CN103409732A - Composite processing method for realizing metallization of surfaces of diamonds - Google Patents
Composite processing method for realizing metallization of surfaces of diamonds Download PDFInfo
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- CN103409732A CN103409732A CN2013103160281A CN201310316028A CN103409732A CN 103409732 A CN103409732 A CN 103409732A CN 2013103160281 A CN2013103160281 A CN 2013103160281A CN 201310316028 A CN201310316028 A CN 201310316028A CN 103409732 A CN103409732 A CN 103409732A
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Abstract
The invention discloses a composite processing method for realizing metallization of the surfaces of diamonds. The method comprises the following steps: performing chemical plating processing on diamond particles to enable the surfaces of the diamond particles to be uniformly coated with chemical plating layers; performing metallized processing on the surfaces of the diamond particles, packing a wave-absorbing material and the diamond particles subjected to chemical plating into a ball mill jar for realizing uniform material mixing, filling a corundum crucible with the mixture, sealing the surface of the corundum crucible and placing the corundum crucible in a vacuum micro-wave heating oven, and slowly rotating the oven for heating and insulating, wherein the heating temperature is 750-900 DEG C, the heating and insulating process takes 10-30 minutes, and the vacuity is 1.3*10<-3>Pa; separating the diamond particles from the wave-absorbing material. According to the invention, the chemical plating technology and the vacuum microwave quick heating technology are combined, so that the deposition temperature of the chemical plating becomes low, and obtained plating can be more uniform and compact; heat energy can be more effectively utilized through vacuum micro-wave heating; moreover, metallurgy diffusion reaction rate is promoted, the processing time is shortened, and graphitization of the diamonds can be well prevented in a vacuum processing environment.
Description
Technical field
The present invention relates to the metallized treatment process of diamond particles surface modification field polycrystalline diamond particle surface.
Background technology
For metal binding agent diamond tool, carcass and adamantine physical chemistry consistency, be one of key factor of implementation tool use properties.Diamond tool adopts vacuum or the preparation of protective atmosphere sintering more, its objective is that the existence that prevents oxidizing atmosphere makes the too early greying of diamond.But adopting technique for overlaying diamond to be mixed to surfacing with Wimet on the steel-tooth oil bit time, because being carries out in air ambient, flame temperature is higher, is easy to cause diamond part greying, reduce its ultimate compression strength, greatly affect the result of use of diamond tool.Therefore, preventing that the diamond under high temperature is transformed into graphite because of oxidation, is to improve diamond tool service efficiency and the key factor in life-span.At present, the general method of coating surface metal 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 metal and diamond generation chemical reaction, generate stable chemical bond, realize metallurgical binding, thereby 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, disclose and adopted vacuum evaporation and vacuum heat treatment to add electric plating method at diamond surface, to form the metallization structure of carbide lamella, alloy layer and electroplated metal layer again, metal layer material used is Ti, Cr, Ta, Nb etc.Patent 200580006497.7 and patent 200580004728.0 disclose and a kind ofly adopt the method that phase vapour deposition or chemical vapour deposition add physical vapor deposition to prepare carbide, nitride and boride layer at diamond surface, to improve the scale resistance of superhard material in preparation and use procedure such as diamond.Patent CN102286742A has reported a kind of Ways of Metallizing Cladding onto Diamond Surface, at first with the solder that binding agent will contain Cr, Ti, evenly apply, with diamond, mix again, and then heating and melting solder in vacuum or inert atmosphere, the alloy layer with metallurgical binding at diamond surface, formed.In addition, Ways of Metallizing Cladding onto Diamond Surface also comprises that electroless plating adds plating, salt bath plating, chemical liquid phase is processed and metal-powder coats sintering etc.
In above-mentioned method for metallising, 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 the metal or alloy layer, and carburization zone is thinner unstable, 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 the heat tracing processing, 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 is in the heating of body of heater and workpiece itself and insulation, the net heat utilization ratio is low, rate of heating is slow.Compare traditional heat treated technology, microwave heating has whole heating, and rate of heating is fast, and the time is short, energy-conservation, can carry out the plurality of advantages such as spatial selectivity heating promotion chemical reaction.At present, micro-wave energy is widely used in the heat treated of inorganic materials, organic polymer and metallic substance, synthetic and sintering research, has no open report and utilize microwave heating to carry out diamond surface metallization.
Summary of the invention
The object of the present invention is to provide a kind of compounding method of diamond surface metallization, the method combines electroless plating and vacuum microwave rapid heating technology, the electroless deposition temperature is low, required equipment is simple, obtain relatively even compact of coating, vacuum microwave rapid heating absorbing material, and heat is passed to chemical plating and diamond particles, more effectively utilize heat energy, can also promote the speed of metallurgical diffusion reaction, shorten the treatment time, process and can better stop adamantine greying in vacuum environment.
Compounding method of the present invention, concrete technological line is as follows: diamond particles is first carried out to the surface chemical plating processing, make its surface uniform apply one deck composite deposite, reduce diamond particles surface crack, defect with calking, the mode of filling; Then the diamond after electroless plating is embedded in the corundum crucible that contains absorbing material, then is placed in the vacuum microwave process furnace and carries out the microwave heating thermal-insulation processing, make chemical plating and diamond surface form carbide lamella.
A kind of compounding method of diamond surface metallization comprises the following steps successively:
(1) diamond particles is carried out to the electroless plating processing, 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) diamond particles is carried out to the surface metalation processing, by absorbing material and the electroless plating diamond particles evenly batch mixing of ball grinder (not adding abrading-ball) of packing into, make the complete embedding diamond particles of absorbing material, and be filled in corundum crucible, then the crucible surface capping of having loaded is placed in the vacuum microwave process furnace, slow circumvolve carries out heat tracing, controls Heating temperature at 750 ℃-900 ℃, the whole time of heating and insulating process is controlled at 10-30 minute, and vacuum tightness is 1.3 * 10
-3Pa;
(3) body of heater to be heated cooling after, crucible is taken out, the standard inspection sieve suitable with the order number separates diamond particles with absorbing material, the diamond particles that filters out surface metalation is standby.
Described electroless plating is processed, and comprises 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 μ m, the mean particle size of selected diamond particles is greater than the absorbing material granularity, is generally 100-350 μ m.
Described vacuum microwave process furnace bottom load sample platform can rotate, and static being placed on sample bench of corundum crucible heated.
Compared with prior art, the present invention combines the features of electroless plating and vacuum microwave heating, and its beneficial effect is as follows: at first, electroless plating is a kind of very ripe surface treatment method, and depositing temperature is low, and required equipment is simple, obtains relatively even compact of coating; Secondly, the vacuum microwave heating technique can the 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, in vacuum environment, process and can better stop adamantine greying, make diamond surface generate the metallization coating, the coating internal layer reacts with diamond interface and forms carbide lamella, skin is the metal or alloy layer, and the thickness of metallization coating is 10-20 μ m.
The accompanying drawing explanation
Fig. 1 is without the stereoscopic pattern of metallization diamond particles;
Fig. 2 is the stereoscopic pattern of metallization diamond particles in embodiment 1;
Fig. 3 is the Analysis of components figure of metallization diamond particles in embodiment 1;
Fig. 4 is the Analysis of components figure of metallization diamond particles in embodiment 2.
Embodiment
Below further illustrate according to drawings and embodiments the present invention.
Reagent and medicine that the present invention uses are commercially available.
Embodiment 1
Adopt electroless plating to prepare Ni-Cr-P coating at diamond surface, diamond particles is 150-180 μ m, and Fig. 1 is its stereoscopic microstructure.Plating solution forms and 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, with ammoniacal liquor and 30% acetic acid, regulating bath pH value is 7-9, and diamond particles is introduced to plating solution, ultrasonicly adds the mechanical stirring plating, bath temperature is 85 ℃, 1 hour time, cooling rear taking-up electroless plating diamond particles, washing and drying.Diamond particles and zirconium white ball milling are mixed, make diamond particles fully by embedding, then batch mixing is placed on to capping in the corundum crucible that capacity is 500ml, be placed on again in the vacuum microwave process furnace heat tracing 20 minutes, microwave power 1.5KW, 900 ℃ of sintering temperatures, vacuum tightness are 1.3 * 10
-3Pa, last furnace cooling, take out and sieve with standard sieve, obtains the diamond particles of surface metalation.Fig. 2 is the stereoscopic pattern after diamond metal, can find out that the surface metalation layer is more even, fine and close.Fig. 3 is the XRD phase collection of illustrative plates after diamond metal, can find out that the phase composition after metallization comprises Cr
3C
2With metal Ni.
Embodiment 2
Adopt electroless plating to prepare Ni-Cr-W-P coating at diamond surface, diamond particles is 150-180 μ m, and plating solution 1 forms and 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, the pH value is 8.8-9.2,90 ℃ of temperature; 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
2O 1-5 g/L, pH value 8-10, mix two kinds of plating solutions fully and stir, in the constant temperature water bath device, 90 ℃ of temperature.Diamond particles is introduced to plating solution, ultrasonicly add the mechanical stirring plating, bath temperature continues to remain 90 ℃, 1 hour time, cooling rear taking-up electroless plating diamond particles, washing and drying.Diamond particles and zirconium white ball milling are mixed, make diamond particles fully by embedding, then batch mixing is placed on to capping in the corundum crucible that capacity is 500ml, be placed on again in the vacuum microwave process furnace heat tracing 20 minutes, microwave power 1.5KW, 800 ℃ of sintering temperatures, vacuum tightness are 1.3 * 10
-3Pa, last furnace cooling, take out and sieve with standard sieve, can obtain the diamond particles of surface metalation.Fig. 4 is the XRD phase collection of illustrative plates after diamond metal, can find out that the phase composition 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 μ m, and plating solution forms and 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, the adjusting bath pH value is 5-6, and diamond particles is introduced to plating solution, ultrasonicly adds the mechanical stirring plating, bath temperature is 80 ℃, 1 hour time, cooling rear taking-up electroless plating diamond particles, washing and drying.Diamond particles and zirconium white ball milling are mixed, make diamond particles fully by embedding, then batch mixing is placed on to capping in the corundum crucible that capacity is 500ml, be placed on again in the vacuum microwave process furnace heat tracing 20 minutes, microwave power 1.5KW, 800 ℃ of sintering temperatures, vacuum tightness are 1.3 * 10
-3Pa, last furnace cooling, take out and sieve with standard sieve, can obtain the diamond particles of surface metalation.
All embodiment all implement under technical scheme prerequisite of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to the above embodiments.Those skilled in the art are by using for reference this paper content, and appropriate change raw material, processing parameter and step etc. realize all being deemed to be included in the present invention in spirit of the present invention, scope and content.
Claims (3)
1. the compounding method of a diamond surface metallization comprises the following steps successively:
(1) diamond particles is carried out to the electroless plating processing, 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) diamond particles is carried out to the surface metalation processing, by absorbing material and the electroless plating diamond particles even batch mixing of ball grinder of packing into, make the complete embedding diamond particles of absorbing material, and be filled in corundum crucible, then the crucible surface capping is placed in the vacuum microwave process furnace, slow circumvolve carries out heat tracing, controls Heating temperature at 750 ℃-900 ℃, the whole time of heating and insulating process is controlled at 10-30 minute, and vacuum tightness is 1.3 * 10
-3Pa;
(3) body of heater to be heated cooling after, crucible is taken out, diamond particles is separated with absorbing material, filter out the diamond particles of surface metalation.
2. compounding method as claimed in claim 1, is characterized in that, described electroless plating is processed, and comprises that diamond particles is clean, alligatoring, sensitization, activation, plating, flushing, oven dry.
3. compounding method as claimed in claim 1, is characterized in that, described absorbing material is zirconium white, chromic oxide or silicon carbide, and mean particle size is 10-30 μ m, and the mean particle size of described diamond particles is 100-350 μ m.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104096938A (en) * | 2014-06-23 | 2014-10-15 | 南京航空航天大学 | Brazing method-based diamond surface activation technology |
| CN105177540A (en) * | 2015-10-08 | 2015-12-23 | 山东建筑大学 | Novel composite coating of diamond applied to stone cutter |
| CN105386018A (en) * | 2015-10-08 | 2016-03-09 | 山东建筑大学 | Diamond surface plating technology applied to stone cutting tool |
| CN106925775A (en) * | 2017-04-17 | 2017-07-07 | 河南工业大学 | A kind of method of diadust plated surface chromium carbide |
| CN106947961A (en) * | 2017-03-23 | 2017-07-14 | 南京三超新材料股份有限公司 | The processing method of nickel plating diamond surface electrocorrosion-resisting |
| 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 |
| 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 |
| CN109182955A (en) * | 2018-11-15 | 2019-01-11 | 广东省新材料研究所 | A kind of absorption coating and preparation method thereof |
| CN110904442A (en) * | 2019-11-27 | 2020-03-24 | 洛阳吉瓦新材料科技有限公司 | Diamond surface modification method |
| CN111270227A (en) * | 2020-02-15 | 2020-06-12 | 常州大学 | Method for preparing micro-nano needle convex super-hydrophobic surface by utilizing microwave |
| WO2020133731A1 (en) * | 2018-12-26 | 2020-07-02 | 郑州元素工具技术有限公司 | Coarsened bare diamond wire saw and method for coarsening diamond |
| CN112410742A (en) * | 2020-10-30 | 2021-02-26 | 东莞市烽元科技有限公司 | In Al2O3Method for plating nano-scale copper film on surface of ceramic substrate by magnetron sputtering |
| CN112974797A (en) * | 2021-02-07 | 2021-06-18 | 哈尔滨工业大学 | Method for preparing high-bonding-strength carbide coating on diamond surface by utilizing microwaves |
| CN115011917A (en) * | 2022-05-18 | 2022-09-06 | 湖南工业职业技术学院 | Diamond particle surface modification method based on vacuum thermal evaporation |
| 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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Cited By (21)
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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 |
| CN104096938A (en) * | 2014-06-23 | 2014-10-15 | 南京航空航天大学 | Brazing method-based diamond surface activation technology |
| CN105177540A (en) * | 2015-10-08 | 2015-12-23 | 山东建筑大学 | Novel composite coating of diamond applied to stone cutter |
| CN105386018A (en) * | 2015-10-08 | 2016-03-09 | 山东建筑大学 | Diamond surface plating technology applied to stone cutting tool |
| 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 |
| CN106947961B (en) * | 2017-03-23 | 2019-02-22 | 南京三超新材料股份有限公司 | The processing method of nickel plating diamond surface electrocorrosion-resisting |
| CN106947961A (en) * | 2017-03-23 | 2017-07-14 | 南京三超新材料股份有限公司 | The processing method of nickel plating diamond surface electrocorrosion-resisting |
| CN106925775B (en) * | 2017-04-17 | 2019-01-25 | 河南工业大学 | A kind of method of diadust surface plating chromium carbide |
| CN106925775A (en) * | 2017-04-17 | 2017-07-07 | 河南工业大学 | A kind of method of diadust plated surface 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 |
| CN109182955A (en) * | 2018-11-15 | 2019-01-11 | 广东省新材料研究所 | A kind of absorption coating and preparation method thereof |
| WO2020133731A1 (en) * | 2018-12-26 | 2020-07-02 | 郑州元素工具技术有限公司 | Coarsened bare diamond wire saw and method for coarsening diamond |
| CN110904442A (en) * | 2019-11-27 | 2020-03-24 | 洛阳吉瓦新材料科技有限公司 | Diamond surface modification method |
| CN111270227A (en) * | 2020-02-15 | 2020-06-12 | 常州大学 | Method for preparing micro-nano needle convex super-hydrophobic surface by utilizing microwave |
| CN112410742A (en) * | 2020-10-30 | 2021-02-26 | 东莞市烽元科技有限公司 | In Al2O3Method for plating nano-scale copper film on surface of ceramic substrate by magnetron sputtering |
| CN112974797A (en) * | 2021-02-07 | 2021-06-18 | 哈尔滨工业大学 | Method for preparing high-bonding-strength carbide coating on diamond surface by utilizing microwaves |
| 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 |
| CN115011917A (en) * | 2022-05-18 | 2022-09-06 | 湖南工业职业技术学院 | Diamond particle surface modification method based on vacuum thermal evaporation |
| CN115011917B (en) * | 2022-05-18 | 2023-06-06 | 湖南工业职业技术学院 | Diamond particle surface modification method based on vacuum thermal evaporation |
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