CN115584540A - Diamond wire saw with composite coating and preparation process thereof - Google Patents

Diamond wire saw with composite coating and preparation process thereof Download PDF

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CN115584540A
CN115584540A CN202211506900.4A CN202211506900A CN115584540A CN 115584540 A CN115584540 A CN 115584540A CN 202211506900 A CN202211506900 A CN 202211506900A CN 115584540 A CN115584540 A CN 115584540A
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diamond
nickel
placing
wire saw
following
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CN115584540B (en
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吉国胜
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Jiangsu Sanchao Diamond Tools Co ltd
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Jiangsu Sanchao Diamond Tools Co ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10Electroplating with more than one layer of the same or of different metals
    • C25D5/12Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/12Process control or regulation
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/06Wires; Strips; Foils
    • C25D7/0607Wires

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention relates to the technical field of diamond wire saws, in particular to a diamond wire saw with a composite coating and a preparation process thereof, wherein the preparation process comprises the following steps: (1) preplating: taking a bus steel wire, placing the bus steel wire in a basic plating solution, and depositing a pre-plated nickel layer to obtain a pre-plated bus; and (2) sanding: placing the preplated bus in a diamond suspension plating solution, and compositing and sanding diamond on the surface of the preplated bus to obtain a diamond sand line; (3) consolidation: and placing the diamond sand wire in consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment to obtain the diamond fretsaw. According to the invention, the surface modification is carried out on the diamond and the diamond sand wire, the patterned deposition of boron nitride on the surface of diamond particles is realized, the exposure height and the self-sharpening property of the modified diamond in the manufactured fretsaw can be improved, the durability of the diamond fretsaw is improved, the holding force of the diamond fretsaw on the diamond and the cutting capability of the fretsaw are effectively improved, and the service life of the fretsaw is prolonged.

Description

Diamond wire saw with composite coating and preparation process thereof
Technical Field
The invention relates to the technical field of diamond wire saws, in particular to a diamond wire saw with a composite coating and a preparation process thereof.
Background
Photovoltaic power generation is an effective way for humans to convert solar energy into electrical energy for production and life. At present, the global solar cell mainly comprises a silicon-based solar cell, and accounts for more than 90% of the global photovoltaic market. With the development of semiconductor and photovoltaic industries, the requirements for cutting and processing precious 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 consolidating diamond abrasive particles on a bus bar matrix through a nickel plating layer by adopting an electrodeposition method. However, when the diameter of a bus steel wire in the diamond wire saw is small, and diamond is plated on the surface of the bus steel wire, the brittleness of the wire saw is large, and the wire saw is easy to brittle after being bent, so that the cutting efficiency and the service life of the wire saw are seriously influenced. Therefore, we propose a diamond wire saw with composite coating and its preparation process.
Disclosure of Invention
The invention aims to provide a diamond wire saw with a composite coating and a preparation process thereof, which aim 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: taking a bus steel wire, placing the bus steel wire in a basic plating solution, and depositing a pre-plated nickel layer to obtain a pre-plated bus;
(2) Sanding: placing the preplated bus in a diamond suspension plating solution, and compositing and sanding diamond on the surface of the preplated bus to obtain a diamond sand line;
(3) Consolidation: and (3) placing the diamond sand wire in consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment to obtain the diamond fretsaw.
Further, the diameter of the bus bar wire is 60 μm.
The bus steel wire is pretreated before the pre-plating process, and the method comprises the following processes:
cleaning the bus steel wire in a sodium hydroxide solution for 30-40 s, treating the bus steel wire in an sulfamic acid solution for 25-35 s after washing, drying, cleaning dirt such as oil stain on the surface of the bus steel wire, removing residual oxide layer and metal rust on the surface, keeping the surface clean and activating a matrix to ensure the electroplating quality of the subsequent bus steel wire;
the mass concentration of the sodium hydroxide solution is 6 percent, and the temperature is 55-65 ℃; the concentration of the sulfamic acid solution is 4 percent, and the treatment temperature is 35-45 ℃.
Further, the pre-plating process (1) comprises the following steps: preplating current density of 15A/dm 2 Pre-plating timeIs 30s;
the basic plating solution comprises the following components: 400-450 g/L nickel sulfamate, 40-50 g/L boric acid and 3-5 g/L nickel chloride trihydrate, wherein the pH is 4.4-4.8, and the temperature is 53-57 ℃.
Taking nickel sulfamic acid solution as pre-plating solution (basic plating solution), taking the cleaned and activated bus steel wire as a cathode and a nickel plate as an anode, and primarily plating nickel on the surface of the bus steel wire under the condition of stirring by air flow to form a pre-plated nickel layer with the thickness of about 0.3 mu m to obtain the pre-plated bus.
Further, the sand applying process (2) comprises the following steps: sanding current density of 5A/dm 2 The sanding time is 30s, and the magnetic induction intensity of the preplated 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 and 15g/L diamond, wherein the pH is 4.2-4.6, and the temperature is 53-57 ℃.
Dispersing diamond particles in nickel sulfamate plating solution as sanding plating solution, taking a preplated bus as a cathode and a nickel plate as an anode, uniformly dispersing the diamond particles in the nickel sulfamate plating solution by air flow stirring to prevent the diamond particles from settling and agglomerating, sanding, fixing the diamond particles on the surface of the preplated bus to form a sanding nickel plating layer with the thickness of about 0.8 mu m, and obtaining the diamond sand wire.
Further, the consolidation process (3) is as follows: 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 and 3-5 g/L nickel chloride trihydrate, wherein the pH is 3.6-4.0, and the temperature is 53-57 ℃.
Further, the heat treatment process in (3) is as follows: the temperature is 180-400 ℃ and the time is 2h.
Taking nickel sulfamate plating solution as thick plating solution, diamond sand wire as cathode and nickel plate as anode, and carrying out thick nickel plating under the condition of air flow stirring, thereby improving the firmness of diamond particles on the bus steel wire and forming a thick nickel plating layer with the thickness of about 1.0 mu m; and then keeping the temperature at 180-400 ℃ for 2h, drying and removing internal hydrogen to obtain the finished product of the diamond wire saw.
Furthermore, the grain diameter of the diamond is 10-20 μm, and the median diameter is 15 μm;
the diamond is subjected to surface modification, and the method specifically comprises the following processes:
1) Alkali washing: placing the diamond in a boiled sodium hydroxide solution with the mass fraction of 10% for treatment for 30min, and washing the diamond to be neutral by pure water;
2) Coarsening: placing the diamond obtained in the last step in a boiled nitric acid solution with the mass fraction of 10% for treatment for 30min, and washing the diamond with pure water to be neutral;
3) Adsorption: placing the diamond obtained in the last step into 0.2-0.4% of ethanol solution of propylene glycol block polyether, treating at room temperature for 10-15 min, and drying by nitrogen;
4) Deposition: placing the diamond obtained in the last step in a chemical vapor deposition device, introducing ammonia gas, boron trichloride, hydrogen and nitrogen, and staying for 0.12-0.18 s at the temperature of 600-700 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia gas, boron trichloride, hydrogen gas and nitrogen gas is 3;
placing the cleaned and coarsened diamond in an ethanol solution of propylene glycol block polyether, and shielding a crystal face (111) of the diamond by utilizing preferential adsorption of the propylene glycol block polyether serving as a nonionic surfactant to the crystal face (111) of the diamond, so that the crystal face (220) of the diamond is relatively exposed; and then performing chemical vapor deposition of boron nitride, so that the boron nitride can be more deposited on the (220) crystal face of the diamond, realizing patterned deposition of the boron nitride on the surface of the diamond particles by controlling the concentration of the propylene glycol block polyether solution, improving the exposure height and the self-sharpening property of the modified diamond in the manufactured wire saw, improving the durability of the diamond wire saw, and prolonging the service life and the cutting capability of the diamond wire saw.
5) Sensitization: placing the diamond obtained in the last step into sensitizing solution, processing for 15-20 min at room temperature, and washing with pure water to be neutral; the sensitizing solution contains 0.8 to 1.0g/L of tin chloride dihydrate and 30 to 40mL/L of hydrochloric acid;
6) And (3) activation: placing the diamond obtained in the last 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: putting the diamond obtained in the last step into a nickel plating solution at 85 ℃, stirring at the rotating speed of 300r/min, and plating nickel for 10-15 min to obtain a modified diamond; the addition amount of the diamond in the nickel plating solution is 7-9 g/L, and the nickel plating solution contains: 25g/L of nickel sulfate hexahydrate, 25-35 g/L of sodium hypophosphite, 18-24 g/L of sodium acetate trihydrate and 12-15 g/L of sodium citrate.
Sensitizing the diamond particles, and adsorbing a large amount of Sn by the redundant carbon atom covalent bonds on the surface of the diamond 2+ A suspension key; then activating Pb in the solution during the activation process 2+ Sn adsorbed on the surface of diamond particles 2+ Reducing the metal Pb into metal Pb, and continuously adsorbing the metal Pb on the surfaces of the diamond particles to form palladium particles. A great deal of metal palladium particles on the surface of the diamond can be used as a catalytic center of chemical nickel plating, and as the lattice structures of Pb and Ni are similar and are all face-centered cubic structures, and the lattice parameters are close, ni is added 2+ Reducing the metal into Ni atoms, depositing the Ni atoms on palladium particles on the surfaces of the diamond particles, and enabling the surfaces of the diamond abrasive particles to be completely wrapped by nickel through continuous deposition and expansion of the nickel, so that the diamond particles are metalized and endowed with conductivity;
in the sanding electroplating process, the motion of the modified diamond is influenced by the hardness of an electric field and moves towards the cathode direction, so that the contact probability between the modified diamond and the pre-plated bus is increased, and the probability that the modified diamond is captured by a plating layer is facilitated; under the action of electric field, the free electrons in the nickel are distributed on the surface, so that Ni 2+ The metal nickel is adsorbed on the modified diamond, can grow on the surface of the preplated bus, also can grow on the surface of the modified diamond and the joint of the preplated layer, and is fixedly connected on the surface of the preplated layer through a metal bond, so that the holding force of the prepared diamond wire saw on the modified diamond and the cutting capacity of the wire saw can be greatly improved, and the service life of the wire saw is prolonged.
Further, the step (3) of modifying before the consolidation process specifically comprises the following steps:
1) Adsorption: placing the diamond sand line in 0.2-0.4 g/L sodium benzene sulfinate solution, treating for 10-15 min at room temperature, and drying by nitrogen;
2) Deposition: 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 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5; the pulse time of the molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the circulation is carried out for 80 to 120 times.
Placing the diamond sand line obtained after sanding in a benzene sulfinic acid sodium solution, and shielding crystal faces (220) and (311) of the metal nickel by utilizing preferential adsorption of the benzene sulfinic acid sodium to the crystal faces so as to relatively expose crystal faces (111) and (200) of the diamond; 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 more deposited on (111) crystal faces of metal nickel in the modified diamond nickel coating and the pre-coating in the diamond yarn, the longitudinal friction of the manufactured diamond wire saw can be reduced, the brittle fracture of the wire saw caused by stress is relieved, the holding force of the diamond wire saw on the modified diamond is improved, and the service life of the wire saw is prolonged.
Further, the consolidation plating solution (3) also comprises 2g/L of propylene glycol block polyether. So that the plating layer presents obvious preferred orientation, the uniformity of the thick nickel plating layer structure is improved, the firmness and the stability of the modified diamond on the bus steel wire are more facilitated, the holding force of the diamond wire saw on the modified diamond is improved, the cutting capability of the wire saw is improved, the service life of the wire saw is prolonged,
compared with the prior art, the invention has the following beneficial effects:
according to the diamond fretsaw with the composite coating and the preparation process thereof, the patterned deposition of boron nitride on the surface of diamond particles is realized by performing surface modification on the diamond and the diamond sand wire, the exposure height and the self-sharpening property of the modified diamond in the fretsaw can be improved, the durability of the diamond fretsaw is improved, the holding force of the diamond fretsaw on the diamond and the cutting capability of the fretsaw are effectively improved, and the service life of the diamond fretsaw is prolonged.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
(1) Pretreatment:
placing the bus steel wire in a sodium hydroxide solution for cleaning for 30s, placing the bus steel wire in an aminosulfonic acid solution for treating for 30s after water cleaning, washing 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:
taking a bus steel wire, placing the bus steel wire in a basic plating solution, and depositing a pre-plated nickel layer to obtain a pre-plated bus; the pre-plating process comprises the following steps: preplating current density of 15A/dm 2 The pre-plating time is 30s; the basic plating solution comprises the following components: 400g/L of nickel sulfamate, 40g/L of boric acid and 3g/L of nickel chloride trihydrate, wherein the pH is 4.8, and the temperature is 53 ℃;
(3) Sanding:
3.1. surface modification of diamond:
1) Alkali washing: placing the diamond in a boiled sodium hydroxide solution with the mass fraction of 10% for treatment for 30min, and washing the diamond to be neutral by pure water;
2) Coarsening: placing the diamond obtained in the last step in a boiled nitric acid solution with the mass fraction of 10% for treatment for 30min, and washing the diamond with pure water to be neutral;
3) Adsorption: placing the diamond obtained in the last step in 0.2% propylene glycol block polyether ethanol solution, treating for 10min at room temperature, and drying with nitrogen;
4) Deposition: placing the diamond obtained in the last step in a chemical vapor deposition device, introducing ammonia gas, boron trichloride, hydrogen and nitrogen, and staying for 0.12s at the temperature of 600 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia gas, boron trichloride, hydrogen gas and nitrogen gas is 3;
5) Sensitization: placing the diamond obtained in the last step in sensitizing solution, treating for 15min at room temperature, and washing with pure water to neutrality; the sensitizing solution contains 0.8g/L of tin chloride dihydrate and 30mL/L of hydrochloric acid;
6) And (3) activation: placing the diamond obtained in the last step in 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: putting the diamond obtained in the last step into a nickel plating solution at 85 ℃, stirring at a rotating speed of 300r/min, and plating nickel for 10min to obtain a modified diamond; the addition amount of the diamond in the nickel plating solution is 7g/L, and the nickel plating solution contains: 25g/L of nickel sulfate hexahydrate, 25g/L of sodium hypophosphite, 18g/L of sodium acetate trihydrate and 12g/L of sodium citrate;
3.2. placing the preplated bus in a diamond suspension plating solution, and compositing and sanding diamond on the surface of the preplated bus to obtain a diamond sand line; the sanding process comprises the following steps: sanding current density of 5A/dm 2 The sanding time is 30s, and the magnetic induction intensity of the preplated bus is 0.6mT; the diamond suspension plating solution comprises the following components: 300g/L of nickel sulfamate, 30g/L of boric acid, 3g/L of nickel chloride trihydrate and 15g/L of diamond, wherein the pH is 4.6, and the temperature is 53 ℃;
(4) Consolidation:
1) Adsorption: placing the diamond sand line in 0.2g/L sodium benzene sulfinate solution, treating for 10min at room temperature, and drying by nitrogen;
2) Deposition: placing the diamond sand line obtained in the last step in a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and depositing at the temperature of 155 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5; the pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the circulation is carried out for 80 times.
3) Putting the diamond sand wire obtained in the last step into consolidation plating solutionDepositing a thick nickel plating layer, and carrying out heat treatment at 180 ℃ for 2h to obtain the diamond wire saw; the consolidation process comprises the following steps: consolidation current density of 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 and 2g/L propylene glycol block polyether, wherein the pH is 4.0, and the temperature is 53 ℃.
Example 2
(2) Pre-plating:
taking a bus steel wire, placing the bus steel wire in a basic plating solution, and depositing a pre-plated nickel layer to obtain a pre-plated bus; the pre-plating process comprises the following steps: preplating current density of 15A/dm 2 The pre-plating time is 30s; the basic plating solution comprises the following components: 420g/L of nickel sulfamate, 45g/L of boric acid and 4g/L of nickel chloride trihydrate, wherein the pH is 4.6, and the temperature is 55 ℃;
(3) Sanding:
3.1. surface modification of diamond:
1) Alkali washing: placing the diamond in a boiled sodium hydroxide solution with the mass fraction of 10% for treatment for 30min, and washing the diamond to be neutral by pure water;
2) Coarsening: placing the diamond obtained in the last step in a boiled nitric acid solution with the mass fraction of 10% for treatment for 30min, and washing the diamond with pure water to be neutral;
3) Adsorption: placing the diamond obtained in the last step in 0.3% propylene glycol block polyether ethanol solution, treating at room temperature for 12min, and drying with nitrogen;
4) Deposition: placing the diamond obtained in the last step in a chemical vapor deposition device, introducing ammonia gas, boron trichloride, hydrogen and nitrogen, and staying for 0.15s at the temperature of 650 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia gas, boron trichloride, hydrogen gas and nitrogen gas is 3;
5) Sensitization: placing the diamond obtained in the last step in sensitizing solution, treating at room temperature for 18min, and washing with pure water to neutrality; the sensitizing solution contains 0.9g/L of tin chloride dihydrate and 35mL/L of hydrochloric acid;
6) Activation: placing the diamond obtained in the last step in an activating solution, treating at room temperature for 18min, 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: putting the diamond obtained in the last step into a nickel plating solution at 85 ℃, stirring at a rotating speed of 300r/min, and plating nickel for 12min to obtain a modified diamond; the addition amount of the diamond in the nickel plating solution is 8g/L, and the nickel plating solution contains: 25g/L of nickel sulfate hexahydrate, 30g/L of sodium hypophosphite, 21g/L of sodium acetate trihydrate and 13g/L of sodium citrate;
3.2. placing the preplated bus in a diamond suspension plating solution, and compositing and sanding diamond on the surface of the preplated bus to obtain a diamond sand line; the sanding process comprises the following steps: sanding current density of 5A/dm 2 The sanding time is 30s, and the magnetic induction intensity of the preplated bus is 0.6mT;
the diamond suspension plating solution comprises the following components: 350g/L of nickel sulfamate, 35g/L of boric acid, 4g/L of nickel chloride trihydrate and 15g/L of diamond, wherein the pH is 4.4, and the temperature is 55 ℃;
(4) Consolidation:
1) Adsorption: placing the diamond sand line in 0.3g/L sodium benzene sulfinate solution, treating for 12min at room temperature, and drying by nitrogen;
2) Deposition: placing the diamond sand line obtained in the last step in a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and depositing at the temperature of 170 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5; the pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the circulation is performed for 100 times.
3) Placing the diamond sand wire obtained in the last step in consolidation plating solution, depositing a thick nickel plating layer, and carrying out heat treatment at 300 ℃ for 2h to obtain a diamond wire saw; the consolidation process comprises the following steps: consolidation current density of 5A/dm 2 The consolidation time is 80s;
the consolidation plating solution comprises the following components: 350g/L of nickel sulfamate, 35g/L of boric acid, 4g/L of nickel chloride trihydrate and 2g/L of propylene glycol block polyether, wherein the pH is 3.8, and the temperature is 55 ℃.
Example 3
(2) Pre-plating:
taking out the steel wire of the bus bar,placing the bus bar in a basic plating solution, and depositing a pre-plated nickel layer to obtain a pre-plated bus bar; the pre-plating process comprises the following steps: preplating current density of 15A/dm 2 The pre-plating time is 30s;
the basic plating solution comprises the following components: 450g/L of nickel sulfamate, 50g/L of boric acid and 5g/L of nickel chloride trihydrate, wherein the pH is 4.4, and the temperature is 57 ℃;
(3) Sanding:
3.1. surface modification of diamond:
1) Alkali washing: placing the diamond in a boiled sodium hydroxide solution with the mass fraction of 10% for treatment for 30min, and washing the diamond to be neutral by pure water;
2) Coarsening: placing the diamond obtained in the last step in a boiled nitric acid solution with the mass fraction of 10% for treatment for 30min, and washing the diamond with pure water to be neutral;
3) Adsorption: placing the diamond obtained in the last step in 0.4% propylene glycol block polyether ethanol solution, treating for 15min at room temperature, and drying with nitrogen;
4) Deposition: placing the diamond obtained in the last step in a chemical vapor deposition device, introducing ammonia gas, boron trichloride, hydrogen and nitrogen, and staying for 0.18s at the temperature of 700 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the pressure is 4.5kPa, the flow ratio of ammonia gas, boron trichloride, hydrogen gas and nitrogen gas is 3;
5) Sensitization: placing the diamond obtained in the last step in sensitizing solution, treating at room temperature for 20min, and washing with pure water to neutrality; the sensitizing solution contains 1.0g/L of tin chloride dihydrate and 40mL/L of hydrochloric acid;
6) And (3) activation: placing the diamond obtained in the last step in an activating solution, treating at room temperature for 20min, 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: putting the diamond obtained in the last step into a nickel plating solution at 85 ℃, stirring at the rotating speed of 300r/min, and plating nickel for 15min to obtain a modified diamond; the addition amount of the 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 and 15g/L sodium citrate;
3.2. placing the preplated bus in a diamond suspension plating solution, and compositing and sanding diamond on the surface of the preplated bus to obtain a diamond sand line; the sanding process comprises the following steps: sanding current density of 5A/dm 2 The sanding time is 30s, and the magnetic induction intensity of the preplated bus is 0.6mT;
the diamond suspension plating solution comprises the following components: 400g/L of nickel sulfamate, 40g/L of boric acid, 5g/L of nickel chloride trihydrate and 15g/L of diamond, wherein the pH is 4.2, and the temperature is 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 by nitrogen;
2) Deposition: placing the diamond sand line obtained in the last step in a deposition device, introducing molybdenum hexacarbonyl, hydrogen sulfide and nitrogen, and depositing at 185 ℃; then sequentially washing with absolute ethyl alcohol and pure water;
the flow ratio of molybdenum hexacarbonyl, hydrogen sulfide and nitrogen is 5; the pulse time of molybdenum hexacarbonyl/nitrogen/hydrogen sulfide/nitrogen is 5s/10s/7s/10s, and the circulation is performed for 120 times.
3) Placing the diamond sand wire obtained in the last step in consolidation plating solution, depositing a thick nickel plating layer, and carrying out heat treatment at 400 ℃ for 2h to obtain a diamond wire saw; the consolidation process comprises the following steps: consolidation current density of 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 and 2g/L propylene glycol block polyether, wherein the pH is 3.6, and the temperature is 57 ℃.
Comparative example 1
Compared to example 1, 3.1. Step 3 of the surface modification process of diamond) was eliminated:
the other process was the same as in example 1 to obtain a diamond wire saw.
Comparative example 2
Compared to example 1, 3.1. Step 3-4 of the surface modification process of diamond) was eliminated:
the other process was the same as in example 1 to obtain a diamond wire saw.
Comparative example 3
Compared to example 1, 3.1. Steps 3-4 in the surface modification process of diamond, and (4) 1 in the consolidation process) were deleted:
the other processes were the same as in example 1 to obtain a diamond wire saw.
Comparative example 4
Compared to example 1, 3.1. Steps 3-4 in the surface modification process of diamond, and (4) 1-2 in the consolidation process) were deleted:
the other process was the same as in example 1 to obtain a diamond wire saw.
Experiment of the invention
Samples were prepared from the diamond wire saws obtained in examples 1 to 3 and comparative examples 1 to 4, and the performance thereof was measured and the measurement results were recorded:
durability: a20 cm long sample was taken and used to cut a 4.0mm thick sheet of glass until the sample failed. The failure manifestation is as follows: the number of diamonds in a unit area is not more than 10; the durability index is: cutting area (mm) 2 ) = depth (mm) of cut glass × thickness (mm) of glass;
brittleness times: bending the samples by 180 degrees, observing whether the samples are broken, bending each selected different part for 10 times, taking 3 bends for each sample, and taking the average value of the brittle failure times of the 3 samples as the brittle failure times of the samples.
Service life: a servo motor is adopted to fix the fretsaw, the fretsaw is driven to cut the plate glass with the thickness of 4.0mm through reciprocating motion of the fretsaw, each cutting lasts for 5min until the number of the abrasive particles in a unit area is not more than 10, the using times of the sample when the sample fails are recorded, and the service life is recorded.
Durability (mm) 2 Number of brittle fracture (times) 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 table above, it is clear that the following conclusions can be drawn:
in comparison with the diamond wire saws obtained in comparative examples 1 to 4, the diamond wire saws obtained in examples 1 to 3 showed that,
compared with the comparative example, the diamond wire saws obtained in the examples 1 to 3 have higher durability and service life data and lower brittle failure times, which fully shows that the invention realizes the improvement of the cutting capability and the service life of the prepared diamond wire saw;
compared with the example 1, the modification process of the diamond and the diamond sand wire in the comparative examples 1 to 4 is different from the modification process of the diamond and the diamond sand wire, the durability and the service life data are reduced, and the brittle failure times are increased.
It is noted that, herein, relational terms such as first and second, and the like may be 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. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process item 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 item or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent change and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation process of a diamond wire saw with a composite coating is characterized in that: the method comprises the following processes:
(1) Pre-plating: taking a bus steel wire, placing the bus steel wire in a basic plating solution, and depositing a pre-plated nickel layer to obtain a pre-plated bus;
(2) Sanding: placing the pre-plated bus in a diamond suspension plating solution, and coating sand on the diamond to the surface of the pre-plated bus to obtain a diamond sand line;
(3) Consolidation: and (3) placing the diamond sand wire in consolidation plating solution, depositing a thick nickel plating layer, and performing heat treatment to obtain the diamond fretsaw.
2. The process for preparing the diamond wire saw with the composite coating according to claim 1, wherein the process comprises the following steps: the pre-plating process (1) comprises the following steps: the pre-plating current density is 15A/dm 2 The pre-plating time is 30s;
the basic plating solution comprises the following components: 400-450 g/L nickel sulfamate, 40-50 g/L boric acid and 3-5 g/L nickel chloride trihydrate, wherein the pH is 4.4-4.8, and the temperature is 53-57 ℃.
3. The process for preparing the diamond wire saw with the composite coating according to claim 1, wherein the process comprises the following steps: the sand feeding process (2) comprises the following steps: sanding current density of 5A/dm 2 The sanding time is 30s, and the magnetic induction intensity of the preplated 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 and 15g/L diamond, wherein the pH is 4.2-4.6, and the temperature is 53-57 ℃.
4. The process for preparing the diamond wire saw with the composite coating according to claim 1, wherein the process comprises the following steps: 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 and 3-5 g/L nickel chloride trihydrate, wherein the pH is 3.6-4.0, and the temperature is 53-57 ℃.
5. The process for preparing the diamond wire saw with the composite coating according to claim 1, wherein the process comprises the following steps: the heat treatment process in the step (3) comprises the following steps: the temperature is 180-400 ℃ and the time is 2h.
6. The process for preparing the diamond wire saw with the composite coating according to claim 1, wherein the process comprises the following steps: the diamond is subjected to surface modification, and the method specifically comprises the following processes:
1) Alkali washing: putting the diamond into a sodium hydroxide solution for treatment;
2) Coarsening: putting the diamond obtained in the last step into a nitric acid solution;
3) Adsorption: placing the diamond obtained in the last step into 0.2-0.4% of ethanol solution of propylene glycol block polyether, treating for 10-15 min at room temperature, and drying by nitrogen;
4) Deposition: placing the diamond obtained in the last step in a chemical vapor deposition device, introducing ammonia gas, boron trichloride, hydrogen and nitrogen, and staying for 0.12-0.18 s at the temperature of 600-700 ℃;
5) Sensitization: placing the diamond obtained in the last step into sensitizing solution, and processing for 15-20 min at room temperature; the sensitizing solution contains tin chloride dihydrate and hydrochloric acid;
6) Activation: placing the diamond obtained in the last step into an activating solution, and treating for 15-20 min at room temperature; the activating solution contains palladium chloride and hydrochloric acid;
7) Chemical plating: and (3) putting the diamond obtained in the last step into a nickel plating solution, stirring and plating nickel for 10-15 min to obtain the modified diamond.
7. The process for preparing the diamond wire saw with the composite coating according to claim 6, wherein the diamond wire saw comprises the following steps: the addition amount of the diamond in the nickel plating solution is 7-9 g/L, and the nickel plating solution contains: 25g/L of nickel sulfate hexahydrate, 25-35 g/L of sodium hypophosphite, 18-24 g/L of sodium acetate trihydrate and 12-15 g/L of sodium citrate.
8. The process for preparing the diamond wire saw with the composite coating according to claim 1, wherein the process comprises the following steps: the diamond sand line is modified before consolidation, and the method specifically comprises the following processes:
1) Adsorption: placing the diamond sand line in 0.2-0.4 g/L sodium benzene sulfinate solution, treating for 10-15 min at room temperature, and drying by nitrogen;
2) 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 ℃.
9. The process for preparing the diamond wire saw with the composite coating according to claim 8, wherein the diamond wire saw comprises the following steps: the consolidation plating solution (3) also comprises 2g/L propylene glycol block polyether.
10. A diamond wire saw with a composite coating prepared by the preparation process according to any one of claims 1 to 9.
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