CN110295361B - Preparation method of multi-edge diamond abrasive particles - Google Patents
Preparation method of multi-edge diamond abrasive particles Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 154
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 154
- 239000002245 particle Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 76
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000007747 plating Methods 0.000 claims abstract description 35
- 239000011259 mixed solution Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 21
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 14
- 239000001119 stannous chloride Substances 0.000 claims abstract description 14
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 14
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 9
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 9
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000006061 abrasive grain Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 5
- 229940093930 potassium iodate Drugs 0.000 claims description 5
- 235000006666 potassium iodate Nutrition 0.000 claims description 5
- 239000001230 potassium iodate Substances 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000000227 grinding Methods 0.000 abstract description 9
- 238000005520 cutting process Methods 0.000 abstract description 5
- 239000007767 bonding agent Substances 0.000 abstract description 3
- 206010070834 Sensitisation Diseases 0.000 abstract 1
- 230000008313 sensitization Effects 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 23
- 229910052759 nickel Inorganic materials 0.000 description 11
- 239000013078 crystal Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000005498 polishing Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1664—Process features with additional means during the plating process
- C23C18/1669—Agitation, e.g. air introduction
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polishing Bodies And Polishing Tools (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a preparation method of multi-edge diamond abrasive particles, which comprises the following steps: putting the diamond micro powder into a mixed solution of stannous chloride and hydrochloric acid for surface sensitization; then placing the diamond micro powder into a mixed solution of palladium chloride and hydrochloric acid to activate the diamond micro powder; placing the diamond micro powder in a plating solution for plating to obtain diamond micro powder with a plated surface; the multi-edge diamond abrasive particles prepared by the method have rough surfaces and large specific surface areas, can greatly enhance holding force by being embedded in a bonding agent, and improve the service life and grinding and cutting efficiency of diamond products.
Description
Technical Field
The invention relates to the technical field of diamond surface treatment and processing, in particular to a preparation method of multi-edge diamond abrasive particles.
Background
The diamond micro powder has high hardness and good wear resistance, and can be widely used for cutting, grinding, drilling, polishing and the like. Is an ideal raw material for grinding and polishing high-hardness materials such as hard alloy, ceramics, gems, optical glass and the like. The diamond micro powder product is a tool and a component which are manufactured by processing the diamond micro powder. When the traditional diamond micro powder is directly used as an abrasive, the grinding force is limited due to the fact that the surface edge angle is small. The surface of the product is provided with a large number of cutting edges, so that more grinding force can be generated, and the grinding and polishing efficiency is greatly improved. When the diamond micro powder is used as a raw material to prepare a diamond product, various binding forces are difficult to form chemical bonds with diamond, and the traditional diamond micro powder has poor holding force due to smooth surface, so that the diamond falls off before being completely utilized.
Other diamond surface roughening technologies focus on forming a diamond foamed structure, so that the self-sharpening performance of the diamond is improved, and meanwhile, a workpiece is not scratched in the grinding process. Although the performance of the diamond is improved by the process, the high-energy crystal faces of the diamond are damaged by isotropic corrosion, so that the strength of the diamond is greatly reduced, and the strength and the service life of the diamond are reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of the multi-edge diamond abrasive particles.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing multi-edge diamond abrasive particles comprises the following steps:
placing diamond micro powder in a mixed solution of stannous chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain surface-sensitized diamond micro powder;
step two, washing the diamond micro powder treated in the step one for 2-3 times by using pure water, then placing the diamond micro powder into a mixed solution of palladium chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain activated diamond micro powder;
step three, washing the diamond micro powder treated in the step two for 6-10 times by using pure water, then placing the diamond micro powder into a plating solution at the temperature of 75-85 ℃ for stirring at the stirring speed of 80-150 r/min until the plating reaction is finished, and obtaining diamond micro powder with the plated surface;
step four, cleaning the diamond micro powder treated in the step three by using pure water, drying, then rapidly treating at a high temperature of 900-1000 ℃, sintering for 5-10 min, and taking out and rapidly cooling;
step five, carrying out high-temperature treatment on the diamond micro powder treated in the step four, carrying out heat preservation treatment for 4-9 hours at the temperature of 500-650 ℃, and cooling to room temperature for later use;
and sixthly, removing impurities from the diamond micro powder treated in the fifth step by sequentially adopting hydrochloric acid and perchloric acid, wherein the treatment temperature of the hydrochloric acid is 45-65 ℃, the treatment temperature of the perchloric acid is 220-280 ℃, then cleaning for 4-7 times by using pure water, and drying to obtain the multi-edge diamond abrasive particles.
Further, in the step one, the median particle size of the diamond micropowder is D50 in microns, m is the weight of the diamond micropowder in grams, and the ratio of the volume of the mixed solution to the total surface area factor of the diamond micropowder particles is as follows: 8-12 ml: (m × D50/8).
Further, in the first step, the mass volume ratio of the stannous chloride to the mixed solution is 10-15 g/L, and the volume fraction of the hydrochloric acid is 5-15%.
Further, in the second step, the median particle size of the diamond micropowder is D50 in microns, m is the weight of diamond in grams, and the ratio of the volume of the mixed solution to the total surface area factor of the diamond micropowder particles is 5-10 ml: (m × D50/8).
Furthermore, in the second step, the mass volume ratio of the palladium chloride to the mixed solution is 0.2-0.5 g/L, and the volume fraction of the hydrochloric acid is 5-15%.
Further, the median particle size of the diamond micropowder in the third step is D50 in micrometer, m is the weight of diamond in gram, and the ratio of the volume of the plating solution to the total surface area factor of the diamond micropowder particles is 100-: (m × D50/8).
Further, the plating solution in the third step comprises 30-35 g/L of nickel sulfate, 40-45 g/L of sodium hypophosphite, 15-20 g/L of boric acid, 13-15 g/L of citric acid, 10-15 g/L of lactic acid, 1-2 mg/L of thiourea, 30-50 mg/L of potassium iodate and 0.2-0.3 g/L of sodium dodecyl benzene sulfonate.
Further, in the third plating reaction step, sodium hypophosphite with the mass volume ratio of 150-200 g/L and nickel sulfate with the mass volume ratio of 100-150 g/L are gradually added into the plating solution, and the weight of the diamond micro powder after plating is increased by 35-55%.
The beneficial effects of the invention are mainly shown in the following aspects: the method is adopted to coarsen the surface of the diamond, corrode the crystal face which is easy to corrode by anisotropic etching, and simultaneously reserve the crystal face with high mechanical strength and higher chemical bond energy; the multi-edge diamond abrasive particles prepared by the method have rough surfaces and large specific surface areas, the holding force can be greatly enhanced by embedding the multi-edge diamond abrasive particles into a bonding agent, the service life and the grinding and cutting efficiency of a diamond product are improved, the median particle size of diamond micro powder is reduced by 0.3-0.7 micrometer compared with the original diamond micro powder, the crystal form of the original diamond micro powder cannot be changed, and the specific surface area of the multi-edge diamond abrasive particles is increased to 1.5-3 times of that of the untreated diamond micro powder.
Drawings
FIG. 1 is a scanning electron microscope image of diamond micropowder without treatment;
fig. 2 is a scanning electron micrograph of a multi-edged diamond abrasive grain according to the present invention.
Detailed Description
The embodiments of the present invention are described in detail with reference to the accompanying drawings, and the embodiments and specific operations of the embodiments are provided on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following embodiments.
Example 1
A method for preparing multi-edge diamond abrasive particles comprises the following steps:
placing diamond micro powder in a mixed solution of stannous chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain surface-sensitized diamond micro powder;
step two, washing the diamond micro powder treated in the step one for 2-3 times by using pure water, then placing the diamond micro powder into a mixed solution of palladium chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain activated diamond micro powder;
step three, washing the diamond micro powder treated in the step two for 6-10 times by using pure water, then placing the diamond micro powder into a plating solution at the temperature of 75-85 ℃ for stirring at the stirring speed of 80-150 r/min until the plating reaction is finished, and obtaining diamond micro powder with the plated surface;
step four, cleaning the diamond micro powder treated in the step three by using pure water, drying, then rapidly treating at a high temperature of 900-1000 ℃, sintering for 5-10 min, and taking out and rapidly cooling;
step five, carrying out high-temperature treatment on the diamond micro powder treated in the step four, carrying out heat preservation treatment for 4-9 hours at the temperature of 500-650 ℃, and cooling to room temperature for later use;
and sixthly, removing impurities from the diamond micro powder treated in the fifth step by sequentially adopting hydrochloric acid and perchloric acid, wherein the treatment temperature of the hydrochloric acid is 45-65 ℃, the treatment temperature of the perchloric acid is 220-280 ℃, then cleaning for 4-7 times by using pure water, and drying to obtain the multi-edge diamond abrasive particles.
Further, the ratio of the volume of the mixed solution to the total surface area factor of the diamond micro powder particles in the step one is as follows: 8-12 ml: (m x D50/8), wherein the median particle size of the diamond micropowder is D50 in microns, and m is the weight of the diamond micropowder in grams.
Further, in the first step, the mass volume ratio of the stannous chloride to the mixed solution is 10-15 g/L, and the volume fraction of the hydrochloric acid in the mixed solution is 5-15%.
Further, the ratio of the volume of the mixed solution to the total surface area factor of the diamond micro powder particles in the second step is 5-10 ml: (m x D50/8), wherein the median particle size of the diamond micropowder is D50 in microns, and m is the diamond weight in grams.
Furthermore, in the second step, the mass volume ratio of the palladium chloride to the mixed solution is 0.2-0.5 g/L, and the volume fraction of the hydrochloric acid in the mixed solution is 5-15%.
Further, the ratio of the volume of the plating solution to the total surface area factor of the diamond micro powder particles in the third step is 100-200 ml: (m x D50/8), wherein the median particle size of the diamond micropowder is D50 in microns, and m is the diamond weight in grams.
Further, the plating solution in the third step comprises 30-35 g/L of nickel sulfate, 40-45 g/L of sodium hypophosphite, 15-20 g/L of boric acid, 13-15 g/L of citric acid, 10-15 g/L of lactic acid, 1-2 mg/L of thiourea, 30-50 mg/L of potassium iodate and 0.2-0.3 g/L of sodium dodecyl benzene sulfonate.
Further, in the third plating reaction step, sodium hypophosphite with the mass volume ratio of 150-200 g/L and nickel sulfate with the mass volume ratio of 100-150 g/L are gradually added into the plating solution, and the weight of the diamond micro powder after plating is increased by 35-55%.
Example 2
A method for preparing multi-edge diamond abrasive particles comprises the following steps:
placing diamond micro powder in a mixed solution of stannous chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain surface-sensitized diamond micro powder; the mass volume ratio of the stannous chloride to the mixed solution is 10-15 g/L, and the volume fraction of hydrochloric acid in the mixed solution is 5-15%; in the step, the median particle size of the diamond micropowder is D50 in unit of micron, m is the weight of the diamond micropowder in unit of gram, and the ratio of the volume of the mixed solution to the total surface area of the diamond micropowder particles is as follows: 8-12 ml: (m × D50/8); m × D50/8 is based on particles having a median particle size of 8; in the step, stannous chloride and hydrochloric acid form a colloidal solution, the diamond micro powder is placed in the stannous chloride colloidal solution, and stannous chloride colloidal particles are adsorbed on the surface of the diamond micro powder;
step two, washing the diamond micro powder treated in the step one for 2-3 times by using pure water, then placing the diamond micro powder into a mixed solution of palladium chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain activated diamond micro powder; the mass volume ratio of the palladium chloride to the mixed solution is 0.2-0.5 g/L, and the volume fraction of hydrochloric acid in the mixed solution is 5-15%; in the step, the median particle size of the diamond micropowder is D50, the unit is micrometer, m is the weight of diamond and the unit is gram, and the ratio of the volume of the mixed solution to the total surface area factor of the diamond micropowder particles is 5-10 ml: (m × D50/8); m × D50/8 is based on particles having a median particle size of 8; in the step, stannous chloride reduces palladium chloride on the surface of the diamond micro powder to generate stannic chloride and palladium elementary substance dissolved in water, and the palladium elementary substance replaces the original position of the stannous chloride and is adsorbed on the surface of the diamond to form a catalytic center.
Step three, washing the diamond micro powder treated in the step two for 6-10 times by using pure water, then placing the diamond micro powder into a plating solution at the temperature of 75-85 ℃ for stirring, wherein the stirring speed is 80-150 r/min, gradually adding 150-200 g/L sodium hypophosphite and 100-150 g/L nickel sulfate into the plating solution in the plating reaction process, and increasing the weight of the plated diamond micro powder by 35-55% to obtain the diamond micro powder with the surface plated; the median particle size of the diamond micropowder in the step is D50, the unit is micrometer, m is the weight of diamond, the unit is gram, and the ratio of the volume of the plating solution to the total surface area factor of the diamond micropowder particles is 100-200 ml: (m × D50/8); m × D50/8 is based on particles having a median particle size of 8; the plating solution in the step comprises 30-35 g/L of nickel sulfate, 40-45 g/L of sodium hypophosphite, 15-20 g/L of boric acid, 13-15 g/L of citric acid, 10-15 g/L of lactic acid, 1-2 mg/L of thiourea, 30-50 mg/L of potassium iodate and 0.2-0.3 g/L of sodium dodecyl benzene sulfonate. The plating process is as follows: in the process of reducing nickel sulfate by sodium hypophosphite, thiourea and potassium iodate are used as stabilizers to reduce the plating speed, reduce the generation of free nickel particles and prevent the self-decomposition of plating solution, boric acid is a pH regulator, H & lt + & gt can be generated in the reaction process and used for stabilizing the pH value, lactic acid and citric acid are complexing agents to reduce free Ni & lt + & gt, so that the reaction is more stable, and sodium dodecyl benzene sulfonate is a surfactant to prevent diamond particles from agglomerating. The nickel plating weight gain index H ranges from 30% to 55%, the weight after nickel plating is B, the weight of the diamond before nickel plating is A, the median particle size of the diamond micro powder is D50, the unit is micrometer, m is the weight of the diamond, the unit is gram, and the nickel plating weight gain index H = (B-A) × (8/D50)/B).
Step four, cleaning the diamond micro powder treated in the step three by using pure water, drying, then rapidly treating at a high temperature of 900-1000 ℃, sintering for 5-10 min, and taking out and rapidly cooling; in the process, the nickel film is expanded by high-temperature quick firing, and is quickly shrunk by quick cooling, and the ductility of the nickel film is too late to form a new film, so that the nickel film is shrunk into nickel particles;
step five, carrying out high-temperature treatment on the diamond micro powder treated in the step four, wherein the heating rate is 3-7 ℃/min, keeping the temperature for 4-9 hours at the temperature of 500-650 ℃, and then reducing the temperature to room temperature at the cooling rate of 3-7 ℃/min for later use; in the high-temperature heat preservation process, the solid solubility of nickel metal and carbon is higher, and diamond is dissolved in a contact area of nickel particles, so that corrosion is formed.
And sixthly, removing impurities from the diamond micro powder treated in the fifth step by sequentially adopting hydrochloric acid and perchloric acid, wherein the treatment temperature of the hydrochloric acid is 45-65 ℃, the treatment temperature of the perchloric acid is 220-280 ℃, then cleaning for 4-7 times by using pure water, and drying to obtain the multi-edge diamond abrasive particles.
The method provided by the invention is adopted to sharpen the surface of the diamond, corrode the crystal face which is easy to corrode by anisotropic etching, and simultaneously reserve the crystal face with high mechanical strength and higher chemical bond energy;
the prepared multi-edge diamond abrasive particles have rough surfaces and large specific surface areas, can greatly enhance holding force by being embedded in a bonding agent, improve the service life and the grinding and cutting efficiency of a diamond product,
the median particle size of the diamond micro powder is reduced by 0.3-0.7 microns compared with the original diamond micro powder, but the crystal form of the original diamond micro powder is not changed, and the specific surface area of the multi-edge diamond abrasive particles is increased to 1.5-3 times of that of the untreated diamond micro powder.
It is further noted that relational terms such as i, ii, and iii may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Claims (6)
1. A method for preparing multi-edge diamond abrasive particles is characterized by comprising the following steps: the method comprises the following steps:
placing diamond micro powder in a mixed solution of stannous chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain surface-sensitized diamond micro powder;
step two, washing the diamond micro powder treated in the step one for 2-3 times by using pure water, then placing the diamond micro powder into a mixed solution of palladium chloride and hydrochloric acid, and stirring for 10-15 min at the temperature of 35-40 ℃ to obtain activated diamond micro powder;
step three, washing the diamond micro powder treated in the step two for 6-10 times by using pure water, then placing the diamond micro powder into a plating solution at the temperature of 75-85 ℃ for stirring at the stirring speed of 80-150 r/min until the plating reaction is finished, and obtaining diamond micro powder with the plated surface;
the plating solution comprises 30-35 g/L of nickel sulfate, 40-45 g/L of sodium hypophosphite, 15-20 g/L of boric acid, 13-15 g/L of citric acid, 10-15 g/L of lactic acid, 1-2 mg/L of thiourea, 30-50 mg/L of potassium iodate and 0.2-0.3 g/L of sodium dodecyl benzene sulfonate in a mass-volume ratio;
in the process of plating reaction, sodium hypophosphite with the mass volume ratio of 150-200 g/L and nickel sulfate with the mass volume ratio of 100-150 g/L are gradually added into the plating solution, and the weight of the diamond micro powder is increased by 35-55% after plating;
step four, cleaning the diamond micro powder treated in the step three by using pure water, drying, then rapidly treating at a high temperature of 900-1000 ℃, sintering for 5-10 min, and taking out and rapidly cooling;
step five, carrying out high-temperature treatment on the diamond micro powder treated in the step four, carrying out heat preservation treatment for 4-9 hours at the temperature of 500-650 ℃, and cooling to room temperature for later use;
and sixthly, removing impurities from the diamond micro powder treated in the fifth step by sequentially adopting hydrochloric acid and perchloric acid, wherein the treatment temperature of the hydrochloric acid is 45-65 ℃, the treatment temperature of the perchloric acid is 220-280 ℃, then cleaning for 4-7 times by using pure water, and drying to obtain the multi-edge diamond abrasive particles.
2. The method for producing a multi-edged diamond abrasive grain according to claim 1, wherein: in the first step, the median particle size of the diamond micropowder is D50 in microns, m is the weight of the diamond micropowder in grams, and the ratio of the volume of the mixed solution to the total surface area factor of the diamond micropowder particles is as follows: 8-12 ml: (m × D50/8).
3. The method for producing a multi-edged diamond abrasive grain according to claim 1, wherein: in the first step, the mass volume ratio of the stannous chloride to the mixed solution is 10-15 g/L, and the volume fraction of the hydrochloric acid is 5-15%.
4. The method for producing a multi-edged diamond abrasive grain according to claim 1, wherein: in the second step, the median particle size of the diamond micro powder is D50, the unit is micron, m is the weight of diamond and the unit is gram, and the ratio of the volume of the mixed solution to the total surface area factor of the diamond micro powder particles is 5-10 ml: (m × D50/8).
5. The method for producing a multi-edged diamond abrasive grain according to claim 1, wherein: in the second step, the mass volume ratio of the palladium chloride to the mixed solution is 0.2-0.5 g/L, and the volume fraction of the hydrochloric acid is 5-15%.
6. The method for producing a multi-edged diamond abrasive grain according to claim 1, wherein: in the third step, the median particle size of the diamond micropowder is D50, the unit is micrometer, m is the weight of diamond, the unit is gram, and the ratio of the volume of the plating solution to the total surface area factor of the diamond micropowder particles is 100-200 ml: (m × D50/8).
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| CN116285892A (en) * | 2022-12-26 | 2023-06-23 | 河南省惠丰金刚石有限公司 | Self-sharpening agglomerated abrasive for resin grinding tool |
| CN116218469A (en) * | 2022-12-26 | 2023-06-06 | 河南省惠丰金刚石有限公司 | Self-sharpening agglomerated abrasive |
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