CN115584540B - Diamond wire saw with composite coating and preparation process thereof - Google Patents
Diamond wire saw with composite coating and preparation process thereof Download PDFInfo
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- CN115584540B CN115584540B CN202211506900.4A CN202211506900A CN115584540B CN 115584540 B CN115584540 B CN 115584540B CN 202211506900 A CN202211506900 A CN 202211506900A CN 115584540 B CN115584540 B CN 115584540B
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 211
- 239000010432 diamond Substances 0.000 title claims abstract description 211
- 239000011248 coating agent Substances 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 107
- 238000007747 plating Methods 0.000 claims abstract description 92
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 53
- 239000004576 sand Substances 0.000 claims abstract description 52
- 238000007596 consolidation process Methods 0.000 claims abstract description 38
- 238000000151 deposition Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 37
- 230000008569 process Effects 0.000 claims abstract description 33
- 230000008021 deposition Effects 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 16
- 239000010959 steel Substances 0.000 claims abstract description 16
- 238000012986 modification Methods 0.000 claims abstract description 15
- 230000004048 modification Effects 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000013329 compounding Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 80
- 229910052757 nitrogen Inorganic materials 0.000 claims description 40
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- 206010070834 Sensitisation Diseases 0.000 claims description 16
- 230000008313 sensitization Effects 0.000 claims description 16
- 230000003213 activating effect Effects 0.000 claims description 15
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 15
- 239000004327 boric acid Substances 0.000 claims description 15
- VCKGYYLUGUKTCX-UHFFFAOYSA-L nickel(2+);dichloride;trihydrate Chemical compound O.O.O.[Cl-].[Cl-].[Ni+2] VCKGYYLUGUKTCX-UHFFFAOYSA-L 0.000 claims description 15
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 14
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims description 14
- 239000011733 molybdenum Substances 0.000 claims description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 229920000570 polyether Polymers 0.000 claims description 13
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 13
- 238000001179 sorption measurement Methods 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- CHLCPTJLUJHDBO-UHFFFAOYSA-M sodium;benzenesulfinate Chemical compound [Na+].[O-]S(=O)C1=CC=CC=C1 CHLCPTJLUJHDBO-UHFFFAOYSA-M 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 claims description 5
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 5
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 5
- 235000017281 sodium acetate Nutrition 0.000 claims description 5
- 229940087562 sodium acetate trihydrate Drugs 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- YJBKVPRVZAQTPY-UHFFFAOYSA-J tetrachlorostannane;dihydrate Chemical compound O.O.Cl[Sn](Cl)(Cl)Cl YJBKVPRVZAQTPY-UHFFFAOYSA-J 0.000 claims description 5
- 238000001994 activation Methods 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 19
- 238000005520 cutting process Methods 0.000 abstract description 12
- 229910052582 BN Inorganic materials 0.000 abstract description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical group N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 5
- 230000002035 prolonged effect Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- 238000004140 cleaning Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 230000007935 neutral effect Effects 0.000 description 12
- 239000013078 crystal Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0607—Wires
Abstract
The invention relates to the technical field of diamond wire saw, in particular to a diamond wire saw with a composite coating and a preparation process thereof, which comprises the following processes: (1) preplating: placing a busbar steel wire in a basic plating solution, and depositing a nickel preplating layer to obtain a preplating busbar; (2) sanding: placing the pre-plated busbar in a diamond suspension plating solution, and carrying out diamond compounding and sanding on the surface of the pre-plated busbar to obtain a diamond sand line; (3) consolidation: and placing the diamond sand line in a consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment to obtain the diamond wire saw. According to the invention, through carrying out surface modification on the diamond and the diamond sand line, the patterned deposition of the boron nitride on the surface of the diamond particles is realized, the exposure height and the self-sharpening property of the modified diamond in the manufactured wire saw can be improved, the durability of the diamond wire saw is improved, the holding force of the diamond wire saw on the diamond and the cutting capability of the wire saw are effectively improved, and the service life of the diamond wire saw is prolonged.
Description
Technical Field
The invention relates to the technical field of diamond wire saw, in particular to a diamond wire saw with a composite coating and a preparation process thereof.
Background
Photovoltaic power generation is an efficient way for humans to convert solar energy into electrical energy for production, life. At present, the global solar cells mainly adopt silicon-based solar cells, and account for more than 90% of the global photovoltaic market. With the development of semiconductor and photovoltaic industries, the cutting processing requirements on noble and hard and brittle materials such as monocrystalline silicon, polycrystalline silicon, sapphire and the like are higher and higher. The diamond wire saw is widely applied by virtue of the advantages of good wear resistance, high cutting efficiency, small environmental pollution and the like. The diamond wire saw is obtained by adopting an electrodeposition method to bond diamond abrasive particles on a busbar matrix through a nickel plating layer. But when the bus wire diameter in the diamond wire saw is smaller, after the surface of the bus wire diameter is plated with diamond, the brittleness of the wire saw is larger, brittle failure phenomenon is easy to occur after bending, and the cutting efficiency and the service life of the wire saw are seriously affected. Therefore, we propose a diamond wire saw with composite coating and a process for preparing the same.
Disclosure of Invention
The invention aims to provide a diamond wire saw with a composite coating and a preparation process thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation process of a diamond wire saw with a composite coating comprises the following steps:
(1) Pre-plating: placing a busbar steel wire in a basic plating solution, and depositing a nickel preplating layer to obtain a preplating busbar;
(2) And (3) sand feeding: placing the pre-plated busbar in a diamond suspension plating solution, and carrying out diamond compounding and sanding on the surface of the pre-plated busbar to obtain a diamond sand line;
(3) Consolidation: and placing the diamond sand line in a consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment to obtain the diamond wire saw.
Further, the diameter of the busbar wire is 60. Mu.m.
The busbar wire is pretreated before the preplating process, which comprises the following processes:
placing the bus steel wire in a sodium hydroxide solution for cleaning for 30-40 s, placing the bus steel wire in an sulfamic acid solution for treating for 25-35 s after water washing, water washing and drying, cleaning dirt such as greasy dirt on the surface of the bus steel wire, removing the residual oxide layer and metal rust on the surface, and keeping the surface clean and the matrix activated so as to ensure the quality of the subsequent bus steel wire electroplating;
the mass concentration of the sodium hydroxide solution is 6%, and the temperature is 55-65 ℃; the concentration of sulfamic acid solution is 4 percent, and the treatment temperature is 35-45 ℃.
Further, the (1) pre-plating process comprises the following steps: preplating current density 15A/dm 2 The preplating time is 30s;
the basic plating solution comprises the following components: 400-450 g/L nickel sulfamate, 40-50 g/L boric acid, 3-5 g/L nickel chloride trihydrate, pH of 4.4-4.8, and temperature of 53-57 ℃.
The nickel sulfamate solution is used as a preplating solution (basic plating solution), the bus steel wire after cleaning and activating is used as a cathode, a nickel plate is used as an anode, and nickel is preliminarily plated on the surface of the bus steel wire under the condition of air flow stirring to form a preplating layer, and the thickness of the preplating layer is about 0.3 mu m, so that the preplating bus is obtained.
Further, the sand feeding process (2) comprises the following steps: sanding current density 5A/dm 2 The sand feeding time is 30s, and the magnetic induction intensity of the preplating busbar is 0.6mT;
the diamond suspension plating solution comprises the following components: 300-400 g/L nickel sulfamate, 30-40 g/L boric acid, 3-5 g/L nickel chloride trihydrate, 15g/L diamond, pH of 4.2-4.6 and temperature of 53-57 ℃.
The diamond particles are dispersed in the nickel sulfamate plating solution to be used as a sand plating solution, a preplating bus is used as a cathode, a nickel plate is used as an anode, the diamond particles are uniformly dispersed in the nickel sulfamate plating solution through air flow stirring to prevent sedimentation and agglomeration, sand plating is carried out, the diamond particles are fixed on the surface of the preplating bus to form a sand plating nickel layer, and the thickness of the sand plating nickel layer is about 0.8 mu m, so that the diamond sand line is obtained.
Further, the consolidation process (3) comprises the following steps: the consolidation current density is 5A/dm2, and the consolidation time is 80s;
the consolidation plating solution comprises the following components: 300-400 g/L nickel sulfamate, 30-40 g/L boric acid, 3-5 g/L nickel chloride trihydrate, pH of 3.6-4.0 and temperature of 53-57 ℃.
Further, the heat treatment process in (3) is as follows: the temperature is 180-400 ℃ and the time is 2 hours.
Nickel sulfamate plating solution is used as thick plating solution, a diamond sand line is used as a cathode, a nickel plate is used as an anode, and nickel layer thick plating is carried out under the condition of air flow stirring, so that the firmness of diamond particles on bus steel wires is improved, a thick nickel plating layer is formed, and the thickness of the thick nickel plating layer is about 1.0 mu m; and then placing the diamond wire saw at 180-400 ℃, preserving heat for 2 hours, drying and removing internal hydrogen to obtain the finished diamond wire saw.
Further, the grain diameter of the diamond is 10-20 mu m, and the median diameter is 15 mu m;
the diamond is subjected to surface modification, and specifically comprises the following processes:
1) Alkali washing: placing diamond into boiled sodium hydroxide solution with mass fraction of 10% for 30min, and washing with pure water to neutrality;
2) Coarsening: placing the diamond obtained in the previous step into boiled nitric acid solution with the mass fraction of 10% for 30min, and washing the diamond to be neutral by pure water;
3) Adsorption: placing the diamond obtained in the previous step into an ethanol solution of 0.2-0.4% propylene glycol block polyether, treating at room temperature for 10-15 min, and drying with nitrogen;
4) And (3) deposition: placing the diamond obtained in the previous step into a chemical vapor deposition device, introducing ammonia, boron trichloride, hydrogen and nitrogen, and retaining for 0.12-0.18 s at the temperature of 600-700 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia, boron trichloride, hydrogen and nitrogen is 3:1:1:6, and the gas flow of boron trichloride is 20mL/min;
placing the cleaned and coarsened diamond in an ethanol solution of propylene glycol block polyether, and shielding the (111) crystal face of the diamond by utilizing preferential adsorption of a nonionic surfactant propylene glycol block polyether on the (111) crystal face of the diamond so that the (220) crystal face of the diamond is relatively exposed; and then performing chemical vapor deposition of boron nitride, so that the boron nitride can be deposited on the (220) crystal face of the diamond, and the patterned deposition of the boron nitride on the surface of the diamond particles is realized by controlling the concentration of the propylene glycol block polyether solution, so that the exposure height and the self-sharpening of the modified diamond in the manufactured wire saw can be improved, the durability of the diamond wire saw is improved, and the service life and the cutting capability of the diamond wire saw are improved.
5) Sensitization: placing the diamond obtained in the previous step into a sensitization solution, treating for 15-20 min at room temperature, and washing with pure water to be neutral; the sensitization liquid contains 0.8-1.0 g/L tin chloride dihydrate and 30-40 mL/L hydrochloric acid;
6) Activating: placing the diamond obtained in the previous step into an activating solution, treating for 15-20 min at room temperature, and washing with pure water to be neutral; the activating solution contains 0.8-1.0 g/L palladium chloride and 16-20 mL/L hydrochloric acid;
7) Chemical plating: placing the diamond obtained in the previous step into a nickel plating solution at 85 ℃, stirring at a rotating speed of 300r/min, and plating nickel for 10-15 min to obtain modified diamond; the addition amount of diamond in the nickel plating solution is 7-9 g/L, and the nickel plating solution contains: 25g/L nickel sulfate hexahydrate, 25-35 g/L sodium hypophosphite, 18-24 g/L sodium acetate trihydrate and 12-15 g/L sodium citrate.
Sensitization of diamond particles, covalent bonding of redundant carbon atoms on the diamond surface to adsorb a large amount of Sn 2+ A suspension key; then, during the activation process, pb in the activation solution 2+ Sn adsorbed by diamond particle surface 2+ Reducing into metal Pb, and continuing to adsorb on the surface of diamond particles to form palladium particles. The large number of metal palladium particles on the diamond surface can be used as the catalytic center of electroless nickel plating, and because Pb and Ni have similar lattice structures and are in face-centered cubic structures, and the lattice parameters are close to each other, ni is added 2+ Reducing into Ni atoms, depositing on palladium particles on the surfaces of the diamond particles, and enabling the surfaces of the diamond particles to be completely wrapped by nickel through continuous deposition and expansion of nickel, metallizing the diamond particles and endowing the diamond particles with conductivity;
in the sand electroplating process, the movement of the modified diamond is influenced by the hardness of an electric field and moves towards the cathode, so that the contact probability between the modified diamond and a preplating bus is increased, and the probability of capturing the modified diamond by a plating layer is facilitated; under the action of electric field, free electrons in nickel are distributed on the surface to make Ni 2+ The metal nickel is adsorbed on the modified diamond, so that the metal nickel can grow on the surface of the preplating busbar, can grow on the surface of the modified diamond and the joint of the modified diamond and the preplating layer, and can be fixedly connected on the surface of the preplating layer through a metal bond, so that the holding force of the prepared diamond wire saw on the modified diamond and the cutting capability of the wire saw can be greatly improved, and the service life of the diamond wire saw is prolonged.
Further, the (3) is modified before the consolidation process, and specifically comprises the following processes:
1) Adsorption: placing the diamond sand line into 0.2-0.4 g/L sodium benzene sulfinate solution, treating at room temperature for 10-15 min, and drying with nitrogen;
2) And (3) deposition: placing the diamond sand line obtained in the previous step into a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and performing deposition at the temperature of 155-185 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5:2:10, and the flow of nitrogen is 100sccm; pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the cycle is 80-120 times.
Placing the diamond sand line obtained after sand feeding in sodium benzene sulfinate solution, and shielding the (220) crystal face and the (311) crystal face of the diamond by utilizing preferential adsorption of sodium benzene sulfinate to the metal nickel crystal face so that the (111) crystal face and the (200) crystal face of the diamond are relatively exposed; and then molybdenum disulfide is deposited on the surface of the diamond yarn by utilizing molybdenum hexacarbonyl and hydrogen sulfide, so that the molybdenum disulfide is deposited on the (111) crystal faces of the modified diamond nickel plating layer in the diamond yarn and the metal nickel in the pre-plating layer, the longitudinal friction of the manufactured diamond wire saw can be reduced, the brittle fracture of the wire saw caused by stress is relieved, and the holding force of the diamond wire saw on the modified diamond and the service life of the wire saw are prolonged.
Further, the consolidation plating solution (3) also comprises 2g/L propylene glycol block polyether. So that the plating layer shows obvious preferred orientation, improves the uniformity of the thick nickel plating layer structure, is more beneficial to the firmness and stability of the modified diamond on the busbar steel wire, improves the holding force of the diamond wire saw on the modified diamond, improves the cutting capability and the service life of the wire saw,
compared with the prior art, the invention has the following beneficial effects:
according to the diamond wire saw with the composite coating and the preparation process thereof, through surface modification of the diamond and the diamond sand line, patterned deposition of boron nitride on the surface of diamond particles is realized, the exposure height and self-sharpening property of the modified diamond in the manufactured wire saw can be improved, the durability of the diamond wire saw is improved, the holding force of the diamond wire saw on the diamond and the cutting capability of the wire saw are effectively improved, and the service life of the diamond wire saw is prolonged.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clearly and completely described, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
(1) Pretreatment:
placing the busbar steel wire in a sodium hydroxide solution for cleaning for 30s, placing the busbar steel wire in an sulfamic acid solution for treatment for 30s after water cleaning, and drying; the mass concentration of the sodium hydroxide solution is 6 percent, and the temperature is 60 ℃; the concentration of the sulfamic acid solution is 4 percent, and the treatment temperature is 40 ℃;
example 1
(2) Pre-plating:
placing a busbar steel wire in a basic plating solution, and depositing a nickel preplating layer to obtain a preplating busbar; the preplating process comprises the following steps: preplating current density 15A/dm 2 The preplating time is 30s; the basic plating solution comprises the following components: 400g/L nickel sulfamate, 40g/L boric acid, 3g/L nickel chloride trihydrate, pH 4.8, and temperature of 53 ℃;
(3) And (3) sand feeding:
3.1. surface modification of diamond:
1) Alkali washing: placing diamond into boiled sodium hydroxide solution with mass fraction of 10% for 30min, and washing with pure water to neutrality;
2) Coarsening: placing the diamond obtained in the previous step into boiled nitric acid solution with the mass fraction of 10% for 30min, and washing the diamond to be neutral by pure water;
3) Adsorption: placing the diamond obtained in the previous step into an ethanol solution of 0.2% propylene glycol block polyether, treating at room temperature for 10min, and drying with nitrogen;
4) And (3) deposition: placing the diamond obtained in the previous step into a chemical vapor deposition device, introducing ammonia, boron trichloride, hydrogen and nitrogen, and staying for 0.12s at 600 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia, boron trichloride, hydrogen and nitrogen is 3:1:1:6, and the gas flow of boron trichloride is 20mL/min;
5) Sensitization: placing the diamond obtained in the previous step into a sensitization solution, treating for 15min at room temperature, and washing with pure water to be neutral; the sensitization liquid contains 0.8g/L tin chloride dihydrate and 30mL/L hydrochloric acid;
6) Activating: placing the diamond obtained in the previous step into an activating solution, treating for 15min at room temperature, and washing with pure water to be neutral; the activating solution contains 0.8g/L palladium chloride and 16mL/L hydrochloric acid;
7) Chemical plating: placing the diamond obtained in the previous step into a nickel plating solution at 85 ℃, stirring at a rotating speed of 300r/min, and plating nickel for 10min to obtain modified diamond; the addition amount of diamond in the nickel plating solution is 7g/L, and the nickel plating solution contains: 25g/L nickel sulfate hexahydrate, 25g/L sodium hypophosphite, 18g/L sodium acetate trihydrate, 12g/L sodium citrate;
3.2. placing the pre-plated busbar in a diamond suspension plating solution, and carrying out diamond compounding and sanding on the surface of the pre-plated busbar to obtain a diamond sand line; the sand feeding process comprises the following steps: sanding current density 5A/dm 2 The sand feeding time is 30s, and the magnetic induction intensity of the preplating busbar is 0.6mT; the diamond suspension plating solution comprises the following components: 300g/L nickel sulfamate, 30g/L boric acid, 3g/L nickel chloride trihydrate, 15g/L diamond, pH 4.6, temperature 53 ℃;
(4) Consolidation:
1) Adsorption: placing the diamond sand line in 0.2g/L sodium benzene sulfinate solution, treating at room temperature for 10min, and drying with nitrogen;
2) And (3) deposition: placing the diamond sand line obtained in the previous step into a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and performing deposition at 155 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5:2:10, and the flow of nitrogen is 100sccm; pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen 5s/10s/7s/10s, and the cycle was 80 times.
3) Placing the diamond sand line obtained in the previous step in a consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment at 180 ℃ for 2 hours to obtain a diamond wire saw; the consolidation process comprises the following steps: consolidation current density 5A/dm 2 The consolidation time is 80s;
the consolidation plating solution comprises the following components: 300g/L nickel sulfamate, 30g/L boric acid, 3g/L nickel chloride trihydrate, 2g/L propylene glycol block polyether, pH 4.0, temperature 53 ℃.
Example 2
(2) Pre-plating:
placing a busbar steel wire in a basic plating solution, and depositing a nickel preplating layer to obtain a preplating busbar; the preplating process comprises the following steps: preplating current density 15A/dm 2 The preplating time is 30s; the basic plating solution comprises the following components: 420g/L nickel sulfamate, 45g/L boric acid, 4g/L nickel chloride trihydrate, pH 4.6, and temperature 55 ℃;
(3) And (3) sand feeding:
3.1. surface modification of diamond:
1) Alkali washing: placing diamond into boiled sodium hydroxide solution with mass fraction of 10% for 30min, and washing with pure water to neutrality;
2) Coarsening: placing the diamond obtained in the previous step into boiled nitric acid solution with the mass fraction of 10% for 30min, and washing the diamond to be neutral by pure water;
3) Adsorption: placing the diamond obtained in the previous step into an ethanol solution of 0.3% propylene glycol block polyether, treating at room temperature for 12min, and drying with nitrogen;
4) And (3) deposition: placing the diamond obtained in the previous step in a chemical vapor deposition device, introducing ammonia, boron trichloride, hydrogen and nitrogen, and staying for 0.15s at the temperature of 650 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia, boron trichloride, hydrogen and nitrogen is 3:1:1:6, and the gas flow of boron trichloride is 20mL/min;
5) Sensitization: placing the diamond obtained in the previous step into a sensitization solution, treating for 18min at room temperature, and washing with pure water to be neutral; the sensitization liquid contains 0.9g/L tin chloride dihydrate and 35mL/L hydrochloric acid;
6) Activating: placing the diamond obtained in the previous step into an activating solution, treating for 18min at room temperature, and washing with pure water to be neutral; the activating solution contains 0.9g/L palladium chloride and 18mL/L hydrochloric acid;
7) Chemical plating: placing the diamond obtained in the previous step into a nickel plating solution at 85 ℃, stirring at a rotating speed of 300r/min, and plating nickel for 12min to obtain modified diamond; the addition amount of diamond in the nickel plating solution is 8g/L, and the nickel plating solution contains: 25g/L nickel sulfate hexahydrate, 30g/L sodium hypophosphite, 21g/L sodium acetate trihydrate, 13g/L sodium citrate;
3.2. placing the pre-plated busbar in a diamond suspension plating solution, and carrying out diamond compounding and sanding on the surface of the pre-plated busbar to obtain a diamond sand line; the sand feeding process comprises the following steps: sanding current density 5A/dm 2 The sand feeding time is 30s, and the magnetic induction intensity of the preplating busbar is 0.6mT;
the diamond suspension plating solution comprises the following components: 350g/L nickel sulfamate, 35g/L boric acid, 4g/L nickel chloride trihydrate, 15g/L diamond, pH 4.4 and temperature 55 ℃;
(4) Consolidation:
1) Adsorption: placing the diamond sand line in 0.3g/L sodium benzene sulfinate solution, treating at room temperature for 12min, and drying with nitrogen;
2) And (3) deposition: placing the diamond sand line obtained in the previous step into a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and performing deposition at 170 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5:2:10, and the flow of nitrogen is 100sccm; pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the cycle is 100 times.
3) Placing the diamond sand line obtained in the previous step in a consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment at 300 ℃ for 2 hours to obtain a diamond wire saw; the consolidation process comprises the following steps: consolidation current density 5A/dm 2 The consolidation time is 80s;
the consolidation plating solution comprises the following components: 350g/L nickel sulfamate, 35g/L boric acid, 4g/L nickel chloride trihydrate, 2g/L propylene glycol block polyether, pH 3.8, and temperature 55 ℃.
Example 3
(2) Pre-plating:
placing a busbar steel wire in a basic plating solution, and depositing a nickel preplating layer to obtain a preplating busbar; the preplating process comprises the following steps: preplating current density 15A/dm 2 The preplating time is 30s;
the basic plating solution comprises the following components: 450g/L nickel sulfamate, 50g/L boric acid, 5g/L nickel chloride trihydrate, pH 4.4, and temperature 57 ℃;
(3) And (3) sand feeding:
3.1. surface modification of diamond:
1) Alkali washing: placing diamond into boiled sodium hydroxide solution with mass fraction of 10% for 30min, and washing with pure water to neutrality;
2) Coarsening: placing the diamond obtained in the previous step into boiled nitric acid solution with the mass fraction of 10% for 30min, and washing the diamond to be neutral by pure water;
3) Adsorption: placing the diamond obtained in the previous step into an ethanol solution of 0.4% propylene glycol block polyether, treating for 15min at room temperature, and drying with nitrogen;
4) And (3) deposition: placing the diamond obtained in the previous step into a chemical vapor deposition device, introducing ammonia, boron trichloride, hydrogen and nitrogen, and staying for 0.18s at the temperature of 700 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia, boron trichloride, hydrogen and nitrogen is 3:1:1:6, and the gas flow of boron trichloride is 20mL/min;
5) Sensitization: placing the diamond obtained in the previous step into a sensitization solution, treating for 20min at room temperature, and washing with pure water to be neutral; the sensitization liquid contains 1.0g/L tin chloride dihydrate and 40mL/L hydrochloric acid;
6) Activating: placing the diamond obtained in the previous step into an activating solution, treating for 20min at room temperature, and washing with pure water to be neutral; the activating solution contains 1.0g/L palladium chloride and 20mL/L hydrochloric acid;
7) Chemical plating: placing the diamond obtained in the previous step into a nickel plating solution at 85 ℃, stirring at a rotating speed of 300r/min, and plating nickel for 15min to obtain modified diamond; the addition amount of diamond in the nickel plating solution is 9g/L, and the nickel plating solution contains: 25g/L nickel sulfate hexahydrate, 35g/L sodium hypophosphite, 24g/L sodium acetate trihydrate, 15g/L sodium citrate;
3.2. placing the pre-plated busbar in a diamond suspension plating solution, and carrying out diamond compounding and sanding on the surface of the pre-plated busbar to obtain a diamond sand line; the sand feeding process comprises the following steps: sanding current density 5A/dm 2 Upper, upperThe sand time is 30s, and the magnetic induction intensity of the preplating busbar is 0.6mT;
the diamond suspension plating solution comprises the following components: 400g/L nickel sulfamate, 40g/L boric acid, 5g/L nickel chloride trihydrate, 15g/L diamond, pH 4.2, and temperature 57 ℃;
(4) Consolidation:
1) Adsorption: placing the diamond sand line in 0.4g/L sodium benzene sulfinate solution, treating for 15min at room temperature, and drying with nitrogen;
2) And (3) deposition: placing the diamond sand line obtained in the previous step into a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and performing deposition at 185 ℃; then sequentially cleaning with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5:2:10, and the flow of nitrogen is 100sccm; pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the cycle is 120 times.
3) Placing the diamond sand line obtained in the previous step in a consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment at 400 ℃ for 2 hours to obtain a diamond wire saw; the consolidation process comprises the following steps: consolidation current density 5A/dm 2 The consolidation time is 80s;
the consolidation plating solution comprises the following components: 400g/L nickel sulfamate, 40g/L boric acid, 5g/L nickel chloride trihydrate, 2g/L propylene glycol block polyether, pH 3.6, and temperature 57 ℃.
Comparative example 1
Step 3) in the surface modification process of 3.1. Diamond was deleted compared to example 1):
other processes were the same as in example 1, to obtain a diamond wire saw.
Comparative example 2
Step 3-4) in the surface modification process of 3.1. Diamond was deleted compared to example 1):
other processes were the same as in example 1, to obtain a diamond wire saw.
Comparative example 3
Step 3-4) in the surface modification process of 3.1. Diamond, and (4) 1) in the consolidation process were deleted as compared to example 1):
other processes were the same as in example 1, to obtain a diamond wire saw.
Comparative example 4
Step 3-4) in the surface modification process of 3.1. Diamond, and (4) 1-2) in the consolidation process were deleted as compared to example 1):
other processes were the same as in example 1, to obtain a diamond wire saw.
Experiment
The diamond wire saw obtained in examples 1 to 3 and comparative examples 1 to 4 was used to prepare test pieces, and the properties thereof were measured and the measurement results were recorded, respectively:
durability degree: a specimen having a length of 20cm was taken, and a plate glass having a thickness of 4.0mm was cut therefrom until the specimen failed. Failure manifestation form: the number of diamond in unit area is not more than 10; the durability index is as follows: cutting area (mm) 2 ) =depth of cut glass (mm) ×thickness of glass (mm);
number of brittleness: bending the samples 180 degrees, observing whether the samples are broken or not, bending each selected different part for 10 times, taking 3 bends for each sample, and taking the average value of the brittle fracture times of the 3 samples as the brittle fracture times of the samples.
Service life is as follows: and fixing the wire saw by adopting a servo motor, driving the wire saw to cut the plate glass with the thickness of 4.0mm through the reciprocating motion of the wire saw, continuously cutting for 5 minutes each time until the number of abrasive particles in a unit area is not more than 10, and recording the use times of the test sample when the test sample fails, wherein the use times are recorded as the service life.
| Durability (mm) 2 ） | Number of brittle failures (secondary) | Service life (times) | |
| Example 1 | 254 | 0 | 12 |
| Example 2 | 273 | 0 | 13 |
| Example 3 | 268 | 0 | 12 |
| Comparative example 1 | 241 | 0 | 11 |
| Comparative example 2 | 226 | 1 | 9 |
| Comparative example 3 | 215 | 1 | 9 |
| Comparative example 4 | 203 | 3 | 8 |
From the data in the above table, the following conclusions can be clearly drawn:
the diamond wire saw obtained in examples 1 to 3 was compared with the diamond wire saw obtained in comparative examples 1 to 4, and it was found that,
compared with the comparative examples, the diamond wire saw obtained in examples 1-3 has higher durability and service life data and lower brittle fracture times, which fully demonstrates that the invention realizes the improvement of the cutting capability and service life of the manufactured diamond wire saw;
compared with the example 1, the modification process of the diamond and diamond sand line in the comparative examples 1-4 is different, the durability and service life data are reduced, the brittle fracture frequency is increased, and the improvement of the cutting capability and service life of the diamond wire saw can be promoted by the arrangement of the diamond and diamond sand line modification process and the components thereof.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation process of a diamond wire saw with a composite coating is characterized by comprising the following steps: the method comprises the following steps:
(1) Pre-plating: placing a busbar steel wire in a basic plating solution, and depositing a nickel preplating layer to obtain a preplating busbar;
(2) And (3) sand feeding: placing the pre-plated busbar in a diamond suspension plating solution, and carrying out diamond compounding and sanding on the surface of the pre-plated busbar to obtain a diamond sand line;
(3) Consolidation: placing the diamond sand line in a consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment to obtain a diamond wire saw;
the diamond is subjected to surface modification, and specifically comprises the following processes:
1) Alkali washing: the diamond is placed in sodium hydroxide solution for treatment;
2) Coarsening: placing the diamond obtained in the previous step into a nitric acid solution;
3) Adsorption: placing the diamond obtained in the previous step into an ethanol solution of 0.2-0.4% propylene glycol block polyether, treating at room temperature for 10-15 min, and drying with nitrogen;
4) And (3) deposition: placing the diamond obtained in the previous step into a chemical vapor deposition device, introducing ammonia, boron trichloride, hydrogen and nitrogen, and retaining for 0.12-0.18 s at the temperature of 600-700 ℃;
5) Sensitization: placing the diamond obtained in the previous step into a sensitization solution, and treating for 15-20 min at room temperature; the sensitization liquid contains tin chloride dihydrate and hydrochloric acid;
6) Activating: placing the diamond obtained in the previous step into an activating solution, and treating for 15-20 min at room temperature; the activation liquid contains palladium chloride and hydrochloric acid;
7) Chemical plating: placing the diamond obtained in the previous step into a nickel plating solution, stirring, and plating nickel for 10-15 min to obtain modified diamond;
the diamond sand line is modified before consolidation, and specifically comprises the following processes:
1) Adsorption: placing the diamond sand line into 0.2-0.4 g/L sodium benzene sulfinate solution, treating at room temperature for 10-15 min, and drying with nitrogen;
2) And (3) deposition: and (3) placing the diamond sand line obtained in the last step into a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and depositing at the temperature of 155-185 ℃.
2. The process for preparing a diamond wire saw with composite coating according to claim 1, wherein: the pre-plating process (1) comprises the following steps: the preplating current density is 15A/dm2, and the preplating time is 30s;
the basic plating solution comprises the following components: 400-450 g/L nickel sulfamate, 40-50 g/L boric acid, 3-5 g/L nickel chloride trihydrate, pH of 4.4-4.8, and temperature of 53-57 ℃.
3. The process for preparing a diamond wire saw with composite coating according to claim 1, wherein: the sand feeding process in the step (2) comprises the following steps: the sand feeding current density is 5A/dm2, the sand feeding time is 30s, and the magnetic induction intensity of the preplating bus is 0.6mT;
the diamond suspension plating solution comprises the following components: 300-400 g/L nickel sulfamate, 30-40 g/L boric acid, 3-5 g/L nickel chloride trihydrate, 15g/L diamond, pH of 4.2-4.6 and temperature of 53-57 ℃.
4. The process for preparing a diamond wire saw with composite coating according to claim 1, wherein: the consolidation process (3) comprises the following steps: the consolidation current density is 5A/dm2, and the consolidation time is 80s;
the consolidation plating solution comprises the following components: 300-400 g/L nickel sulfamate, 30-40 g/L boric acid, 3-5 g/L nickel chloride trihydrate, pH of 3.6-4.0 and temperature of 53-57 ℃.
5. The process for preparing a diamond wire saw with composite coating according to claim 1, wherein: the heat treatment process in (3) is as follows: the temperature is 180-400 ℃ and the time is 2 hours.
6. The process for preparing a diamond wire saw with composite coating according to claim 1, wherein: the addition amount of the diamond in the nickel plating solution is 7-9 g/L, and the nickel plating solution contains: 25g/L nickel sulfate hexahydrate, 25-35 g/L sodium hypophosphite, 18-24 g/L sodium acetate trihydrate and 12-15 g/L sodium citrate.
7. The process for preparing a diamond wire saw with composite coating according to claim 1, wherein: the consolidation plating solution (3) also comprises 2g/L propylene glycol block polyether.
8. A diamond wire saw with composite coating produced by the process according to any one of claims 1 to 7.
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