CN107699938B - Preparation process of diamond cutting line - Google Patents
Preparation process of diamond cutting line Download PDFInfo
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- CN107699938B CN107699938B CN201710969360.6A CN201710969360A CN107699938B CN 107699938 B CN107699938 B CN 107699938B CN 201710969360 A CN201710969360 A CN 201710969360A CN 107699938 B CN107699938 B CN 107699938B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
- B28D5/045—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools by cutting with wires or closed-loop blades
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- 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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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- 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
- C25D5/48—After-treatment of electroplated surfaces
-
- 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 provides a preparation process of a diamond cutting wire, which comprises the following steps: (1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire; (2) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting line; (3) and (3) wiring the crude product of the diamond cutting line obtained in the step (2) in ionic liquid to prepare the diamond cutting line. The diamond in the step (1) is prepared by adopting a microwave plasma chemical vapor deposition method, wherein the main parameters are as follows: using p-type Si (100) single crystal wafer as substrate and CH4/H2The system is used as a gas source, wherein the substrate temperature is divided into two stages, the substrate temperature in the first stage is 650 ℃, and the substrate temperature in the second stage is 720 ℃.
Description
Technical Field
The invention relates to the field of steel wire cutting, in particular to a preparation process of a diamond cutting wire.
Background
Diamond cutting wires are also known as diamond wires, also known as diamond cutting wires or diamond wires. At present, the mainstream silicon slice cutting line used in the photovoltaic field is an ultra-fine cutting steel wire, the diameter of the cutting steel wire is about 120 microns, the raw material adopts high-carbon steel, and the material quality is different from 80C, 86C and 90C. Diamond cutting wires have their own advantages: the high-speed cutting can be realized, the cutting speed can be improved to 2 times of the original cutting speed, and the time consumption is reduced naturally; and in the environment-friendly production, only water or water-based cooling cleaning solution is needed in the cutting process of the gold and steel wire, so that the environment-friendly production and manufacturing are really realized.
The diamond cutting wire is still a relatively new technology at present and has not yet been popularized, the main diamond wire depends on import, the supply of the diamond wire of local companies in China is less, so the price is higher, and the price of the diamond material is much higher than that of a copper-plated zinc-plated material. Meanwhile, the diamond wire is too thick to cause a large loss of the silicon wafer. The loss of the silicon chip is directly related to the thickness of the cutting line, and the thicker the silicon chip, the more the silicon chip naturally loses. The cutting wire that is currently the mainstream is a super fine cutting wire, about 120um in diameter. Whereas the diameter of the diamond wire in practical use is about 250um, which is more than twice that of the ultra-fine cutting wire. Due to the existence of the diamond, the conversion efficiency of the crystalline silicon battery piece is low due to the fact that cutting marks exist after cutting.
In view of the above problems, the present invention provides a process for manufacturing a diamond cutting wire, which can solve the above problems.
Disclosure of Invention
The invention provides a preparation process of a diamond cutting wire, which comprises the following steps:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting line;
(3) and (3) wiring the crude product of the diamond cutting line obtained in the step (2) in ionic liquid to prepare the diamond cutting line.
As an embodiment of the present invention, the diamond in step (1) is prepared by using a microwave plasma chemical vapor deposition method, wherein the main parameters are as follows:
using p-type Si (100) single crystal wafer as substrate and CH4/H2The system is used as a gas source, wherein the temperature of the substrate is divided into two stages, the temperature of the substrate in the first stage is 650 ℃, and the temperature of the substrate in the second stage is 720 ℃;
when the temperature of the substrate is 650 ℃, the power of the microwave is 3500W, the deposition air pressure is 2.3kPa, and the deposition time is 4 h; when the temperature of the substrate is 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, and the deposition time is 0.5 h.
As an embodiment of the present invention, the CH4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm.
As an embodiment of the present invention, the pretreatment liquid is prepared from raw materials including:
80-100 parts of water, 5-10 parts of zinc polyacrylate, 0.1-3 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.1 part of stearyl trimethyl ammonium bromide.
As an embodiment of the present invention, the pretreatment liquid is prepared from raw materials including:
90-100 parts of water, 5-8 parts of zinc polyacrylate, 0.1-2 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.05 part of stearyl trimethyl ammonium bromide.
As an embodiment of the present invention, the pretreatment liquid is prepared from raw materials including:
99 parts of water, 5 parts of zinc polyacrylate, 0.15 part of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.02 part of stearyl trimethyl ammonium bromide.
As an embodiment of the present invention, the preparation method of the zinc polyacrylate comprises the following steps:
adding 1 weight part of zinc chloride solution into 2 weight parts of acrylic acid under stirring, adjusting the pH value of the reaction solution to 9 by ammonia water, adding 0.1 part of ammonium persulfate with 0.5g/ml and 0.1 part of sodium bisulfite solution with 0.5g/ml after stirring uniformly, placing in a water bath at 60 ℃ for reacting for 4 hours to obtain light yellow gel, vacuumizing and drying in a vacuum oven at 60 ℃, and crushing.
In one embodiment of the present invention, the electroplating solution electroplated in step (2) includes water, a boric acid solution, anhydrous nickel dichloride, and sodium picryl sulfonate.
As an embodiment of the present invention, the ionic liquid is 1-carboxymethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt.
A second aspect of the present invention provides a diamond cutting wire produced by the above-described process for producing a diamond cutting wire.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1: the scanning electron microscope image (JSM-IT100 multifunctional scanning electron microscope) of the diamond prepared by the microwave plasma chemical vapor deposition method is provided.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" embraces the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer".
"interpolymer" means a polymer prepared by polymerizing at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is generally used to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is generally used to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing four or more monomers. "blend" means a polymer formed by two or more polymers being mixed together by physical or chemical means.
The invention provides a preparation process of a diamond cutting wire, which comprises the following steps:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting line;
(3) and (3) wiring the crude product of the diamond cutting line obtained in the step (2) in ionic liquid to prepare the diamond cutting line.
Diamond
Diamond is commonly known as "diamond". That is, the original body of diamond, which is a mineral composed of carbon elements, is a particulate matter composed of elementary elements in nature, and is a carbon allotrope (diamond, graphene, fullerene, carbon nanotube, sudachi, etc.).
Diamond is currently the hardest of the many naturally occurring substances found on the earth, and diamond is not produced only on the earth, but is found in the anagenic phase of diamond in the meteorites of the celestial body.
Diamond is used in a wide variety of applications, for example: artware and cutting tools in industry.
The diamond film is prepared by two methods, namely Thermal Chemical Vapor Deposition (TCVD) and Plasma Chemical Vapor Deposition (PCVD). The diamond film developed is being studied and used as wear-resistant coating, acoustic diaphragm, optical window, and high-heat-conductivity substrate of integrated circuit.
Conventional diamond used on a steel wire is generally plated with granular diamond by an electroplating method, and the diamond wire prepared by the method is thick and has a rough cutting surface.
The invention provides a preparation method of diamond, which is mainly prepared by a microwave plasma chemical vapor deposition Method (MPCVD).
The microwave plasma (CVD) is characterized in that a quartz tube is used as a reaction chamber, reaction gas sources such as methane and hydrogen are input from the top of the reaction chamber, a substrate for deposition is placed on a substrate seat, microwaves with the frequency of 2.45GHz or 915MHz are input from a waveguide tube in the middle of the reaction chamber to form a glow discharge area, and diamond is deposited on the substrate.
The microwave plasma CVD method can use a high-intensity microwave source to excite a gas source above a substrate to generate plasma, so as to realize the deposition of diamond.
The diamond prepared by the method is in a nano film structure, so that the prepared diamond wire can reach the hyperfine level, has a smooth surface and can meet the cutting requirement on the market.
As an embodiment of the invention, the main experimental parameters of the microwave plasma chemical vapor deposition are as follows:
using p-type Si (100) single crystal wafer as substrate and CH4/H2The system is used as a gas source, wherein the temperature of the substrate is divided into two stages, the temperature of the substrate in the first stage is 650 ℃, and the temperature of the substrate in the second stage is 720 ℃;
when the temperature of the substrate is 650 ℃, the power of the microwave is 3500W, the deposition air pressure is 2.3kPa, and the deposition time is 4 h; when the temperature of the substrate is 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, and the deposition time is 0.5 h.
The CH4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm.
In the invention, the diamond preparation by microwave plasma chemical vapor deposition is divided into two stages, the substrate temperature in the first stage is 650 ℃, the microwave power is 3500W, the deposition pressure is 2.3kPa, the deposition time is 4h, and the CH is4/H2In the systemThe concentration of each gas is: h2Is 200sccm, CH4Is 15 sccm; after the reaction is finished, when the temperature of the substrate is adjusted to be 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, the deposition time is 0.5h, and the CH is4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm.
In the invention, the structure of the diamond prepared by two stages is a composite structure, namely, diamond particles are compounded on the surface of the diamond film, and the diamond shape is a shape which is not found in the prior stage.
Pretreatment liquid
The preparation raw materials of the pretreatment solution comprise:
80-100 parts of water, 5-10 parts of zinc polyacrylate, 0.1-3 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.1 part of stearyl trimethyl ammonium bromide.
As an embodiment of the present invention, the pretreatment liquid is prepared from raw materials including:
90-100 parts of water, 5-8 parts of zinc polyacrylate, 0.1-2 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.05 part of stearyl trimethyl ammonium bromide.
As an embodiment of the present invention, the pretreatment liquid is prepared from raw materials including: 99 parts of water, 5 parts of zinc polyacrylate, 0.15 part of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.02 part of stearyl trimethyl ammonium bromide.
As an embodiment of the present invention, the preparation method of the zinc polyacrylate comprises the following steps: adding 1 weight part of zinc chloride solution into 2 weight parts of acrylic acid under stirring, adjusting the pH value of the reaction solution to 9 by ammonia water, adding 0.1 part of ammonium persulfate with 0.5g/ml and 0.1 part of sodium bisulfite solution with 0.5g/ml after stirring uniformly, placing in a water bath at 60 ℃ for reacting for 4 hours to obtain light yellow gel, vacuumizing and drying in a vacuum oven at 60 ℃, and crushing.
Electroplating of
The plating test in the present invention was carried out under ultrasonic waves.
The electroplating solution in the electroplating process comprises water, boric acid solution, anhydrous nickel dichloride and sodium picryl sulfonate.
In one embodiment of the present invention, the plating solution comprises the following components in parts by weight: 50 parts by weight of water, 1.5 parts by weight of boric acid solution, 15 parts by weight of anhydrous nickel dichloride and 12 parts by weight of sodium picryl sulfonate.
The concentration of the boric acid solution is 35 g/L.
The test parameters of the electroplating are as follows: the pH value of the electroplating solution is 3.5, and the current density is 2.5A/dm2The temperature of the plating solution is 42 ℃, the plating time is 0.5h, and the frequency of the ultrasonic wave is 25 KHZ.
Electroplating the pretreated metal wire to obtain a crude product of the diamond cutting wire.
Ionic liquids
Ionic liquids (or ionic liquids) are liquids composed entirely of ions, such as KCI at high temperature, KOH in liquid state, and they are ionic liquids. A substance composed of ions which is liquid at or around room temperature is called a room-temperature ionic liquid or a room-temperature molten salt.
The ionic liquid is a salt which is in a liquid state at or near room temperature and is completely composed of anions and cations, and is also called low-temperature molten salt. The main reason why the ionic liquid is used as an ionic compound and has a low melting point is that ions cannot be regularly accumulated into crystals due to the asymmetry of certain substituents in the structure of the ionic liquid. The anion ion exchange resin is generally composed of organic cations and inorganic or organic anions, wherein common cations comprise quaternary ammonium salt ions, quaternary phosphonium salt ions, imidazolium salt ions, pyrrole salt ions and the like, and anions comprise halogen ions, tetrafluoroborate ions, hexafluorophosphate ions and the like.
According to the invention, the prepared crude product of the diamond cutting line is wired in the ionic liquid, so that the diamond cutting line can be prepared. In the invention, the ionic liquid is 1-carboxymethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt.
According to the invention, the mass ratio of the diamond to the pretreatment liquid in the treatment liquid A is 1: 4.
in one embodiment of the present invention, the metal wire rod is subjected to an acid washing step before being run in the treatment solution a.
The pickling step comprises the following steps:
a) completely immersing the metal wire into a pickling tank, wherein the time control range is as follows: 3-5 minutes;
b) washing the metal wire in the step a) with clear water;
c) adding an acid washing solution into an acid washing tank, completely immersing the metal wire in the step b) into the acid washing solution, and controlling the time within the range: 3-5 minutes;
d) and (3) washing the surface of the metal wire by using water, and washing the residual pickling solution on the surface of the metal wire.
The preparation raw materials of the pickling solution comprise the following components in percentage by mass: h2SO415 wt%, thiourea 0.1 wt%, zinc L-aspartate 1 wt% and the balance water.
As an embodiment of the present invention, the metal wire is a stainless steel wire having a diameter of 0.14 mm.
The mechanism is explained as follows: the nano-diamond prepared by the conventional microwave plasma chemical vapor deposition method is required to have smooth surface and high quality. According to the invention, the nano-diamond prepared by microwave plasma chemical vapor deposition is compounded with diamond particles on a smooth surface, and after the diamond particles with the morphology are mixed with the metal wire, the cutting efficiency of the diamond wire can be improved, and the roughness of the cut surface is greatly improved; the diameter of the obtained diamond wire also meets the requirement of the ultra-fine cutting steel wire; and the invention increases the acting force between the diamond and the metal wire by wiring in the ionic liquid at the later stage and the acting force between the negative and positive ions, and can make up for the overlarge concave-convex between the diamonds and improve the cutting efficiency.
Embodiment 1: the embodiment provides a preparation process of a diamond cutting wire, which comprises the following steps:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting line;
(3) and (3) wiring the crude product of the diamond cutting line obtained in the step (2) in ionic liquid to prepare the diamond cutting line.
Embodiment 2. the process for preparing a diamond cutting wire according to embodiment 1, wherein the diamond in step (1) is prepared by microwave plasma chemical vapor deposition, wherein the main parameters are as follows:
using p-type Si (100) single crystal wafer as substrate and CH4/H2The system is used as a gas source, wherein the temperature of the substrate is divided into two stages, the temperature of the substrate in the first stage is 650 ℃, and the temperature of the substrate in the second stage is 720 ℃;
when the temperature of the substrate is 650 ℃, the power of the microwave is 3500W, the deposition air pressure is 2.3kPa, and the deposition time is 4 h; when the temperature of the substrate is 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, and the deposition time is 0.5 h.
Embodiment 3. Process for preparing a diamond-cutting wire according to embodiment 2, wherein CH4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm.
Embodiment 4. the process of preparing a diamond cutting wire according to embodiment 1, wherein the pretreatment liquid is prepared from a raw material comprising:
80-100 parts of water, 5-10 parts of zinc polyacrylate, 0.1-3 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.1 part of stearyl trimethyl ammonium bromide.
Embodiment 5 the process of preparing a diamond-cutting wire according to embodiment 3, wherein the pretreatment liquid is prepared from a raw material comprising:
90-100 parts of water, 5-8 parts of zinc polyacrylate, 0.1-2 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.05 part of stearyl trimethyl ammonium bromide.
Embodiment 6 the process of preparing a diamond-cutting wire according to embodiment 3, wherein the pretreatment liquid is prepared from a raw material comprising:
99 parts of water, 5 parts of zinc polyacrylate, 0.15 part of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.02 part of stearyl trimethyl ammonium bromide.
Embodiment 7 is the process for manufacturing a diamond-cutting wire according to embodiment 3, wherein the zinc polyacrylate is prepared by the following steps:
adding 1 weight part of zinc chloride solution into 2 weight parts of acrylic acid under stirring, adjusting the pH value of the reaction solution to 9 by ammonia water, adding 0.1 part of ammonium persulfate with 0.5g/ml and 0.1 part of sodium bisulfite solution with 0.5g/ml after stirring uniformly, placing in a water bath at 60 ℃ for reacting for 4 hours to obtain light yellow gel, vacuumizing and drying in a vacuum oven at 60 ℃, and crushing.
Embodiment 8 is the process of preparing a diamond-cutting wire according to embodiment 1, wherein the plating solution plated in the step (2) includes water, a boric acid solution, anhydrous nickel dichloride, and sodium picryl sulfonate.
Embodiment 9. the process of preparing a diamond cutting wire according to embodiment 1, wherein the ionic liquid is 1-carboxymethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt.
Embodiment 10 this embodiment provides a diamond cutting wire produced by the process for producing a diamond cutting wire according to any one of embodiments 1 to 9.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Example 1: the embodiment provides a preparation process of a diamond cutting wire, which comprises the following steps:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting line;
(3) and (3) wiring the crude product of the diamond cutting line obtained in the step (2) in ionic liquid to prepare the diamond cutting line.
In the step (1)
The diamond is prepared by adopting a microwave plasma chemical vapor deposition method, and the specific preparation parameters are as follows:
the substrate temperature in the first stage is 650 ℃, the microwave power is 3500W, the deposition gas pressure is 2.3kPa, the deposition time is 4h, and the CH is4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm; after the reaction is finished, when the temperature of the substrate is adjusted to be 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, the deposition time is 0.5h, and the CH is4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm.
Using p-type Si (100) single crystal wafer as substrate and CH4/H2The system is used as a gas source, wherein the temperature of the substrate is divided into two stages, the temperature of the substrate in the first stage is 650 ℃, and the temperature of the substrate in the second stage is 720 ℃;
when the temperature of the substrate is 650 ℃, the power of the microwave is 3500W, the deposition air pressure is 2.3kPa, and the deposition time is 4 h; when the temperature of the substrate is 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, and the deposition time is 0.5 h.
The preparation raw materials of the pretreatment solution comprise: 99 parts of water, 5 parts of zinc polyacrylate, 0.15 part of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.02 part of stearyl trimethyl ammonium bromide.
The preparation method of the zinc polyacrylate comprises the following steps: adding 1 weight part of zinc chloride solution into 2 weight parts of acrylic acid under stirring, adjusting the pH value of the reaction solution to 9 by ammonia water, adding 0.1 part of ammonium persulfate with 0.5g/ml and 0.1 part of sodium bisulfite solution with 0.5g/ml after stirring uniformly, placing in a water bath at 60 ℃ for reacting for 4 hours to obtain light yellow gel, vacuumizing and drying in a vacuum oven at 60 ℃, and crushing.
In this embodiment, the mass ratio of the diamond to the pretreatment liquid in the treatment liquid a is 1: 4.
before the metal wire is wired in the treatment fluid A, the metal wire is subjected to an acid washing step.
The pickling step comprises the following steps:
a) completely immersing the metal wire into a pickling tank, wherein the time control range is as follows: 3-5 minutes;
b) washing the metal wire in the step a) with clear water;
c) adding an acid washing solution into an acid washing tank, completely immersing the metal wire in the step b) into the acid washing solution, and controlling the time within the range: 3-5 minutes;
d) and (3) washing the surface of the metal wire by using water, and washing the residual pickling solution on the surface of the metal wire.
The preparation raw materials of the pickling solution comprise the following components in percentage by mass: h2SO415 wt%, thiourea 0.1 wt%, zinc L-aspartate 1 wt% and the balance water.
In the step (2), the step (c),
the plating test was carried out under ultrasonic waves.
In one embodiment of the present invention, the plating solution comprises the following components in parts by weight: 50 parts by weight of water, 1.5 parts by weight of boric acid solution, 15 parts by weight of anhydrous nickel dichloride and 12 parts by weight of sodium picryl sulfonate.
The concentration of the boric acid solution is 35 g/L.
The test parameters of the electroplating are as follows: the pH value of the electroplating solution is 3.5, and the current density is 2.5A/dm2The temperature of the plating solution is 42 ℃, the plating time is 0.5h, and the frequency of the ultrasonic wave is 25 KHZ.
Electroplating the pretreated metal wire to obtain a crude product of the diamond cutting wire.
Said step (3)
The ionic liquid is 1-carboxymethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt.
After wiring in the ionic liquid, washing the surface of the diamond wire by using water, and flushing the residual ionic liquid on the surface of the diamond wire.
The diamond wire is prepared by adopting the preparation process of the diamond cutting wire. The metal wire is a stainless steel wire with a diameter of 0.14 mm.
Example 2: in this example, the difference from example 1 is that the diamond is a diamond powder generally purchased in the market, specifically, from zhhai national red abrasive grinding apparatus limited.
Example 3: in the present embodiment, the difference from embodiment 1 is that the diamond is prepared by a microwave plasma chemical vapor deposition method, and the specific preparation parameters are as follows:
the substrate temperature is 650 ℃, the microwave power is 3500W, the deposition pressure is 2.3kPa, the deposition time is 4.5h, and the CH is4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm.
A p-type Si (100) single crystal wafer is used as a substrate.
Example 4: in this example, the difference from example 1 is that the preparation raw material of the pretreatment liquid does not contain zinc polyacrylate.
Example 5: in this example, the difference from example 1 is that the raw material for preparing the plating solution does not contain sodium picryl sulfonate.
Example 6: in this example, the difference from example 1 is that sodium picryl sulfonate is replaced with sodium 1,3, 6-naphthalenetrisulfonate.
Example 7: in this embodiment, the difference from embodiment 1 is that the preparation method of the preparation process is as follows:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) and (3) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting wire.
And does not pass through the ionic liquid.
Example 8: in this example, the difference from example 1 is that the starting material for the acid wash does not contain zinc L-aspartate.
Example 9: in this embodiment, the difference from embodiment 1 is that the preparation method of the preparation process is as follows:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) wiring the pretreated metal wire obtained in the step (1) in ionic liquid to obtain a crude product of the diamond cutting wire;
(3) and (3) electroplating the crude product of the diamond cutting line in the step (2) to obtain the diamond cutting line.
Example 10: in this example, the difference from example 1 is that the pretreatment liquid does not contain octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride.
And (3) testing:
1. the invention uses a Nippon imported Anmingguan steel wire slicer TW320-C to carry out a cutting test, the material uses a single crystal silicon rod, the length, the width and the height are as follows: 150mm 25mm, the main cutting process conditions were as follows: the cutting linear speed is 500-600m/min, the cutting feed is 0.50-1.50mm/min, the tension of the wire saw is 25-40N, the cutting time is the end of the cutting of the silicon wafer, and the aqueous cutting fluid of Tianjin Tylen company is cooled.
TABLE 1 Diamond wire-electrode cutting Performance index
The foregoing examples are illustrative only, and serve to explain some of the features of the present disclosure. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. And that advances in science and technology will result in possible equivalents or sub-substitutes not currently contemplated for reasons of inaccuracy in language representation, and such changes should also be construed where possible to be covered by the appended claims.
Claims (5)
1. The preparation process of the diamond cutting wire is characterized by comprising the following steps of:
(1) preparing a diamond, mixing the diamond and the pretreatment liquid to obtain a treatment liquid A, and routing a metal wire in the treatment liquid A to obtain a pretreated metal wire;
(2) electroplating the pretreated metal wire in the step (1) to obtain a crude product of the diamond cutting line;
(3) wiring the crude product of the diamond cutting line obtained in the step (2) in ionic liquid to prepare the diamond cutting line;
before the metal wire is wired in the treatment fluid A, the metal wire is subjected to an acid pickling step; the preparation raw materials of the pickling solution in the pickling step comprise the following components in percentage by weight: h2SO415 wt%, thiourea 0.1 wt%, zinc L-aspartate 1 wt% and the balance water;
the diamond in the step (1) is prepared by adopting a microwave plasma chemical vapor deposition method, wherein the main parameters are as follows:
using p-type Si (100) single crystal wafer as substrate and CH4/H2The system is used as a gas source, wherein the temperature of the substrate is divided into two stages, the temperature of the substrate in the first stage is 650 ℃, and the temperature of the substrate in the second stage is 720 ℃;
when the temperature of the substrate is 650 ℃, the power of the microwave is 3500W, the deposition air pressure is 2.3kPa, and the deposition time is 4 h; when the temperature of the substrate is 720 ℃, the power of the microwave is 3000W, the deposition pressure is 3.4kPa, and the deposition time is 0.5 h; the CH4/H2The concentration of each gas in the system is respectively as follows: h2Is 200sccm, CH4Is 15 sccm;
the electroplating solution electroplated in the step (2) comprises water, a boric acid solution, anhydrous nickel dichloride and sodium picryl sulfonate;
the preparation raw materials of the pretreatment solution comprise:
80-100 parts of water, 5-10 parts of zinc polyacrylate, 0.1-3 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.1 part of stearyl trimethyl ammonium bromide;
the ionic liquid is 1-carboxymethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt.
2. The process for manufacturing a diamond-cutting wire according to claim 1, wherein the pretreatment liquid is prepared from a raw material comprising:
90-100 parts of water, 5-8 parts of zinc polyacrylate, 0.1-2 parts of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.01-0.05 part of stearyl trimethyl ammonium bromide.
3. The process for manufacturing a diamond-cutting wire according to claim 1, wherein the pretreatment liquid is prepared from a raw material comprising:
99 parts of water, 5 parts of zinc polyacrylate, 0.15 part of octadecyl-dimethyl- (3-trimethoxysilylpropyl) ammonium chloride and 0.02 part of stearyl trimethyl ammonium bromide.
4. The process for preparing a diamond cutting wire according to claim 1, wherein the zinc polyacrylate is prepared by the following method:
adding 1 weight part of zinc chloride solution into 2 weight parts of acrylic acid under stirring, adjusting the pH value of the reaction solution to 9 by ammonia water, adding 0.1 part of ammonium persulfate with 0.5g/ml and 0.1 part of sodium bisulfite solution with 0.5g/ml after stirring uniformly, placing in a water bath at 60 ℃ for reacting for 4 hours to obtain light yellow gel, vacuumizing and drying in a vacuum oven at 60 ℃, and crushing.
5. A diamond cutting wire produced by the process for producing a diamond cutting wire according to any one of claims 1 to 4.
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