Diamond wire and preparation method and application thereof

Abstract

The invention relates to a diamond wire and a preparation method and application thereof. The diamond wire sequentially comprises a diamond wire bus, an impact nickel layer, an upper sand nickel layer and a solid sand nickel layer from inside to outside. The impact nickel layer and / or the upper sand nickel layer comprise / comprises a dispersion reinforcing phase; the dispersion enhancing phase comprises dispersion enhancing phase micro powder with positive charges modified on the surface. According to the diamond wire, the dispersion strengthening phase is introduced into the impact nickel layer and / or the upper sand layer, so that the tensile strength of the electroplated layer can be enhanced, the deformation synergy between the electroplated layer and the bus is effectively improved, the quality of the diamond wire is improved, and the cutting rate is increased.

Description

Technical Field

[0001] The present application relates to the technical field of diamond wire production, and in particular to a diamond wire and a preparation method and application thereof. Background Art

[0002] At present, tungsten wire diamond wire saw follows the design of high carbon steel wire diamond wire saw, which is composed of mother bar, impact nickel layer, upper sand layer and solid sand layer. The impact nickel layer and upper sand layer make the diamond particles tightly bonded to the mother bar, which plays a key role in the quality of diamond wire saw.

[0003] The tensile strength of nickel and high carbon steel wire is similar, and they have good deformation synergy during use. At the same time, the electrolytic saturated nickel coating can improve the tensile strength of steel, increase the hardness and fatigue resistance of the material surface. However, the tensile strength of tungsten (110kg / mm 2 ) is nickel (40~50kg / mm 2 ), under the action of tensile stress, deformation first occurs on the side with low tensile strength, making the coating easy to peel off. The impact of this lack of deformation coordination on the quality of the wire saw is particularly prominent under high-speed cutting.

[0004] Therefore, the traditional technology still needs to be improved. Summary of the invention

[0005] Based on this, the present application provides a diamond wire and a preparation method and application thereof, which can effectively improve the deformation synergy between the nickel plating layer and the diamond wire busbar, enhance the tensile strength of the diamond wire, and thus enhance the cutting rate.

[0006] The specific technical solutions are as follows:

[0007] On the one hand, the present application provides a diamond wire, which includes, from the inside to the outside, a diamond wire busbar, an impact nickel layer, an upper sand nickel layer and a solid sand nickel layer; the impact nickel layer and / or the upper sand nickel layer include a dispersed reinforcement phase; the dispersed reinforcement phase includes dispersed reinforcement phase micropowder with a surface modified with positive charge.

[0008] The above-mentioned diamond wire of the present application includes a diamond wire busbar, an impact nickel layer, an upper sand nickel layer and a solid sand nickel layer. A dispersion strengthening phase is introduced into the impact nickel layer and / or the upper sand layer. The dispersion strengthening phase includes a dispersion strengthening phase micropowder with a surface modified with a positive charge. The surface of the dispersion strengthening phase micropowder is modified with a positive charge to prevent the micropowder particles from approaching and agglomerating with each other, so that it can be evenly dispersed in the preparation system of the diamond wire. In this way, the uniformity of the distribution of the dispersion strengthening phase micropowder in the nickel plating layer can be ensured, thereby improving the quality and performance stability of the diamond wire. In addition, the modification of positive charge can act as a bridge between the dispersed reinforced phase powder and the nickel-plated layer. On the one hand, it can combine with the surface of the dispersed reinforced phase powder, and on the other hand, it can undergo a certain physical or chemical adsorption with the surface of the nickel-plated layer, thereby enhancing the bonding force between the dispersed reinforced phase powder and the nickel-plated layer, improving the overall strength and service life of the diamond wire, and introducing the dispersed reinforced phase into the impact nickel layer and / or the upper sand layer can enhance the tensile strength of the electroplated layer, effectively improving the deformation synergy between the coating and the diamond wire mother bar, thereby improving the quality of the diamond wire and increasing the cutting rate.

[0009] In some embodiments, the dispersed reinforcement phase powder includes at least one of aluminum oxide, zirconium oxide, tungsten carbide, titanium carbide and silicon oxide;

[0010] And / or, the particle size of the dispersed reinforcement phase powder is 50nm~500nm;

[0011] And / or, the diamond wire busbar comprises a tungsten diamond wire busbar.

[0012] In some embodiments, the dispersed reinforcement phase is obtained by reacting dispersed reinforcement phase powder with a surface modifier.

[0013] Another aspect of the present application also provides a method for preparing a diamond wire, comprising the following steps:

[0014] Pre-treating the diamond wire busbar;

[0015] Performing a first electroplating on the pretreated diamond wire busbar to form an impact nickel layer on the surface of the diamond wire busbar to obtain a first diamond wire;

[0016] Performing a second electroplating on the first diamond wire to form a nickel layer on the surface of the first diamond wire to obtain a second diamond wire;

[0017] The second diamond wire is subjected to a third electroplating to form a solid nickel layer on the surface of the second diamond wire to obtain the diamond wire; the impact nickel layer and / or the upper nickel layer includes a dispersed reinforcement phase; the dispersed reinforcement phase includes dispersed reinforcement phase micropowder with a surface modified with positive charge.

[0018] In some embodiments, the first electroplating conditions are: the first electroplating solution includes nickel sulfamate and a solvent, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 0.5s~5s.

[0019] In some embodiments, the second electroplating conditions are: the second electroplating solution includes diamond, nickel sulfamate and solvent, the concentration of diamond is 0.5 g / L~2.0 g / L, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 30s~100s.

[0020] In some embodiments, the first electroplating solution and / or the second electroplating solution further comprises 2% to 30% by weight of the dispersed reinforcing phase powder, which is obtained by subjecting the dispersed reinforcing phase powder to a reaction treatment using a surface modifier.

[0021] In some embodiments, the surface modifier includes at least one of polyacrylic acid, polymethacrylic acid, polyethyleneimine, sodium stearate, sodium humate, sodium citrate, tetrabutylammonium hydroxide, mercapto polyethylene glycol monomethyl ether and a silane coupling agent.

[0022] In some embodiments, the conditions of the third electroplating are: the third electroplating solution includes nickel sulfamate and a solvent, the concentration of the nickel sulfamate is 30wt%~50wt%, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 30s~100s.

[0023] Another aspect of the present application further provides an application of the above-mentioned diamond wire or the diamond wire produced by the above-mentioned diamond wire production method in the production of a wire saw product for cutting. DETAILED DESCRIPTION

[0024] References to embodiments of the present application will now be provided in detail, one or more examples of which are described below. Each example is provided as an explanation rather than a limitation of the present application. In fact, it will be apparent to those skilled in the art that various modifications and variations may be made to the present application without departing from the scope or spirit of the present application. For example, a feature described or described as part of one embodiment may be used in another embodiment to produce a further embodiment.

[0025] Therefore, it is intended that the present application covers such modifications and variations that fall within the scope of the appended claims and their equivalents. Other objects, features and aspects of the present application are disclosed in or are apparent from the following detailed description. It will be appreciated by those of ordinary skill in the art that this discussion is merely a description of exemplary embodiments and is not intended to limit the broader aspects of the present application.

[0026] The term "comprises", "comprising" or any other variant thereof is intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements includes not only those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such process, method, article or equipment. In the absence of more restrictions, the elements defined by the sentence "comprising one..." do not exclude the presence of other identical elements in the process, method, article or equipment including the elements. The indefinite articles "a kind of" and "one" before the elements or components of the present application are not restrictive to the quantity requirements (i.e., the number of occurrences) of the elements or components. Therefore, "one" or "a kind of" should be interpreted as including one or at least one, and the elements or components in the singular form also include the plural form, unless the number obviously refers only to the singular form. The meaning of "multiple" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0027] The weight of the relevant components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also indicate the weight ratio between the components. Therefore, as long as the content of the relevant components is proportionally enlarged or reduced according to the description of the embodiments of the present invention, it is within the scope disclosed in the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiments of the present invention may be a mass unit known in the chemical industry such as μg, mg, g, kg, etc.

[0028] Except as shown in the operating examples or otherwise indicated, all numbers used in the specification and claims to indicate the amount of ingredients, physicochemical properties, etc. are understood to be adjusted by the term "about" in all cases. For example, therefore, unless otherwise indicated, the numerical parameters listed in the above specification and the attached claims are approximate values, and those skilled in the art can use the teachings disclosed herein to seek to obtain the desired properties and appropriately change these approximate values. The use of numerical ranges expressed as endpoints includes all numbers within the range and any range within the range, for example, 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4 and 5, etc.

[0029] An embodiment of the present application provides a diamond wire, which includes, from the inside to the outside, a diamond wire busbar, an impact nickel layer, an upper sand nickel layer and a solid sand nickel layer; the impact nickel layer and / or the upper sand nickel layer include a dispersed reinforcement phase; the dispersed reinforcement phase includes dispersed reinforcement phase micropowder with a surface modified with positive charge.

[0030] In some embodiments, the above-mentioned dispersion reinforcement phase powder includes at least one of aluminum oxide, zirconium oxide, tungsten carbide, titanium carbide and silicon oxide.

[0031] In some of the embodiments, the particle size of the dispersed reinforcement phase powder is 50nm~500nm.

[0032] In some embodiments, the diamond wire busbar comprises a tungsten diamond wire busbar.

[0033] In some of the embodiments, the diameter of the diamond wire busbar is 22 μm to 45 μm, but is not limited to the above diameter range.

[0034] In some embodiments, the diameter of the diamond wire is 30 μm to 55 μm, but is not limited to the above diameter range.

[0035] In some embodiments, the above-mentioned dispersed reinforcing phase is obtained by reacting dispersed reinforcing phase powder with a surface modifier.

[0036] The above-mentioned diamond wire of the present application includes a diamond wire busbar, an impact nickel layer, an upper sand nickel layer and a solid sand nickel layer. A dispersion strengthening phase is introduced into the impact nickel layer and / or the upper sand layer. The dispersion strengthening phase includes a dispersion strengthening phase micropowder with a surface modified with a positive charge. The surface of the dispersion strengthening phase micropowder is modified with a positive charge to prevent the micropowder particles from approaching and agglomerating with each other, so that it can be evenly dispersed in the preparation system of the diamond wire. In this way, the uniformity of the distribution of the dispersion strengthening phase micropowder in the nickel plating layer can be ensured, thereby improving the quality and performance stability of the diamond wire. In addition, the modification of positive charge can act as a bridge between the dispersed reinforced phase powder and the nickel-plated layer. On the one hand, it can combine with the surface of the dispersed reinforced phase powder, and on the other hand, it can undergo a certain physical or chemical adsorption with the surface of the nickel-plated layer, thereby enhancing the bonding force between the dispersed reinforced phase powder and the nickel-plated layer, improving the overall strength and service life of the diamond wire, and introducing the dispersed reinforced phase into the impact nickel layer and / or the upper sand layer can enhance the tensile strength of the electroplated layer, effectively improving the deformation synergy between the coating and the diamond wire mother bar, thereby improving the quality of the diamond wire and increasing the cutting rate.

[0037] An embodiment of the present application further provides a method for preparing a diamond wire, the method comprising steps S10 to S40.

[0038] Step S10: pre-processing the diamond wire busbar.

[0039] In some embodiments, the pretreatment method includes degreasing and pickling the diamond wire busbar in sequence.

[0040] Step S20: performing a first electroplating on the pretreated diamond wire busbar to form an impact nickel layer on the surface of the pretreated diamond wire busbar to obtain a first diamond wire.

[0041] In some embodiments, the first electroplating conditions are: the first electroplating solution includes nickel sulfamate and a solvent, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 0.5s~5s.

[0042] The above current density is 0.05A / cm 2 ~0.5A / cm 2 In the range, the values ​​include the minimum and maximum values ​​of the range, and each value between the minimum and maximum values, and specific examples include but are not limited to the point values ​​in the embodiment and the following point values: 0.05 A / cm 2 , 0.06 A / cm 2 , 0.07 A / cm 2 , 0.08 A / cm 2 , 0.09 A / cm 2 , 0.1 A / cm 2 , 0.15 A / cm 2 , 0.2 A / cm 2 , 0.25 A / cm 2 , 0.3 A / cm 2 , 0.35 A / cm 2 , 0.4 A / cm 2 , 0.45 A / cm 2 , 0.5 A / cm 2 ; or a range consisting of any two of these values, including, for example: 0.05 A / cm 2 ~0.3 A / cm 2 .

[0043] In some embodiments, the current density is 0.1 A / cm 2 ~0.25A / cm 2 .

[0044] It can be understood that the coating generation speed within the above current density range can better control the uniformity, density and surface smoothness of the coating.

[0045] Step S30: performing a second electroplating on the first diamond wire to form a nickel layer on the surface of the first diamond wire to obtain a second diamond wire.

[0046] In some embodiments, the second electroplating conditions are as follows: the second electroplating solution includes diamond, nickel sulfamate and a solvent, the mass concentration of the diamond is 0.5 g / L to 2.0 g / L, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 30s~100s.

[0047] The mass concentration of diamond is 0.5 g / L~2.0 g / L, and the values ​​include the minimum and maximum values ​​of the range, and every value between the minimum and maximum values. Specific examples include but are not limited to the point values ​​in the embodiments and the following point values: 0.5 g / L, 0.6 g / L, 0.7 g / L, 0.8 g / L, 0.9 g / L, 1 g / L, 1.1 g / L, 1.2 g / L, 1.3 g / L, 1.4 g / L, 1.5 g / L, 1.6 g / L, 1.7 g / L, 1.8 g / L, 1.9 g / L or 2 g / L; or a range composed of any two of these values, as an example, including: 0.5 g / L ~1 g / L.

[0048] In some of the embodiments, the mass concentration of the diamond is 0.9 g / L-1.6 g / L.

[0049] It can be understood that by controlling the mass concentration of the diamond within the above-mentioned specific range, an electroplating layer with better bonding performance and more appropriate thickness can be obtained.

[0050] The above current density is 0.05 A / cm 2 ~0.5A / cm 2 In the range, the values ​​include the minimum and maximum values ​​of the range, and each value between the minimum and maximum values, and specific examples include but are not limited to the point values ​​in the embodiment and the following point values: 0.05 A / cm 2 , 0.06 A / cm 2 , 0.07 A / cm 2 , 0.08 A / cm 2 , 0.09 A / cm 2 , 0.1 A / cm 2 , 0.15 A / cm 2 , 0.2 A / cm 2 , 0.25 A / cm 2 , 0.3 A / cm 2 , 0.35 A / cm 2 , 0.4 A / cm2 , 0.45 A / cm 2 or 0.5 A / cm 2 ; or a range consisting of any two of these values, including, for example: 0.1 A / cm 2 ~0.3A / cm 2 .

[0051] In some embodiments, the current density is 0.1 A / cm 2 ~0.25A / cm 2 .

[0052] The above time is 30s~100s, and the values ​​include the minimum and maximum values ​​of the range, and every value between the minimum and maximum values. Specific examples include but are not limited to the point values ​​in the embodiments and the following point values: 30s, 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s, 90s, 95s or 100s; or a range composed of any two of these values, as an example, including: 30s~80s.

[0053] In some embodiments, the above time is 50s~80s.

[0054] In some embodiments, the first electroplating solution and / or the second electroplating solution further comprises 2% to 30% by weight of the dispersed reinforcing phase powder, which is obtained by subjecting the dispersed reinforcing phase powder to a reaction treatment using a surface modifier.

[0055] The mass proportion of the above-mentioned dispersed reinforcement phase powder is 2%~30%, and the values ​​include the minimum and maximum values ​​of the range, as well as each value between the minimum and maximum values. Specific examples include but are not limited to the point values ​​in the embodiments and the following point values: 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30%; or a range composed of any two of these values, as an example, including: 5%~30%.

[0056] In some embodiments, the mass proportion of the dispersed reinforcing phase powder is 5% to 20%.

[0057] Further controlling the mass proportion of the dispersed reinforcing phase powder within the above-mentioned ratio range can allow it to be more evenly dispersed in the preparation system of the diamond wire, thus ensuring the uniformity of the distribution of the dispersed reinforcing phase powder in the nickel plating layer, thereby improving the quality and performance stability of the diamond wire.

[0058] Step S40: performing a third electroplating on the second diamond wire to form a solid nickel layer on the surface of the second diamond wire to prepare the diamond wire; the impact nickel layer and / or the upper nickel layer include a dispersed reinforcement phase; the dispersed reinforcement phase includes dispersed reinforcement phase powder with a surface modified with positive charge.

[0059] Specifically, the preparation of the above-mentioned dispersed reinforcing phase includes the following steps: subjecting dispersed reinforcing phase powder to a reaction treatment using a surface modifier to obtain the dispersed reinforcing phase powder.

[0060] In some embodiments, the surface modifier includes at least one of polyacrylic acid (PAA), polymethacrylic acid (PMAA), polyethyleneimine (PEI), sodium stearate, sodium humate, sodium citrate, tetrabutylammonium hydroxide, mercapto polyethylene glycol monomethyl ether and a silane coupling agent.

[0061] It can be understood that the use of the above-mentioned modifiers can change the surface charge properties of the dispersed reinforcement phase powder, thereby affecting its dispersibility in the preparation of diamond wire, its interaction with other components and other properties, making it easier to interact with the nickel plating layer, thereby improving the cutting and grinding performance of the diamond wire.

[0062] In some embodiments, the silane coupling agent includes at least one of KH550, KH570 and SCA1603.

[0063] In some embodiments, the conditions of the third electroplating are as follows: the third electroplating solution includes nickel sulfamate and a solvent, the concentration of the nickel sulfamate is 30wt%~50wt%, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 30s~100s.

[0064] The above current density is 0.05 A / cm 2 ~0.5A / cm 2 In the range, the values ​​include the minimum and maximum values ​​of the range, and each value between the minimum and maximum values, and specific examples include but are not limited to the point values ​​in the embodiment and the following point values: 0.05 A / cm 2 , 0.06 A / cm 2 , 0.07 A / cm 2 , 0.08 A / cm 2 , 0.09 A / cm 2 , 0.1 A / cm 2 , 0.15 A / cm 2 , 0.2 A / cm 2 , 0.25 A / cm 2 , 0.3 A / cm 2, 0.35 A / cm 2 , 0.4 A / cm 2 , 0.45 A / cm 2 or 0.5 A / cm 2 ; or a range consisting of any two of these values, including, for example: 0.05~0.3

[0065] In some embodiments, the current density is 0.1 A / cm 2 ~0.25A / cm 2 .

[0066] The above time is 30s~100s, and the values ​​include the minimum and maximum values ​​of the range, and every value between the minimum and maximum values. Specific examples include but are not limited to the point values ​​in the embodiments and the following point values: 30s, 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s, 90s, 95s or 100s; or a range composed of any two of these values, as an example, including: 30s~80s.

[0067] In some embodiments, the above time is 50s~80s.

[0068] The preparation method is simple to operate and relatively low in cost, and is conducive to the large-scale production of high-quality diamond wires.

[0069] One embodiment of the present application also provides an application of the diamond wire and the diamond wire produced by the diamond wire production method in the production of a wire saw product for cutting.

[0070] In some of the embodiments, the diamond wire is used to cut silicon rods / silicon carbide ingots in the upstream of the photovoltaic industry chain.

[0071] The application of the above-mentioned diamond wire can effectively improve the deformation coordination between the nickel plating layer and the diamond wire mother bar, enhance the tensile strength of the diamond wire, and thus enhance the cutting rate.

[0072] The following is a detailed description in conjunction with specific examples. The following examples do not include other components except for inevitable impurities unless otherwise specified. The reagents and instruments used in the examples are conventionally selected in the art unless otherwise specified. The experimental methods for which specific conditions are not specified in the examples are implemented according to conventional conditions, such as the conditions described in the literature, books, or methods recommended by the manufacturer.

[0073] Example 1

[0074] (1) Provide tungsten wire busbar (35 wire diameter tungsten wire busbar produced by China Tungsten High-Tech). The wire diameter of the tungsten wire busbar is 35μm. After electrolytic degreasing, pickling, water washing and drying, the pre-treated diamond wire busbar is obtained.

[0075] (2) The pretreated diamond wire busbar is subjected to the first electroplating, and the first electroplating is carried out in the first electroplating solution, which includes nickel sulfamate (purchased from Yinglang Chemical, with a purity of 98%), a mixed salt solution of nickel chloride and boric acid, and a dispersed reinforcing phase powder. The total mass of nickel sulfamate and solvent (mixed salt solution of nickel chloride and boric acid) is used as the basis, and the concentration of nickel sulfamate is 40wt%. 5wt% of tungsten carbide powder (purchased from Deke Island Gold, with a particle size of 150nm) is added to the nickel sulfamate solution. The particle size of the tungsten carbide powder is 150nm, and the surface is modified with tetrabutylammonium hydroxide (purchased from Kent Catalytic Materials Co., Ltd., with a purity of 99%). After stirring and standing, the tungsten carbide powder forms a uniform suspension in the first electroplating solution due to the charge, and the current used is 0.1A / cm 2 , time 1.2s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0076] (3) The first diamond wire is subjected to a second electroplating, wherein the second electroplating is performed in a second electroplating solution, wherein the second electroplating solution comprises nickel sulfamate, a solvent and diamond powder, wherein the concentration of the nickel sulfamate is 40 wt %, diamond powder is added to the nickel sulfamate solution, and the mass concentration of the diamond powder is 1.5 g / L, and the process current is 0.1 A / cm 2 , time 50s, a sand nickel layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0077] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 40 wt %. The process current is 0.1 A / cm 2 , time 50s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0078] Example 2

[0079] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 35 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0080] (2) The pretreated diamond wire busbar is subjected to the first electroplating. The first electroplating is carried out in a first electroplating solution. The first electroplating solution includes nickel sulfamate, a solvent and a dispersed reinforcing phase powder. The total mass of nickel sulfamate and the solvent (a mixed salt solution of nickel chloride and boric acid) is used as a reference. The concentration of nickel sulfamate is 40wt%. 2.0wt% alumina powder (purchased from Maoguo Nano, 500nm medium-sized alumina powder) is added to the nickel sulfamate solution. The particle size of the alumina powder is 500nm, and the surface is modified with polyacrylic acid (purchased from ALFA, purity 50%). After stirring and standing, the alumina powder forms a uniform suspension in the first electroplating solution due to the charge. The current used is 0.1A / cm 2 , time 1.2s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0081] (3) The first diamond wire is subjected to a second electroplating, wherein the second electroplating is performed in a second electroplating solution, wherein the second electroplating solution comprises nickel sulfamate, a solvent, aluminum oxide powder and diamond powder, wherein the concentration of the nickel sulfamate is 40 wt %. Diamond powder and aluminum oxide powder are added to the nickel sulfamate solution, wherein the mass concentration of the diamond powder is 1.5 g / L, the amount of aluminum oxide added is 2.0 wt %, and the process current is 0.5 A / cm 2 , time 30s, a sand nickel layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0082] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 40 wt %. The process current is 0.5 A / cm 2 , time 30s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0083] Example 3

[0084] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 35 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0085] (2) The pretreated diamond wire busbar is subjected to the first electroplating, and the first electroplating is carried out in a first electroplating solution, which includes nickel sulfamate, a solvent and a dispersed reinforcing phase powder. The total mass of nickel sulfamate and the solvent (a mixed salt solution of nickel chloride and boric acid) is used as a reference, and the concentration of nickel sulfamate is 40wt%. 30wt% of titanium carbide powder (purchased from Zhongke Yannuo, with a purity of 99.9% and a medium particle size of 50nm) is added to the nickel sulfamate solution. The particle size of the titanium carbide powder is 50nm, and the surface is modified with polyethyleneimine (purchased from Hunan Bangyun Biology, with a purity of >95%). After stirring and standing, the titanium carbide powder forms a uniform suspension in the first electroplating solution due to the action of the charge, and the current used is 0.5A / cm 2 , time 0.5s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0086] (3) The first diamond wire is subjected to a second electroplating, wherein the second electroplating is performed in a second electroplating solution, wherein the second electroplating solution comprises nickel sulfamate, a solvent, titanium carbide powder and diamond powder, wherein the concentration of nickel sulfamate is 40 wt %. Diamond powder and titanium carbide powder are added to the nickel sulfamate solution, wherein the mass concentration of diamond powder is 1.5 g / L, and the amount of titanium carbide powder added is 30 wt %. The process current used is 0.05 A / cm 2 , time 100s, a nickel sand layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0087] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 40 wt %. The process current is 0.05 A / cm 2 , time 100s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0088] Example 4

[0089] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 35 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0090] (2) The pretreated diamond wire busbar is subjected to the first electroplating, and the first electroplating is carried out in a first electroplating solution, which includes nickel sulfamate, a solvent and a dispersed reinforcing phase powder. The total mass of the nickel sulfamate and the solvent (a mixed salt solution of nickel chloride and boric acid) is used as a reference, and the concentration of the nickel sulfamate is 34wt%. 4.6wt% zirconium oxide powder (purchased from Zhongke Yannuo, with a particle size of 75nm) is added to the nickel sulfamate solution, and the particle size of the zirconium oxide powder is 75nm; after stirring and standing for 3s, the zirconium oxide powder forms a uniform suspension in the first electroplating solution due to the charge, and the current used is 0.1A / cm2 , time 1.6s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0091] (3) The first diamond wire is subjected to a second electroplating, wherein the second electroplating is performed in a second electroplating solution, wherein the second electroplating solution comprises nickel sulfamate, a solvent, zirconium oxide micropowder and diamond micropowder, wherein the concentration of the nickel sulfamate is 34 wt %. Diamond micropowder and zirconium oxide micropowder are added to the nickel sulfamate solution, wherein the mass concentration of the diamond micropowder is 1.5 g / L, and the amount of zirconium oxide micropowder added is 4.6 wt %. The process current used is 0.1 A / cm 2 , time 70s, a nickel sand layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0092] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 34 wt %. The process current is 0.1 A / cm 2 , time 70s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0093] Example 5

[0094] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 22 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0095] (2) The pretreated diamond wire busbar is subjected to a first electroplating, and the first electroplating is carried out in a first electroplating solution. The first electroplating solution includes nickel sulfamate, a solvent and a dispersed reinforcing phase powder. The total mass of the nickel sulfamate and the solvent (a mixed salt solution of nickel chloride and boric acid) is used as a reference, and the concentration of the nickel sulfamate is 34wt%. 4.6wt% zirconium oxide powder (purchased from Zhongke Yannuo, with a particle size of 75nm) is added to the nickel sulfamate solution, and the particle size of the zirconium oxide powder is 75nm. After stirring and standing for 3s, the zirconium oxide powder forms a uniform suspension in the first electroplating solution due to the charge. A current of 0.1A / cm2 and a time of 1.6s are used to form an impact nickel layer on the surface of the pretreated diamond wire busbar to obtain the first diamond wire.

[0096] (3) The first diamond wire is subjected to a second electroplating, wherein the second electroplating is performed in a second electroplating solution, wherein the second electroplating solution comprises nickel sulfamate, a solvent, zirconium oxide micropowder and diamond micropowder, wherein the concentration of the nickel sulfamate is 34 wt %. Diamond micropowder and zirconium oxide micropowder are added to the nickel sulfamate solution, wherein the mass concentration of the diamond micropowder is 1.5 g / L, and the amount of zirconium oxide micropowder added is 4.6 wt %. The process current used is 0.1 A / cm 2, time 70s, a nickel sand layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0097] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 34 wt %. The process current is 0.1 A / cm 2 , time 70s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0098] Example 6

[0099] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 45 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0100] (2) The pretreated diamond wire busbar is subjected to the first electroplating, and the first electroplating is carried out in a first electroplating solution, which includes nickel sulfamate, a solvent and a dispersed reinforcing phase powder. The total mass of nickel sulfamate and the solvent (a mixed salt solution of nickel chloride and boric acid) is used as a reference, and the concentration of nickel sulfamate is 40wt%. 30wt% of titanium carbide powder (purchased from Zhongke Yannuo, with a purity of 99.9% and a medium particle size of 50nm) is added to the nickel sulfamate solution. The particle size of the titanium carbide powder is 50nm, and the surface is modified with polyethyleneimine (purchased from Hunan Bangyun Biology, with a purity of >95%). After stirring and standing, the titanium carbide powder forms a uniform suspension in the first electroplating solution due to the action of the charge, and the current used is 0.5A / cm 2 , time 0.5s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0101] (3) The first diamond wire is subjected to a second electroplating, wherein the second electroplating is performed in a second electroplating solution, wherein the second electroplating solution comprises nickel sulfamate, a solvent, titanium carbide powder and diamond powder, wherein the concentration of nickel sulfamate is 40 wt %. Diamond powder and titanium carbide powder are added to the nickel sulfamate solution, wherein the mass concentration of diamond powder is 1.5 g / L, and the amount of titanium carbide powder added is 30 wt %. The process current used is 0.05 A / cm 2 , time 100s, a nickel sand layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0102] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 40 wt %. The process current is 0.05 A / cm 2 , time 100s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0103] Comparative Example 1

[0104] The preparation methods of the diamond wires in Comparative Example 1 and Example 1 are basically the same, the only difference being that there is no dispersion strengthening process.

[0105] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 35 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0106] (2) The pretreated diamond wire busbar is subjected to a first electroplating, wherein the first electroplating is performed in a first electroplating solution, wherein the first electroplating solution comprises nickel sulfamate and a solvent, and the total mass of the nickel sulfamate and the solvent (a mixed salt solution of nickel chloride and boric acid) is taken as a reference, the concentration of the nickel sulfamate is 40wt%, and the current used is 0.1A / cm 2 , time 1.2s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0107] (3) performing a second electroplating on the first diamond wire, the second electroplating being performed in a second electroplating solution, the second electroplating solution comprising nickel sulfamate and a solvent, the concentration of the nickel sulfamate being 40 wt %, and the process current being 0.1 A / cm 2 , time 50s, a sand nickel layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0108] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 40 wt %. The process current is 0.1 A / cm 2 , time 50s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0109] Comparative Example 2

[0110] The preparation method of the diamond wire in Comparative Example 1 is basically the same as that in Comparative Example 1, and the only difference is that the wire diameter of the tungsten wire busbar is different.

[0111] (1) A tungsten wire busbar is provided, the wire diameter of the tungsten wire busbar is 22 μm, and after electrolytic degreasing, pickling, water washing, and drying, a pre-treated diamond wire busbar is obtained.

[0112] (2) The pretreated diamond wire busbar is subjected to a first electroplating, wherein the first electroplating is performed in a first electroplating solution, wherein the first electroplating solution comprises nickel sulfamate and a solvent (a mixed salt solution of nickel chloride and boric acid), and the concentration of nickel sulfamate is 34 wt % based on the total mass of the nickel sulfamate and the solvent, and the current used is 0.1 A / cm 2 , time 1.6s, an impact nickel layer is formed on the surface of the pretreated diamond wire mother bar to obtain the first diamond wire.

[0113] (3) performing a second electroplating on the first diamond wire, the second electroplating being performed in a second electroplating solution, the second electroplating solution comprising nickel sulfamate and a solvent, the concentration of the nickel sulfamate being 34 wt %, and the process current being 0.1 A / cm 2 , time 70s, a nickel sand layer is formed on the surface of the first diamond wire to obtain a second diamond wire.

[0114] (4) The second diamond wire is subjected to a third electroplating process. The third electroplating process is carried out in a third electroplating solution. The third electroplating solution is a nickel sulfamate solution. The concentration of the nickel sulfamate solution is 34 wt %. The process current is 0.1 A / cm 2 , time 70s, a solid sand nickel layer is formed on the surface of the second diamond wire to prepare a diamond wire.

[0115] test

[0116] 1. Tensile strength test

[0117] The diamond wires prepared in each embodiment and comparative example are subject to the requirements of GB / T 228.1-2021 standard.

[0118] 2. Maximum wire speed detection

[0119] Taking the cutting of a 6-inch silicon carbide single crystal rod as an example, this is the maximum cutting speed at which the diamond wire does not break in the conventional cutting process.

[0120] The test results are shown in Table 1.

[0121] Table 1

[0122]

[0123] In summary, the diamond wire produced by adopting the technical solution of the present application effectively improves the deformation coordination between the coating and the diamond wire mother bar, improves the tensile strength of the diamond wire, and further improves the cutting rate.

[0124] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0125] The above-described embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be construed as limiting the scope of the patent application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent application shall be subject to the attached claims.

Claims

1. A diamond wire, characterized in that: From the inside to the outside, it includes a diamond wire busbar, an impact nickel layer, an upper sand nickel layer and a solid sand nickel layer in sequence; the impact nickel layer and / or the upper sand nickel layer includes a dispersed reinforcement phase; the dispersed reinforcement phase includes dispersed reinforcement phase micropowder with a surface modified with positive charge.

2. The diamond wire according to claim 1, characterized in that The dispersed reinforcement phase powder includes at least one of aluminum oxide, zirconium oxide, tungsten carbide, titanium carbide and silicon oxide; And / or, the particle size of the dispersed reinforcement phase powder is 50nm~500nm; And / or, the diamond wire busbar comprises a tungsten diamond wire busbar.

3. The diamond wire according to any one of claims 1 to 2, characterized in that The dispersed reinforcing phase is obtained by reacting dispersed reinforcing phase micropowder with a surface modifier.

4. A method for preparing a diamond wire, characterized in that: The following steps are involved: Pre-treating the diamond wire busbar; Performing a first electroplating on the pretreated diamond wire busbar to form an impact nickel layer on the surface of the diamond wire busbar to obtain a first diamond wire; Performing a second electroplating on the first diamond wire to form a nickel layer on the surface of the first diamond wire to obtain a second diamond wire; The second diamond wire is subjected to a third electroplating to form a solid nickel layer on the surface of the second diamond wire to obtain the diamond wire; the impact nickel layer and / or the upper nickel layer includes a dispersed reinforcement phase; the dispersed reinforcement phase includes dispersed reinforcement phase micropowder with a surface modified with positive charge.

5. The method for preparing a diamond wire according to claim 4, characterized in that: The conditions of the first electroplating are: the first electroplating solution includes nickel sulfamate and a solvent, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 0.5s~5s.

6. The method for preparing a diamond wire according to claim 5, characterized in that: The conditions of the second electroplating are as follows: the second electroplating solution includes diamond, nickel sulfamate and solvent, the concentration of diamond is 0.5 g / L-2.0 g / L, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 30s~100s.

7. The method for preparing a diamond wire according to claim 6, characterized in that: The first electroplating solution and / or the second electroplating solution further include the dispersed reinforcing phase powder in an amount of 2% to 30% by mass, and the dispersed reinforcing phase powder is obtained by subjecting the dispersed reinforcing phase powder to a reaction treatment using a surface modifier.

8. The method for preparing a diamond wire according to claim 7, characterized in that: The surface modifier includes at least one of polyacrylic acid, polymethacrylic acid, polyethylene imine, sodium stearate, sodium humate, sodium citrate, tetrabutylammonium hydroxide, mercapto polyethylene glycol monomethyl ether and a silane coupling agent.

9. The method for preparing a diamond wire according to any one of claims 4 to 8, characterized in that: The conditions of the third electroplating are as follows: the third electroplating solution includes nickel sulfamate and a solvent, the concentration of the nickel sulfamate is 30wt% to 50wt%, and the current density is 0.05 A / cm 2 ~0.5A / cm 2 , the time is 30s~100s.

10. Use of the diamond wire according to any one of claims 1 to 3 or the diamond wire prepared by the method for preparing the diamond wire according to any one of claims 4 to 9 in the preparation of a cutting wire saw product.

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