CN103409732B - A kind of compounding method of diamond surface metallization - Google Patents
A kind of compounding method of diamond surface metallization Download PDFInfo
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- CN103409732B CN103409732B CN201310316028.1A CN201310316028A CN103409732B CN 103409732 B CN103409732 B CN 103409732B CN 201310316028 A CN201310316028 A CN 201310316028A CN 103409732 B CN103409732 B CN 103409732B
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- diamond particles
- diamond
- heating
- absorbing material
- electroless plating
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Abstract
The invention discloses a kind of compounding method of diamond surface metallization, comprising: electroless plating process is carried out to diamond particles, make its surface uniform apply one deck chemical plating; Surface metalation process is carried out to diamond particles, absorbing material and electroless plating diamond particles are loaded the even batch mixing of ball grinder, be filled in corundum crucible, crucible surface capping is placed in vacuum microwave process furnace, slow circumvolve carries out heating and thermal insulation, Heating temperature is at 750 DEG C-900 DEG C, and the time of heating and insulating process, vacuum tightness was 1.3 × 10 at 10-30 minute
-3pa; Diamond particles is separated with absorbing material.Electroless plating and vacuum microwave rapid heating technology combine by the present invention, electroless deposition temperature is low, obtain coating and compare even compact, vacuum microwave heating more effectively utilizes heat energy, metallurgical diffusion reaction speed can also be promoted, shorten the treatment time, can better stop adamantine greying in vacuum environment process.
Description
Technical field
The present invention relates to the metallized treatment process of diamond particle surfaces modification field polycrystalline diamond particle surface.
Background technology
For metal binding agent diamond tool, carcass and adamantine physical chemistry consistency are one of key factors of implementation tool use properties.Diamond tool many employings vacuum or the preparation of protective atmosphere sintering, its objective is and prevent the existence of oxidizing atmosphere from making the too early greying of diamond.But adopt technique for overlaying diamond mixed with Wimet surfacing on steel-tooth oil bit time, owing to being carry out in air ambient, flame temperature is higher, is easy to cause diamond fraction greying, reduce its ultimate compression strength, greatly affect the result of use of diamond tool.Therefore, preventing the diamond under high temperature to be transformed into graphite because of oxidation, is improve diamond tool service efficiency and the key factor in life-span.At present, the general method of surface metallization that adopts reduces diamond high temperature graphitization tendency both at home and abroad, reduce the interfacial energy between diamond and metal lining, realize the infiltration of diamond and various metals material, and by this layer of metal and diamond generation chemical reaction, generate stable chemical bond, realize metallurgical binding, thus improve the bonding strength of diamond and matrix, be beneficial to give full play to adamantine performance.
The method of diamond surface metallization is existing a lot, as patent CN85100286A discloses adopt vacuum evaporation and vacuum heat treatment to add again electric plating method to form carbide lamella, alloy layer and electroplated metal layer metallization structure at diamond surface, metal layer material used is Ti, Cr, Ta, Nb etc.Patent 200580006497.7 and patent 200580004728.0 disclose a kind of method adopting the vapour deposition of thing phase or chemical vapour deposition to add physical vapor deposition and prepare carbide, nitride and boride layer at diamond surface, to improve the scale resistance of the superhard materials such as diamond in preparation and use procedure.Patent CN102286742A reports a kind of Ways of Metallizing Cladding onto Diamond Surface, first with binding agent, the solder containing Cr, Ti is evenly applied, mix with diamond again, and then heating and melting solder in vacuum or inert atmosphere, the alloy layer with metallurgical binding is formed at diamond surface.In addition, Ways of Metallizing Cladding onto Diamond Surface also comprises electroless plating and adds plating, salt bath plating, chemical liquid phase process and the coated sintering of metal-powder etc.
In above-mentioned method for metallising, thing phase and chemical gaseous phase depositing process need professional equipment, and process parameter control is strict, and cost is higher.Electroless plating adds electric plating method and is mainly used to prepare metal or alloy layer, the thinner instability of carburization zone, inadequate to adamantine hold, easily in use and subsequent process, causes diamond drop-off, and the instrument that affects uses.Powder covers in the metallized process of diamond sintering and all adopts electricity or gas heat treatment furnace to carry out heating and thermal insulation process, its subject matter is from heating to insulation at least 2 hours in whole metallization processes, process time is long, production efficiency is lower, and amount of heat consumption in the heating of body of heater and workpiece itself with in insulation, net heat utilization ratio is low, rate of heating is slow.Compare traditional heat treatment technique, microwave heating has overall heating, and rate of heating is fast, and the time is short, energy-conservation, can carry out spatial selectivity heating and promote the plurality of advantages such as chemical reaction.At present, micro-wave energy is widely used in the heat treated of inorganic materials, organic polymer and metallic substance, synthesis and sintering research, and utilizes microwave heating to carry out diamond surface metallization to have no open report.
Summary of the invention
The object of the present invention is to provide a kind of compounding method of diamond surface metallization, electroless plating and vacuum microwave rapid heating technology combine by the method, electroless deposition temperature is low, required equipment is simple, obtain coating and compare even compact, vacuum microwave rapid heating absorbing material, and heat is passed to chemical plating and diamond particles, more effectively utilize heat energy, the speed of metallurgical diffusion reaction can also be promoted, shorten the treatment time, can better stop adamantine greying in vacuum environment process.
Compounding method of the present invention, concrete technological line is as follows: first carry out surface chemical plating process to diamond particles, makes its surface uniform apply one deck composite deposite, reduces diamond particle surfaces crackle, defect with calking, the mode of filling; Then the diamond after electroless plating is embedded in the corundum crucible containing absorbing material, then is placed in vacuum microwave process furnace and carries out microwave heating thermal-insulation process, make chemical plating and diamond surface form carbide lamella.
A compounding method for diamond surface metallization, comprises the following steps successively:
(1) carry out electroless plating process to diamond particles, make its surface uniform apply one deck chemical plating, described chemical plating is Ni-P, Ni-Cr-P or Ni-W-Cr-P composite bed;
(2) surface metalation process is carried out to diamond particles, absorbing material and electroless plating diamond particles are loaded ball grinder (not adding abrading-ball) evenly batch mixing, absorbing material is made to embed diamond particles completely, and be filled in corundum crucible, then be placed in vacuum microwave process furnace by the crucible surface capping loaded, slow circumvolve carries out heating and thermal insulation, controls Heating temperature at 750 DEG C-900 DEG C, the whole time controling of heating and insulating process is at 10-30 minute, and vacuum tightness is 1.3 × 10
-3pa;
(3), after body of heater cooling to be heated, taken out by crucible, diamond particles is separated with absorbing material by the standard inspection sieve suitable with order number, and the diamond particles filtering out surface metalation is for subsequent use.
Described electroless plating process, comprise that diamond particles is clean, alligatoring, sensitization, activation, plating, flushing, oven dry etc.
Described absorbing material is zirconium white (ZrO
2), chromic oxide (Cr
2o
3) or silicon carbide (SiC), mean particle size is 10-30 μm, and the mean particle size of selected diamond particles is greater than absorbing material granularity, is generally 100-350 μm.
Bottom described vacuum microwave process furnace, load sample platform can rotate, and static being placed on sample bench of corundum crucible is heated.
Compared with prior art, present invention incorporates the features of electroless plating and vacuum microwave heating, its beneficial effect is as follows: first, and electroless plating is a kind of very ripe surface treatment method, and depositing temperature is low, and required equipment is simple, obtains coating and compares even compact; Secondly, vacuum microwave heating technique can rapid heating absorbing material, and heat is passed to chemical plating and diamond particles, and heat-up rate is exceedingly fast, and more effectively utilizes heat energy; And, microwave heating can promote the speed of metallurgical diffusion reaction, shorten the treatment time, in addition, can better stop adamantine greying in vacuum environment process, make diamond surface generate metallization coating, coating internal layer and diamond interface react and form carbide lamella, skin is then metal or alloy layer, and the thickness of metallization coating is 10-20 μm.
Accompanying drawing explanation
Fig. 1 is without the stereoscopic pattern of metalized diamond particle;
Fig. 2 is the stereoscopic pattern of metalized diamond particle in embodiment 1;
Fig. 3 is the Analysis of components figure of metalized diamond particle in embodiment 1;
Fig. 4 is the Analysis of components figure of metalized diamond particle in embodiment 2.
Embodiment
Further illustrate the present invention according to drawings and embodiments below.
The reagent that the present invention uses and medicine are commercially available.
embodiment 1
Adopt electroless plating to prepare Ni-Cr-P coating at diamond surface, diamond particles is 150-180 μm, Fig. 1 is its stereoscopic microstructure.Plating solution composition comprises NiSO
47H
2o 10-20g/L, CrCl
36H
2o 10-15g/L, NaH
2pO
2h
2o 35-45g/L, C
6h
8o
7h
2o 30-35g/L, C
3h
6o
310-20g/L, NH
4cl 30-50g/L, regulates bath pH value to be 7-9 with ammoniacal liquor and 30% acetic acid, diamond particles is introduced plating solution, ultrasonicly adds mechanical stirring plating, and bath temperature is 85 DEG C, 1 hour time, takes out electroless plating diamond particles, washing and drying after cooling.Diamond particles and zirconium white ball milling are mixed, diamond particles is embedded completely, the capacity that is then placed on by batch mixing is capping in the corundum crucible of 500ml, to be placed in vacuum microwave process furnace heating and thermal insulation again 20 minutes, microwave power 1.5KW, sintering temperature 900 DEG C, vacuum tightness is 1.3 × 10
-3pa, last furnace cooling, taking-up standard sieve sieves, and obtains the diamond particles of surface metalation.Fig. 2 is the stereoscopic pattern after diamond metal, can find out that side metallization is more even, fine and close.Fig. 3 is the XRD thing phase collection of illustrative plates after diamond metal, can find out that the thing phase composite after metallization comprises Cr
3c
2and W metal.
embodiment 2
Adopt electroless plating to prepare Ni-Cr-W-P coating at diamond surface, diamond particles is 150-180 μm, and plating solution 1 composition comprises NiSO
47H
2o 20-30g/L, Na
2wO
42H
2o 50-70g/L, NaH
2pO
2h
2o 15-25g/L, Na
3c
6h
5o
7h
2o 100-110g/L, (NH
4)
2sO
430-35g/L, pH value is 8.8-9.2, temperature 90 DEG C; Plating solution 2 consists of CrF
310-20 g/L, NaH
2pO
2h
2o 5-10 g/L, Na
3c
6h
5o
7h
2o 5-10g/L, CrCl
36H
2two kinds of plating solution mixing are fully stirred by O 1-5 g/L, pH value 8-10, as in constant temperature water bath device, and temperature 90 DEG C.Diamond particles is introduced plating solution, ultrasonicly adds mechanical stirring plating, bath temperature continues to remain 90 DEG C, 1 hour time, takes out electroless plating diamond particles, washing and drying after cooling.Diamond particles and zirconium white ball milling are mixed, diamond particles is embedded completely, the capacity that is then placed on by batch mixing is capping in the corundum crucible of 500ml, to be placed in vacuum microwave process furnace heating and thermal insulation again 20 minutes, microwave power 1.5KW, sintering temperature 800 DEG C, vacuum tightness is 1.3 × 10
-3pa, last furnace cooling, taking-up standard sieve sieves, and can obtain the diamond particles of surface metalation.Fig. 4 is the XRD thing phase collection of illustrative plates after diamond metal, can find out that the thing phase composite after metallization comprises Ni, CrC, Ni
3p, WC and Ni
4w.
embodiment 3
Adopt electroless plating to prepare Ni-P coating at diamond surface, diamond particles is 150-180 μm, and plating solution composition comprises NiSO
46H
2o 20-30g/L, NaAc 40-50 g/L, NaH
2pO
2h
2o 30-40 g/L, CH
3cOONH
410-20 g/L, a small amount of sulfuric acid, adjustment bath pH value is 5-6, and diamond particles is introduced plating solution, ultrasonicly adds mechanical stirring plating, and bath temperature is 80 DEG C, 1 hour time, takes out electroless plating diamond particles, washing and drying after cooling.Diamond particles and zirconium white ball milling are mixed, diamond particles is embedded completely, the capacity that is then placed on by batch mixing is capping in the corundum crucible of 500ml, to be placed in vacuum microwave process furnace heating and thermal insulation again 20 minutes, microwave power 1.5KW, sintering temperature 800 DEG C, vacuum tightness is 1.3 × 10
-3pa, last furnace cooling, taking-up standard sieve sieves, and can obtain the diamond particles of surface metalation.
All embodiments are all implemented under technical scheme prerequisite of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention are not limited to the above embodiments.Those skilled in the art are by using for reference present disclosure, and appropriate change raw material, processing parameter and step etc. realize the present invention, are all deemed to be included in spirit of the present invention, scope and content.
Claims (3)
1. a compounding method for diamond surface metallization, comprises the following steps successively:
(1) carry out electroless plating process to diamond particles, make its surface uniform apply one deck chemical plating, described chemical plating is Ni-P, Ni-Cr-P or Ni-W-Cr-P composite bed;
(2) surface metalation process is carried out to diamond particles, absorbing material and electroless plating diamond particles are loaded the even batch mixing of ball grinder, absorbing material is made to embed diamond particles completely, and be filled in corundum crucible, then be placed in vacuum microwave process furnace by crucible surface capping, slow circumvolve carries out heating and thermal insulation, controls Heating temperature at 750 DEG C-900 DEG C, the whole time controling of heating and insulating process is at 10-30 minute, and vacuum tightness is 1.3 × 10
-3pa;
(3), after body of heater cooling to be heated, crucible is taken out, diamond particles is separated with absorbing material, filters out the diamond particles of surface metalation.
2. compounding method as claimed in claim 1, is characterized in that, described electroless plating process, comprise that diamond particles is clean, alligatoring, sensitization, activation, plating, flushing, oven dry.
3. compounding method as claimed in claim 1, it is characterized in that, described absorbing material is zirconium white, chromic oxide or silicon carbide, and mean particle size is 10-30 μm, and the mean particle size of described diamond particles is 100-350 μm.
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| CN103409732B true CN103409732B (en) | 2015-11-04 |
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| CN103962551A (en) * | 2014-04-15 | 2014-08-06 | 昆明理工大学 | Method for plating chromium on surface of artificial diamond on microwave heating condition |
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| CN105177540B (en) * | 2015-10-08 | 2017-12-12 | 山东建筑大学 | A kind of diamond composite deposite applied to stone cutter tool |
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| CN106925775B (en) * | 2017-04-17 | 2019-01-25 | 河南工业大学 | A kind of method of diadust surface plating chromium carbide |
| CN108950530A (en) * | 2018-07-25 | 2018-12-07 | 芜湖昌菱金刚石工具有限公司 | A kind of Ways of Metallizing Cladding onto Diamond Surface of high bond strength |
| CN108914096A (en) * | 2018-07-25 | 2018-11-30 | 芜湖昌菱金刚石工具有限公司 | A kind of preparation method of diamond surface cladding Ni-W-P metallization coating |
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| CN112974797B (en) * | 2021-02-07 | 2022-03-04 | 哈尔滨工业大学 | Method for preparing high-bonding-strength carbide coating on diamond surface by utilizing microwaves |
| CN116496760A (en) * | 2022-01-19 | 2023-07-28 | 中南大学 | Superhard material abrasive particles with multi-principal element medium/high entropy alloy coating layer and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1096725A (en) * | 1993-06-22 | 1994-12-28 | 李惠东 | Diamond electrode for bead welding |
| CN101186513A (en) * | 2007-12-14 | 2008-05-28 | 武汉理工大学 | Device for continuously sintering material product by microwave and realization thereof |
| CN101279366A (en) * | 2008-05-28 | 2008-10-08 | 天津大学 | Method for producing diamond reinforced Cu-matrix compound material by surface metallization and chemical deposition |
| CN101870592A (en) * | 2010-06-30 | 2010-10-27 | 武汉理工大学 | Preparation method of titanium-nitride silicon carbide fibers |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5346719A (en) * | 1993-08-02 | 1994-09-13 | General Electric Company | Tungsten metallization of CVD diamond |
-
2013
- 2013-07-25 CN CN201310316028.1A patent/CN103409732B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1096725A (en) * | 1993-06-22 | 1994-12-28 | 李惠东 | Diamond electrode for bead welding |
| CN101186513A (en) * | 2007-12-14 | 2008-05-28 | 武汉理工大学 | Device for continuously sintering material product by microwave and realization thereof |
| CN101279366A (en) * | 2008-05-28 | 2008-10-08 | 天津大学 | Method for producing diamond reinforced Cu-matrix compound material by surface metallization and chemical deposition |
| CN101870592A (en) * | 2010-06-30 | 2010-10-27 | 武汉理工大学 | Preparation method of titanium-nitride silicon carbide fibers |
Non-Patent Citations (2)
| Title |
|---|
| 氧化环境对金属化金刚石热稳定性能的影响;黄敏等;《金刚石与磨料磨具工程》;20090630(第3期);第48页左栏"实验"及第50页右栏"结论" * |
| 金刚石表面化学镀Ni-P的研究;冒爱琴;《粉末冶金技术》;20080229;第26卷(第1期);第15页右栏"金刚石预处理" * |
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