed slurry for obtaining S2 heat reaction, heating reaction in the case where pressure is 100000Pa inert gas shielding
Temperature be 1100 DEG C, time 50min, crossing 30 mesh, 80 mesh, 150 mesh sieve after cooling respectively, to remove extra metallization mixed
Powder is closed, the diamond that surface has high-temperature stable coating is obtained.
Embodiment 5
A kind of method that diamond surface forms high-temperature stable coating, includes the following steps:
S1, the TiC of the Si powder of 30wt%, the Co powder of 40wt% and 30wt% is added in ball grinder by weight percentage,
Dehydrated alcohol is added as medium and carries out ball milling, is dried after ball milling 20h, obtains metallization mixed-powder after crossing 200 meshes, wherein
Granularity≤5um of the Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity >=99wt%；The grain of the TiC
Degree≤2um, purity >=99wt%；
It S2, is 200 μm of diadust and the silicon powder 5:8:1 in mass ratio that calcium chloride powder, partial size are 7 μm by partial size
It is added in high speed mixer and is uniformly mixed, in vacuum degree≤10-3Insulation reaction 50min after being warming up to 1050 DEG C under conditions of Pa,
After being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then using hot-water soak, rinse, then using go from
Sub- water ultrasonic cleaning, then rinsed using dehydrated alcohol, the diadust of the coating surface silicon layer is obtained after vacuum drying；It presses
Weight ratio 12:5:1 adds the metallization mixed-powder and organic solvent that the diadust of coating surface silicon layer and S1 are obtained
Enter in blender and be uniformly mixed, the organic solvent is the combination of dehydrated alcohol, polyvinyl alcohol and diethy-aceto oxalate, drying
After obtain mixed slurry；
S3, the mixed slurry for obtaining S2 heat reaction in the case where pressure is 50000Pa inert gas shielding, heat reaction
Temperature is 1200 DEG C, time 50min, crosses 30 mesh, 80 mesh, 150 mesh sieve after cooling respectively and removes extra metallization mixing
Powder obtains the diamond that surface has high-temperature stable coating.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method that diamond surface forms high-temperature stable coating, which comprises the steps of:
S1, the TiC or WC of the Si powder of 20-50wt%, the Co powder of 30-60wt% and 10-30wt% mixed by weight percentage
After conjunction, dehydrated alcohol is added as medium and carries out ball milling, is dried after ball milling 20-30h, metallization mixed-powder is obtained after sieving；
S2, the obtained metallization mixed-powder of the diadust of coating surface silicon layer and S1 and organic solvent are mixed
It is even, mixed slurry is obtained after drying；
S3, the mixed slurry for obtaining S2 heat reaction under vacuum conditions or under inert gas protection, heat the temperature of reaction
Degree is 1000-1300 DEG C, time 30-60min, is sieved after cooling and removes extra metallization mixed-powder, obtains surface tool
There is the diamond of high-temperature stable coating.
2. the method that diamond surface according to claim 1 forms high-temperature stable coating, which is characterized in that in S1, institute
State granularity≤5um of Si powder, purity >=99wt%；Granularity≤3um of the Co powder, purity >=99wt%；The granularity of the TiC
≤ 2um, purity >=99wt%；Granularity≤2um of the WC, purity >=99wt%.
3. the method that diamond surface according to claim 1 or 2 forms high-temperature stable coating, which is characterized in that in S2,
The diadust of the coating surface silicon layer is obtained in diadust coating surface silicon layer by salt bath process；Preferably, will
The silicon powder 3-6:5-8:1 in mass ratio that the diadust and calcium chloride powder, partial size that partial size is 100-200 μm are 5-10 μm adds
Enter in high speed mixer and be uniformly mixed, in vacuum degree≤10-3Insulation reaction 30- after being warming up to 1050-1150 DEG C under conditions of Pa
60min, after being cooled to room temperature, calcium chloride powder and extra silicon powder are removed in sieving, then using hot-water soak, flushing, then adopt
It is cleaned by ultrasonic with deionized water, then is rinsed using dehydrated alcohol, the diamond of the coating surface silicon layer is obtained after vacuum drying
Micro mist.
4. the method that diamond surface according to claim 3 forms high-temperature stable coating, which is characterized in that by Buddha's warrior attendant
Stone micro mist and calcium chloride powder, silicon powder are added before high speed mixer, clean to diamond；Specifically by diadust
It is immersed in dilution heat of sulfuric acid, the insulated and stirred 60-90min at 60-80 DEG C, using distilled water repeated flushing to washing after filtering
Liquid pH is 6-7, then is cleaned by ultrasonic 30-60min using acetone, is then cleaned by ultrasonic 10-30min using distilled water, adopts after filtering
It is rinsed, then is dried in vacuo with dehydrated alcohol.
5. the method that diamond surface according to claim 1-4 forms high-temperature stable coating, which is characterized in that
In S2, the weight ratio of the diadust of the coating surface silicon layer, metallization mixed-powder and the mixed-powder that metallizes is 6-
15:2-10:1-3。
6. the method that diamond surface according to claim 1-5 forms high-temperature stable coating, which is characterized in that
In S2, the organic solvent is one or more of dehydrated alcohol, polyvinyl alcohol, polyethylene glycol, ethylene glycol and oxalic acid two
The combination of ethyl ester.
7. the method that diamond surface according to claim 1-6 forms high-temperature stable coating, which is characterized in that
In S3, the mixed slurry that S2 is obtained carries out under vacuum conditions or in the inert gas shielding that pressure is 100-100000Pa
Heating reaction.
8. the method that diamond surface according to claim 1-7 forms high-temperature stable coating, which is characterized in that
In S3, when extra metallization mixed-powder is removed in sieving, 30 mesh, 80 mesh, 150 mesh sieve are specifically crossed respectively and remove extra gold
Categoryization mixed-powder.
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| WO2022095747A1 (en) * | 2020-11-05 | 2022-05-12 | 上海征世科技股份有限公司 | Method for modification of diamond surface and use thereof |
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Application publication date: 20181207 |