CN117862967A - Diamond surface treatment process - Google Patents
Diamond surface treatment process Download PDFInfo
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- CN117862967A CN117862967A CN202410284107.7A CN202410284107A CN117862967A CN 117862967 A CN117862967 A CN 117862967A CN 202410284107 A CN202410284107 A CN 202410284107A CN 117862967 A CN117862967 A CN 117862967A
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- 239000010432 diamond Substances 0.000 title claims abstract description 154
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 137
- 238000000034 method Methods 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 18
- 238000004381 surface treatment Methods 0.000 title claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 78
- 238000007747 plating Methods 0.000 claims abstract description 50
- 230000007246 mechanism Effects 0.000 claims abstract description 37
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 230000007480 spreading Effects 0.000 claims abstract description 8
- 239000012530 fluid Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 67
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 46
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 40
- 229910052802 copper Inorganic materials 0.000 claims description 30
- 239000010949 copper Substances 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000013016 damping Methods 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 229910052759 nickel Inorganic materials 0.000 claims description 23
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 14
- 206010070834 Sensitisation Diseases 0.000 claims description 13
- 230000008313 sensitization Effects 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 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 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910052763 palladium Inorganic materials 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000001509 sodium citrate Substances 0.000 claims description 10
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 10
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 229910000343 potassium bisulfate Inorganic materials 0.000 claims description 7
- 239000004323 potassium nitrate Substances 0.000 claims description 7
- 235000010333 potassium nitrate Nutrition 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000002131 composite material Substances 0.000 description 6
- 239000011889 copper foil Substances 0.000 description 5
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910001431 copper ion Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
Landscapes
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention discloses a diamond surface treatment process, which specifically comprises the following steps: step one: cleaning the diamond, spreading the diamond in a lifting fence, installing the lifting fence in a grinding mechanism, pouring grinding fluid into the grinding mechanism, and starting the grinding mechanism to grind the surface of the diamond for 5-15min; before plating the diamond, the grinding mechanism is used for grinding the diamond surface in the lifting fence, so that impurities on the diamond surface can be removed, the phenomenon that the impurities which are difficult to clean are used for reducing the stability of a film formed by plating on the diamond surface when the diamond surface is plated is avoided, and meanwhile, fine protrusions or depressions can be formed on the diamond surface by grinding the diamond surface, so that the adhesion strength of the film on the diamond surface is improved.
Description
Technical Field
The invention relates to the technical field of diamond treatment, in particular to a diamond surface treatment process.
Background
Diamond is a material having excellent hardness, wear resistance, thermal conductivity and electrical insulation, and is widely used in the fields of industry, medical treatment, scientific research, etc. However, diamond also has some limitations such as high processing difficulty, high processing cost, low processing efficiency, etc., which limit the performance of diamond in certain applications, and thus, diamond is surface plated to improve its surface properties.
Chinese patent discloses a method for coating copper on the surface of diamond/copper composite material (grant bulletin number: CN 112974809B), wherein spherical copper powder or copper foil is laid in a mold, diamond/copper composite material is placed, spherical copper powder or copper foil with a certain thickness is laid on the surface of diamond/copper composite material; or spreading spherical copper powder or copper foil in the mold, and placing diamond/copper composite material on the spherical copper powder or copper foil; or placing the diamond/copper composite material in a mould, spreading spherical copper powder or copper foil on the surface of the diamond/copper composite material, and spark plasma sintering, wherein the surface of the diamond possibly has certain impurities, and a film formed during plating covers the surface of the impurities, so that the film adhesion capability is lower during use.
Disclosure of Invention
The invention aims to provide a diamond surface treatment process, which is characterized in that before plating diamond, the diamond surface in a lifting fence is ground by a grinding mechanism, so that impurities on the diamond surface can be removed, the phenomenon that the stability of a film formed by plating is reduced when the impurities which are difficult to clean are plated on the diamond surface, and meanwhile, fine bulges or depressions on the diamond surface can be increased when the diamond surface is ground, so that the adhesion strength of the film on the diamond surface is improved.
The aim of the invention can be achieved by the following technical scheme:
the diamond surface treatment process specifically comprises the following steps:
step one: cleaning the diamond, spreading the diamond in a lifting fence, installing the lifting fence in a grinding mechanism, pouring grinding fluid into the grinding mechanism, and starting the grinding mechanism to grind the surface of the diamond for 5-15min;
step two: after finishing grinding, taking down the lifting fence from the grinding mechanism, cleaning the diamond in the lifting fence by deionized water, and drying the diamond by nitrogen;
step three: placing the dried diamond and the lifting fence into a sensitization pond, adding a palladium sulfate solution and a potassium hydrogen sulfate solution into the sensitization pond, and soaking for 10-15min;
step four: immersing the sensitized diamond in a nickel plating solution, heating the nickel plating solution to 80-100 ℃ and stirring for 30min, transferring diamond particles into a copper plating solution, heating the copper plating solution to 60-80 ℃ and stirring for 60min;
step five: and taking out the deposited diamond, flushing the diamond by deionized water, putting the diamond into a solution containing potassium nitrate and boric acid at the temperature of 100 ℃ for 10 minutes, and taking out the diamond to dry.
As a further scheme of the invention: in the third step, the mass fraction of the palladium sulfate solution is 0.01% -0.1%, and the mass fraction of the potassium hydrogen sulfate solution is 0.1% -1%.
As a further scheme of the invention: the preparation method of the nickel plating solution in the fourth step comprises the following steps: the method comprises the following steps:
a1: adding 500ml of deionized water, 150-200g of nickel sulfate, 30-50g of sodium sulfate, 80-100g of sodium citrate, 40-50g of sodium ethylenediamine tetraacetate and 7-10g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution A;
a2: adding deionized water again to dilute the reaction kettle to dilute the mixed solution A to 1000ml, thereby obtaining the nickel plating solution.
As a further scheme of the invention: the preparation method of the copper plating solution in the fourth step comprises the following steps:
b2: adding 500ml of deionized water, 150-200g of copper sulfate, 30-50g of sodium sulfate, 80-100g of sodium citrate, 40-50g of sodium ethylenediamine tetraacetate and 7-10g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution B;
b2: adding deionized water again to dilute the mixed solution B to 1000ml, thereby obtaining copper plating solution.
As a further scheme of the invention: in the fifth step, the mass fraction of the potassium nitrate solution is 5-15%, and the mass fraction of the boric acid solution is 1-5%.
As a further scheme of the invention: the grinding mechanism comprises a mounting frame, a placing groove is formed in the mounting frame, a liquid outlet pipe used for liquid discharge is arranged on one side of the placing groove in a penetrating mode, a separation plate is fixedly connected to the inner surface of the placing groove, a plurality of ultrasonic transducers are fixedly connected to the bottom of the separation plate, and a grinding assembly used for increasing the adhesion capacity of the diamond surface is arranged in the mounting frame;
the grinding assembly comprises a connecting seat capable of lifting, an electric telescopic rod capable of driving the connecting seat to move up and down and a grinding disc for grinding diamond, wherein a driving motor is fixedly connected to the top of the connecting seat, an output shaft is fixedly connected to the bottom output end of the driving motor, the bottom end of the output shaft penetrates through the connecting seat and is connected with a connecting sleeve, the grinding disc is arranged at the bottom of the connecting sleeve, the electric telescopic rod is arranged inside the mounting frame, the top of the electric telescopic rod is fixedly connected with a side opening rod, the outer surface of the side opening rod is slidably connected with a sliding sleeve, the output end of the electric telescopic rod is fixedly connected with the inner surface of the sliding sleeve, a supporting rod is fixedly connected with the connecting seat, a connecting spring is sleeved on the surface of the output shaft, the bottom end of the connecting spring is fixedly connected with the top of the connecting sleeve, a plurality of limiting strips are fixedly connected to the bottom of the output shaft, and clamping grooves matched with the limiting strips are formed in the inner surface of the connecting sleeve.
As a further scheme of the invention: the lifting fence comprises an annular plate fixedly mounted on a connecting seat, a connecting plate sleeved on the annular plate and a bottom plate for placing diamonds, wherein a fixing ring is arranged at the bottom of the connecting plate through a connecting assembly, the connecting assembly is used for rapidly taking and placing diamonds in a grinding mechanism and a sensitization pond so as to move mass diamonds, a plurality of connecting rods are fixedly connected to the bottom of the fixing ring, a limiting ring used for limiting the diamonds is fixedly connected to the top of the bottom plate, and the top of the limiting ring is fixedly connected with the bottom end of the connecting rods.
As a further scheme of the invention: the connecting assembly comprises a plurality of through grooves on the connecting plate and a limiting rod in the through grooves, wherein a plurality of damping strips used for limiting are fixedly connected to the outer surface of the limiting rod, a plurality of limiting grooves are formed in the top of the fixing ring, and a plurality of damping rings used for limiting the damping strips are fixedly connected to the inner surfaces of the limiting grooves.
The invention has the beneficial effects that:
1. according to the invention, before plating the diamond, the diamond surface in the lifting fence is ground by the grinding mechanism, so that impurities on the diamond surface can be removed, the phenomenon that the stability of a film formed by plating is reduced when the impurities which are difficult to clean are plated on the diamond surface is avoided, and meanwhile, fine bulges or depressions are generated on the diamond surface by grinding the diamond surface, so that the adhesion strength of the film on the diamond surface is improved.
2. According to the invention, the placing groove is arranged in the grinding mechanism, the ultrasonic transducer is matched to vibrate the grinding liquid in the placing groove, so that the grinding liquid is uniformly dispersed, microbubbles in the liquid continuously vibrate under the action of sound waves to destroy and separate dirt and impurities attached to the surface of the diamond, the grinding disc is driven to grind the surface of the diamond by the rotation of the driving motor in the grinding mechanism, the efficiency of grinding the diamond can be improved by utilizing polycrystalline diamond in the grinding liquid, and certain pressure is given to the diamond when the grinding disc rotates by matching with the connecting spring on the surface of the output shaft, so that the grinding efficiency of the diamond can be further improved.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of a diamond surface treatment process according to the present invention;
FIG. 2 is a schematic view showing the use state of the internal structure of the grinding mechanism in the present invention;
FIG. 3 is a schematic view showing the internal structure of the grinding mechanism of the present invention;
FIG. 4 is a schematic diagram of the connection of the lifting rail to the connection base in the present invention;
FIG. 5 is a top view of the connection sleeve of the present invention;
fig. 6 is an enlarged view of a partial structure at a in fig. 4 according to the present invention.
In the figure: 1. hoisting a fence; 10. a bottom plate; 11. a connecting plate; 12. a fixing ring; 13. a connecting rod; 14. a limiting ring; 15. a limit rod; 16. damping strips; 17. a through groove; 18. a limit groove; 19. a damping ring; 2. a grinding mechanism; 21. a mounting frame; 22. a placement groove; 23. a liquid outlet pipe; 24. a partition plate; 25. an ultrasonic transducer; 26. an electric telescopic rod; 27. a side opening rod; 28. a sliding sleeve; 29. a support rod; 210. a connecting seat; 211. a driving motor; 212. an output shaft; 213. connecting sleeves; 214. grinding disc; 215. a connecting spring; 216. a limit bar; 217. clamping grooves, 218 and an annular plate.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-6, the present invention provides the following embodiments.
Example 1
The diamond surface treatment process specifically comprises the following steps:
step one: cleaning the diamond, spreading the diamond in the lifting fence 1, installing the lifting fence 1 in a grinding mechanism, pouring grinding fluid into the grinding mechanism 2, and starting the grinding mechanism 2 to grind the surface of the diamond for 5min;
step two: after finishing grinding, taking the lifting fence 1 off the grinding mechanism 2, cleaning the diamond in the lifting fence 1 by deionized water, and then drying the diamond by nitrogen;
step three: placing the dried diamond together with the lifting column 1 into a sensitization pond, and adding 0.01% palladium sulfate (PdSO) into the sensitization pond 4 ) Solution and potassium bisulfate (KHSO) with mass fraction of 0.1% 4 ) Soaking the solution for 10min to enable palladium sulfate to be adsorbed on the surface of the diamond so as to form a layer of catalytic center;
step four: immersing the sensitized diamond in a nickel plating solution, heating the nickel plating solution to 80-100 ℃ and stirring for 30min, transferring diamond particles into a copper plating solution, heating the copper plating solution to 60 ℃ and stirring for 60min, so that copper ions undergo a reduction reaction on a nickel layer and are deposited on the surface of the diamond;
step five: taking out the deposited diamond, washing with deionized water, and adding potassium nitrate (KNO) with mass fraction of 5% 3 ) And boric acid (H) with mass fraction of 1% 3 BO 3 ) The temperature is 100 ℃ for 10 minutes, then annealing treatment is carried out to remove residues and stress and improve the surface smoothness and stability of the solution, and finally the solution is taken out, filtered and dried to obtain the copper plating layer.
The preparation method of the nickel plating solution in the fourth step comprises the following steps: the method comprises the following steps:
a1: adding 500ml of deionized water, 150g of nickel sulfate, 30g of sodium sulfate, 80g of sodium citrate, 40g of sodium ethylenediamine tetraacetate and 7g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution A;
a2: adding deionized water again to dilute the reaction kettle to dilute the mixed solution A to 1000ml, thereby obtaining the nickel plating solution.
The preparation method of the copper plating solution in the fourth step comprises the following steps:
b2: adding 500ml of deionized water, 150g of copper sulfate, 30g of sodium sulfate, 80g of sodium citrate, 40g of sodium ethylenediamine tetraacetate and 70g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution B;
b2: adding deionized water again to dilute the mixed solution B to 1000ml, thereby obtaining copper plating solution.
Example 2
The diamond surface treatment process specifically comprises the following steps:
step one: cleaning the diamond, spreading the diamond in the lifting fence 1, installing the lifting fence 1 in a grinding mechanism, pouring grinding fluid into the grinding mechanism 2, and starting the grinding mechanism 2 to grind the surface of the diamond for 10min;
step two: after finishing grinding, taking the lifting fence 1 off the grinding mechanism 2, cleaning the diamond in the lifting fence 1 by deionized water, and then drying the diamond by nitrogen;
step three: placing the dried diamond together with the lifting column 1 into a sensitization pond, and adding palladium sulfate (PdSO) with mass fraction of 0.05% into the sensitization pond 4 ) Solution and potassium bisulfate (KHSO) with mass fraction of 0.5% 4 ) Soaking the solution for 10min to enable palladium sulfate to be adsorbed on the surface of the diamond so as to form a layer of catalytic center;
step four: immersing the sensitized diamond in a nickel plating solution, heating the nickel plating solution to 80-100 ℃ and stirring for 30min, transferring diamond particles into a copper plating solution, heating the copper plating solution to 70 ℃ and stirring for 60min, so that copper ions undergo a reduction reaction on a nickel layer and are deposited on the surface of the diamond;
step five: taking out the deposited diamond, washing with deionized water, and adding potassium nitrate (KNO) with mass fraction of 10% 3 ) And 3% boric acid (H) 3 BO 3 ) In the solution of (2), the temperature is 100 ℃ for 10 minutes, and then annealing treatment is carried out to remove residues and stress and improve the surface smoothness and stability, and finally the solution is taken out, filtered and dried to obtainTo have a copper plating.
The preparation method of the nickel plating solution in the fourth step comprises the following steps: the method comprises the following steps:
a1: adding 500ml of deionized water, 170g of nickel sulfate, 40g of sodium sulfate, 90g of sodium citrate, 45g of sodium ethylenediamine tetraacetate and 8g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution A;
a2: adding deionized water again to dilute the reaction kettle to dilute the mixed solution A to 1000ml, thereby obtaining the nickel plating solution.
The preparation method of the copper plating solution in the fourth step comprises the following steps:
b2: adding 500ml of deionized water, 170g of copper sulfate, 40g of sodium sulfate, 90g of sodium citrate, 45g of sodium ethylenediamine tetraacetate and 8g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution B;
b2: adding deionized water again to dilute the mixed solution B to 1000ml, thereby obtaining copper plating solution.
Example 3
The diamond surface treatment process specifically comprises the following steps:
step one: cleaning the diamond, spreading the diamond in the lifting fence 1, installing the lifting fence 1 in a grinding mechanism, pouring grinding fluid into the grinding mechanism 2, and starting the grinding mechanism 2 to grind the surface of the diamond for 15min;
step two: after finishing grinding, taking the lifting fence 1 off the grinding mechanism 2, cleaning the diamond in the lifting fence 1 by deionized water, and then drying the diamond by nitrogen;
step three: placing the dried diamond together with the lifting column 1 into a sensitization pond, and adding 0.1% palladium sulfate (PdSO) into the sensitization pond 4 ) Solution and 1% potassium bisulfate (KHSO) 4 ) Soaking the solution for 10min to enable palladium sulfate to be adsorbed on the surface of the diamond so as to form a layer of catalytic center;
step four: immersing the sensitized diamond in a nickel plating solution, heating the nickel plating solution to 100 ℃ and stirring for 30min, transferring diamond particles into a copper plating solution, heating the copper plating solution to 80 ℃ and stirring for 60min, so that copper ions undergo a reduction reaction on a nickel layer and are deposited on the surface of the diamond;
step five: taking out the deposited diamond, washing with deionized water, and adding 15% potassium nitrate (KNO) 3 ) And boric acid (H) with mass fraction of 5% 3 BO 3 ) The temperature is 100 ℃ for 10 minutes, then annealing treatment is carried out to remove residues and stress and improve the surface smoothness and stability of the solution, and finally the solution is taken out, filtered and dried to obtain the copper plating layer.
The preparation method of the nickel plating solution in the fourth step comprises the following steps: the method comprises the following steps:
a1: adding 500ml of deionized water, 200g of nickel sulfate, 50g of sodium sulfate, 100g of sodium citrate, 50g of sodium ethylenediamine tetraacetate and 10g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution A;
a2: adding deionized water again to dilute the reaction kettle to dilute the mixed solution A to 1000ml, thereby obtaining the nickel plating solution.
The preparation method of the copper plating solution in the fourth step comprises the following steps:
b2: adding 500ml of deionized water, 200g of copper sulfate, 50g of sodium sulfate, 100g of sodium citrate, 50g of sodium ethylenediamine tetraacetate and 10g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution B;
b2: adding deionized water again to dilute the mixed solution B to 1000ml, thereby obtaining copper plating solution.
Comparative example 1
On the basis of example 2, steps one and two were not carried out, the remaining steps remaining unchanged.
The diamonds obtained in examples 1-3 and comparative example 1 were tested as follows:
the obtained diamond was placed in a sealed furnace at 500 ℃ and immersed in a solution containing 10% hydrochloric acid, 10% sulfuric acid, 10% nitric acid, and 10% sodium carbonate, and stirred, and after 24 hours of holding, the weight change rate (x) of the diamond was measured, the weight before test was designated as a, and the weight after test was designated as b, where x= (1-b/a)%, and the test results were as follows:
TABLE 1
，
As is clear from table 1, the weight change rates of the diamonds in examples 1 to 3 were all smaller than that of the diamond in comparative example 1, and the stability of adhesion of the copper-nickel alloy to the diamond surface was improved by grinding the diamond before coating the diamond.
The grinding mechanism 2 in the embodiments 1-3 comprises a mounting frame 21, a placing groove 22 is arranged on the mounting frame 21, a liquid outlet pipe 23 for liquid discharge is arranged on one side of the placing groove 22 in a penetrating manner, a separation plate 24 is fixedly connected to the inner surface of the placing groove 22, a plurality of ultrasonic transducers 25 are fixedly connected to the bottom of the separation plate 24, the ultrasonic transducers 25 are matched with an ultrasonic generator to be used as the prior art, excessive details are not needed, and a grinding component for increasing the adhesive capacity of the diamond surface is arranged in the mounting frame 21;
the grinding assembly comprises an electric telescopic rod 26 arranged inside a mounting frame 21, a side opening rod 27 is fixedly connected to the top of the electric telescopic rod 26, a sliding sleeve 28 is slidably connected to the outer surface of the side opening rod 27, the output end of the electric telescopic rod 26 is fixedly connected with the inner surface of the sliding sleeve 28, a supporting rod 29 is fixedly connected to one side of the sliding sleeve 28, a connecting seat 210 is fixedly connected to the supporting rod 29, a driving motor 211 is fixedly connected to the top of the connecting seat 210, an output shaft 212 is fixedly connected to the bottom output end of the driving motor 211, the bottom of the output shaft 212 penetrates through the connecting seat 210 and is connected with a connecting sleeve 213, a grinding disc 214 for grinding diamonds is fixedly connected to the bottom of the connecting sleeve 213, the mesh number of the grinding disc 214 is 100-200 meshes, a connecting spring 215 is sleeved on the surface of the output shaft 212, the bottom of the connecting spring 215 is fixedly connected with the top of the connecting sleeve 213, a plurality of limiting strips 216 are fixedly connected to the inner surface of the connecting sleeve 213, clamping grooves 217 matched with the limiting strips 216 are formed in the inner surface of the connecting sleeve 213, sliding between the output shaft 212 and the connecting sleeve 213 can be kept through the matching of the limiting strips 216 and the clamping grooves 217.
The lifting fence 1 in the embodiments 1-3 comprises an annular plate 218 fixedly installed on a connecting seat 210, a connecting plate 11 sleeved on the annular plate 218 and a bottom plate 10 for placing diamonds, wherein the connecting plate 11 is supported by the annular plate 218, a fixed ring 12 is arranged at the bottom of the connecting plate 11 through a connecting component, the connecting component rapidly picks up and places the diamonds in a grinding mechanism 2 and a sensitization pond, so that a large number of diamonds are moved, a plurality of connecting rods 13 are fixedly connected to the bottom of the fixed ring 12, the distance between two adjacent connecting rods 13 is larger than the width of the diamonds, the diamonds are prevented from passing through the two connecting rods 13, a limiting ring 14 for limiting the diamonds is fixedly connected to the top of the bottom plate 10, and the top of the limiting ring 14 is fixedly connected with the bottom ends of the connecting rods 13;
the connecting assembly comprises a plurality of penetrating grooves 17 which are formed in a penetrating mode and are positioned at the top of the connecting plate 11, limiting rods 15 are slidably connected to the inner surfaces of the penetrating grooves 17, a plurality of damping strips 16 used for limiting are fixedly connected to the outer surfaces of the limiting rods 15, a plurality of limiting grooves 18 are formed in the tops of the fixing rings 12, a plurality of damping rings 19 used for limiting the damping strips 16 are fixedly connected to the inner surfaces of the limiting grooves 18, a gap used for containing the damping rings 19 to penetrate is reserved between the upper damping strips 16 and the lower damping strips 16, a gap used for containing the damping strips 16 to penetrate is reserved between the same left damping rings 19 and the same right damping rings 19, rotation of the limiting rods 15 can be prevented through damping between the damping rings 19 and the damping strips 16, and the lifting fence 1 can be used in multiple pieces of equipment, and is convenient to take out and place a large number of diamonds.
The working principle is as follows: firstly, diamond to be ground is placed on the bottom plate 10, then the fixed ring 12 is sleeved outside the connecting seat 210 from bottom to top and is contacted with the bottom of the connecting plate 11, at this time, the limiting rod 15 is inserted into the limiting groove 18, the damping strips 16 penetrate between the two damping rings 19 until the bottom end of the limiting rod 15 is contacted with the bottom of the inner cavity of the limiting groove 18, then the limiting rod 15 is rotated, the damping rings 19 are positioned between the upper damping strip 16 and the lower damping strip 16, so that the mounting of the lifting rail 1 is completed, at this time, the side opening rod 27 is started to shorten and drive the sliding sleeve 28 to slide downwards on the surface of the side opening rod 27, so that the supporting rod 29 on the sliding sleeve 28 is driven to move downwards, the lifting rail 1 on the connecting seat 210 is further placed on the isolating plate 24, at this time, the electric telescopic rod 26 is continuously shortened, so that the connecting plate 11 moves on the surface of the connecting seat 210, the grinding disc 214 is contacted with diamond, the output shaft 212 slides downwards in the inner part of the limiting groove 18, and the connecting spring 215 is in a compressed state, so that diamond pressure is given, then the damping ring 19 is positioned between the upper damping strip 16 and lower damping strip 16, so that the mounting of the lifting rail 22 is completed, at this time, the side opening rod 27 is started to drive the sliding sleeve 28, the surface of the lifting rod 27, the lifting rod 29 is driven to slide on the side opening rod 27, the diamond, the lifting rod is driven to rotate the diamond table, and the diamond carrier 214, and the ultrasonic grinding ultrasonic wave is driven to rotate the diamond carrier 214, and the ultrasonic grinding ultrasonic wave groove 214 is driven and the ultrasonic transducer to rotate the lifting the diamond roller.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (8)
1. The diamond surface treatment process is characterized by comprising the following steps of:
step one: cleaning diamond, spreading the diamond in a lifting fence (1), installing the lifting fence (1) in a grinding mechanism, pouring grinding fluid into the grinding mechanism (2), and starting the grinding mechanism (2) to grind the surface of the diamond for 5-15min;
step two: after finishing grinding, taking the lifting fence (1) off the grinding mechanism (2), cleaning the diamond in the lifting fence (1) by deionized water, and then drying the diamond by nitrogen;
step three: putting the dried diamond and the lifting fence (1) into a sensitization pond, adding a palladium sulfate solution and a potassium hydrogen sulfate solution into the sensitization pond, and soaking for 10-15min;
step four: immersing the sensitized diamond in a nickel plating solution, heating the nickel plating solution to 80-100 ℃ and stirring for 30min, transferring diamond particles into a copper plating solution, heating the copper plating solution to 60-80 ℃ and stirring for 60min;
step five: and taking out the deposited diamond, flushing the diamond by deionized water, putting the diamond into a solution containing potassium nitrate and boric acid at the temperature of 100 ℃ for 10 minutes, and taking out the diamond to dry.
2. A diamond surface treatment process according to claim 1, wherein in step three, the mass fraction of the palladium sulfate solution is 0.01% -0.1%, and the mass fraction of the potassium hydrogen sulfate solution is 0.1% -1%.
3. The diamond surface treatment process according to claim 1, wherein the preparation method of the nickel plating solution in the fourth step comprises: the method comprises the following steps:
a1: adding 500ml of deionized water, 150-200g of nickel sulfate, 30-50g of sodium sulfate, 80-100g of sodium citrate, 40-50g of sodium ethylenediamine tetraacetate and 7-10g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution A;
a2: adding deionized water again to dilute the reaction kettle to dilute the mixed solution A to 1000ml, thereby obtaining the nickel plating solution.
4. The diamond surface treatment process according to claim 1, wherein the preparation method of the copper plating solution in the fourth step comprises the following steps:
b2: adding 500ml of deionized water, 150-200g of copper sulfate, 30-50g of sodium sulfate, 80-100g of sodium citrate, 40-50g of sodium ethylenediamine tetraacetate and 7-10g of sodium hypophosphite into a reaction kettle in sequence, and stirring through the reaction kettle to obtain a mixed solution B;
b2: adding deionized water again to dilute the mixed solution B to 1000ml, thereby obtaining copper plating solution.
5. The diamond surface treatment process according to claim 1, wherein in the fifth step, the mass fraction of the potassium nitrate solution is 5-15%, and the mass fraction of the boric acid solution is 1-5%.
6. The diamond surface treatment process according to claim 1, wherein the grinding mechanism (2) comprises a mounting frame (21), a placing groove (22) is formed in the mounting frame (21), a liquid outlet pipe (23) for discharging liquid is arranged on one side of the placing groove (22) in a penetrating mode, a separation plate (24) is fixedly connected to the inner surface of the placing groove (22), a plurality of ultrasonic transducers (25) are fixedly connected to the bottom of the separation plate (24), and a grinding assembly for increasing the adhesion capacity of the diamond surface is arranged in the mounting frame (21);
the grinding assembly comprises a connecting seat (210) capable of lifting, an electric telescopic rod (26) for driving the connecting seat (210) to move up and down and a grinding disc (214) for grinding diamond, wherein the top of the connecting seat (210) is fixedly connected with a driving motor (211), the bottom output end of the driving motor (211) is fixedly connected with an output shaft (212), the bottom end of the output shaft (212) penetrates through the connecting seat (210) and is connected with a connecting sleeve (213), and the grinding disc (214) is arranged at the bottom of the connecting sleeve (213).
7. The diamond surface treatment process according to claim 6, wherein the lifting fence (1) comprises an annular plate (218) fixedly installed on a connecting seat (210), a connecting plate (11) sleeved on the annular plate (218) and a bottom plate (10) for placing diamonds, the bottom of the connecting plate (11) is provided with a fixing ring (12) through a connecting component, the connecting component is used for taking and placing the diamonds in the grinding mechanism (2) and the sensitization pond, a plurality of connecting rods (13) are fixedly connected to the bottom of the fixing ring (12), a limiting ring (14) used for limiting the diamonds is fixedly connected to the top of the bottom plate (10), and the top of the limiting ring (14) is fixedly connected with the bottom end of the connecting rod (13).
8. The diamond surface treatment process according to claim 7, wherein the connecting assembly comprises a plurality of through grooves (17) positioned on the connecting plate (11) and a limiting rod (15) positioned in the through grooves (17), a plurality of damping strips (16) used for limiting are fixedly connected to the outer surface of the limiting rod (15), a plurality of limiting grooves (18) are formed in the top of the fixing ring (12), and a plurality of damping rings (19) used for limiting the damping strips (16) are fixedly connected to the inner surface of the limiting grooves (18).
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