CN104894614A - Electroplating liquid for preparing nickel plating thorn abrasive grains and electroplating method - Google Patents
Electroplating liquid for preparing nickel plating thorn abrasive grains and electroplating method Download PDFInfo
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Abstract
The invention relates to electroplating liquid for preparing nickel plating thorn abrasive grains and an electroplating method; and the electroplating liquid contains water solution of the following components: nickel sulfate, boric acid, sodium chloride, aminobenzenesulfonic acid and benzene sulfinic acid sodium salt. The nickel plating thorn abrasive grains, prepared by the electroplating liquid, have a lot of needle-shaped or rod-shaped nickel thorns on the surfaces; the binding force of the nickel plating thorn abrasive grains and a resin binding agent is improved by 50-200% compared with general nickel plating abrasive grains; and the service life of resin binding agent abrasive tools, prepared by the product, is prominently prolonged.
Description
Technical field
The present invention relates to electroplate liquid, be specifically related to a kind of electroplate liquid and the electro-plating method of producing nickel plating thorn abrasive particle.
Background technology
Diamond has high rigidity, high strength, and the physics-chem characteristic of high-wearing feature and a series of excellence such as linear expansivity is little, obtains increasingly extensive application in ground finish field.But at normal temperatures and pressures, diamond is inferior stable state, and its thermotolerance is not high, and there are some surface imperfection, in the course of processing, often can there is the reaction such as oxidation weight loss or greying thus reduce working (machining) efficiency.In addition, owing to being generally mechanically inlay between diamond abrasive grain and bonding agent in grinding tool, under the effect of grinding force, diamond abrasive grain very easily comes off, thus the work-ing life of grinding tool is had a greatly reduced quality.
Along with the continuous expansion of diamond abrasive grain purposes, how to improve adamantine intensity, how to extend the work-ing life of goods and arouse great concern, and take various processing and treating method.Wherein diamond surface plating layer of metal is a kind of the most effective method.
Can give diamond many new characteristics in diamond surface nickel plating: the physical and chemical performance improve the Interface adhesive strength of adamantine intensity, diamond and matrix, oxygen barrier is protected, alleviating diamond thermal damage degree, improve diamond and basal body interface, wear resistance and the cutting power of diamond tool can also be improved.
Wang Yanhui etc. are at diamond surface nickel plating technology research (sufacing, 22nd volume the 1st phase in 1993,12-14) mention in a literary composition: because diamond particle surface plating Ni is to improve adamantine intensity and the cohesiveness with resene bonding agent, the bonding force of shaggy coating and bonding agent is higher, and diamond particles is difficult drop-off more.He adopts the formula of the dark Ni of common plating to be: Ni SO46H2O, 200g/L; H3BO3,30g/L; NaCl, 15g/L; PH value 4.5-5.5, temperature 35 DEG C, and adopt upper limit current density l.5A/d m2., also mention in the document, before electroless plating, diamond particles will carry out sensitization, activation and reduction treatment meanwhile, and object forms metal particle at diamond surface, makes chemical plating depend on these metal particles and be formed in diamond top layer.
Xu Xiangtao is at the adamantine manufacture of nickel plating and applied research (Xu Xiangtao, the adamantine manufacture of nickel plating and applied research, superhard material engineering, 17th volume the 3rd phase total 61st phase in 2005,25-30) disclose nickel plating in a literary composition and have two kinds of methods, one is chemical nickel plating, a kind of is plating, plating solution formula is single nickel salt 200g/L, rose vitriol 19g/L, boric acid 30g/L, sodium-chlor 15g/L, and pH value is 4-4.5, and temperature is 40 ± 2 DEG C.
But, there are the following problems for common nickel plating Buddha's warrior attendant abrasive particle stone: when for resinoid bonded grinding tool, cohesive force between common nickel plating diamond abrasive grain and resinoid bond is lower, abrasive particle easily comes off from resinoid bond, cause grinding tool low for work-ing life, and easily produce cut at workpiece surface, affect the problem of workpiece quality.
Nickel plating thorn diamond abrasive grain is that the nickel metal of surperficial institute plating presents needle prick shape form, namely diamond abrasive grain surface metal nickel present uneven in length, the different form such as ice slush shape, conch shape, mammillary, shape of growing thickly, surface roughness is much larger than common nickel plating diamond abrasive grain.Nickel plating thorn diamond abrasive grain is the same with the purposes of common nickel plating diamond abrasive grain, all be applied in resinoid bonded grinding tool, difference is: the hold of nickel plating thorn diamond abrasive grain in resinoid bond is far longer than common plating nickel gold hard rock, effect, the work-ing life of ground finish are also obviously better than the latter, effectively raise the work-ing life of grinding tool and the quality of grinding workpiece.
The superfine people of Sun Yu stings adamantine SEM microstructure (diamond and grinding materials and grinding tool engineering in nickel plating, in June, 2003, total 135th phase phase the 3rd, 53-55) in a literary composition, adamantine some SEM exterior appearances are stung in the nickel plating that illustrates of macroscopic view, but do not disclose the processing condition of barrel plating and the formula of plating solution.
The processing method of other plating solution formulas in grain surface nickel plating thorn and nickel plating thorn has no report.
Summary of the invention
The object of the invention is the shortcoming for common nickel plating diamond abrasive grain, a kind of electroplate liquid and the electro-plating method of producing nickel plating thorn abrasive particle are provided.
The first object of the present invention is to provide a kind of electroplate liquid producing nickel plating thorn abrasive particle, and described electroplate liquid is the aqueous solution containing following composition: single nickel salt, boric acid, sodium-chlor, aniline sulfonic acid, benzene sulfinic acid sodium salt and water.
Concrete, single nickel salt, the boric acid of 7-50g, the sodium-chlor of 5-25g, the aniline sulfonic acid of 0.01-0.5g, the benzene sulfinic acid sodium salt of 0.01-0.5g containing following composition: 50-300g in often liter of described electroplate liquid.
Preferably, single nickel salt, the boric acid of 25-30g, the sodium-chlor of 18-20g, the aniline sulfonic acid of 0.01-0.5g, the benzene sulfinic acid sodium salt of 0.01-0.5g containing following composition: 200-300g in often liter of described electroplate liquid.
Further preferably, single nickel salt, the boric acid of 25-30g, the sodium-chlor of 18-20g, the aniline sulfonic acid of 0.1-0.5g, the benzene sulfinic acid sodium salt of 0.1-0.5g containing following composition: 200-300g in often liter of described electroplate liquid.
The best, single nickel salt, the boric acid of 30g, the sodium-chlor of 18g, the aniline sulfonic acid of 0.2g, the benzene sulfinic acid sodium salt of 0.2g containing following composition: 300g in often liter of described electroplate liquid.
Another object of the present invention is to provide a kind of nickel plating thorn abrasive particle, and its technique comprises the following steps:
Step 1, get abrasive particle raw material 1000ct, add the stannous chloride solution 0.5-2L of 0.5-2g/L, sensitized treatment 10-40min, cleaning, obtain sensitization abrasive particle;
Add the palladium chloride solution 0.5-2L of 0.5-2g/L, activation treatment 10-40min, cleaning in step 2, the sensitization abrasive particle that obtains in step 1, obtain activation abrasive particle;
Add the ortho phosphorous acid sodium solution 0.5-2L of 10-50g/L, reduction treatment 10-40min, cleaning in step 3, the activation abrasive particle that obtains in step 2, obtain reduction abrasive particle;
Step 4, preparation 4L pre-plating solution, in often liter of pre-plating solution, the concentration of each component is: the single nickel salt of 25-375g/L, the citric acid of 10-150g/L are received, the sodium acetate of 10-150g/L, the inferior sodium phosphate of 20-300g/L, reduction abrasive particle step 3 obtained is poured in pre-plating solution and is stirred, temperature controls at 50-90 DEG C, continue plating time 20-60min, form nickel preplating abrasive particle;
Step 5, preparation 1L electroplate liquid, the concentration of each composition is: single nickel salt 50-300g/L, boric acid 7-50g/L, sodium-chlor 5-25g/L, aniline sulfonic acid 0.01-0.5g/L, benzene sulfinic acid sodium salt 0.01-0.5g/L, mix;
Step 6, nickel preplating abrasive particle step 4 obtained put into plating bottle, by bottled for described plating on rolling electroplating meter, add the electroplate liquid prepared in step 5; Electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor; Step 7, control nickel plating stage initial current are 0.5-2A; After 2-30h, electric current is tuned up 2A-3A; After 10-72h, electric current is tuned up 3-4A; Plating bottle rotating speed controls at 5-16r/min, and suitably adjusts according to current density change; Maintain bath pH values with the dilution heat of sulfuric acid of 25% in Ni-Speed, described pH value controls between 2 and 6; Nickel plating continued propagation 20-120h;
Step 8, plating terminate rear to nickel plating thorn abrasive particle collect, clean, dry, detect.
In above-mentioned abrasive particle raw material:
Described abrasive particle raw material comprises diamond and/or cubic boron nitride, described diamond be preferably in single-crystal diamond, polycrystalline diamond one or both;
The granularity of described abrasive particle raw material is tested at laser particle analyzer, D50 >=10 μm, is preferably 15-50 μm; D50 is median size;
In step 6, following setting is also carried out to plating bottle: described plating bottle is fixed with magnet, magnet number >=2 piece, in electronickelling thorn process, produces uniform magnetic field effect.
Present invention also offers the preparation method of nickel plating thorn abrasive particle, the method comprises the following steps:
Step 1, get abrasive particle raw material 1000ct, add the stannous chloride solution 0.5-2L of 0.5-2g/L, sensitized treatment 10-40min, cleaning, obtain sensitization abrasive particle;
Add the palladium chloride solution 0.5-2L of 0.5-2g/L, activation treatment 10-40min, cleaning in step 2, the sensitization abrasive particle that obtains in step 1, obtain activation abrasive particle;
Add the ortho phosphorous acid sodium solution 0.5-2L of 10-50g/L, reduction treatment 10-40min, cleaning in step 3, the activation abrasive particle that obtains in step 2, obtain reduction abrasive particle;
Step 4, preparation 4L pre-plating solution, in often liter of pre-plating solution, the concentration of each component is: the single nickel salt of 25-375g/L, the citric acid of 10-150g/L are received, the sodium acetate of 10-150g/L, the inferior sodium phosphate of 20-300g/L, reduction abrasive particle step 3 obtained is poured in pre-plating solution and is stirred, temperature controls at 50-90 DEG C, continue plating time 20-60min, form nickel preplating abrasive particle;
Step 5, preparation 1L electroplate liquid, the concentration of each composition is: single nickel salt 50-300g/L, boric acid 7-50g/L, sodium-chlor 5-25g/L, aniline sulfonic acid 0.01-0.5g/L, benzene sulfinic acid sodium salt 0.01-0.5g/L, mix;
Step 6, nickel preplating abrasive particle step 4 obtained put into plating bottle, by bottled for described plating on rolling electroplating meter, add the electroplate liquid prepared in step 5; Electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor;
Step 7, control nickel plating stage initial current are 0.5-2A; After 2-30h, electric current is tuned up 2-3A; After 10-72h, electric current is tuned up 3-4A; Plating bottle rotating speed controls at 5-16r/min, and suitably adjusts according to current density change; Maintain bath pH values with the dilution heat of sulfuric acid of 25% in Ni-Speed, described pH value controls between 2 and 6; Nickel plating continued propagation 20-120h;
Step 8, plating terminate rear to nickel plating thorn abrasive particle collect, clean, dry, detect.
In aforesaid method:
In step 6, following setting is also carried out to plating bottle: described plating bottle is fixed with magnet, magnet number >=2 piece, in electronickelling thorn process, produces uniform magnetic field effect.
Last object of the present invention is to provide the abrasive particle of above-mentioned nickel plating thorn, and its surface has a large amount of nickel thorn, described nickel thorn to present form be major axis is 2:1-10:1 needle prick shape with the ratio of minor axis; Described nickel plating thorn abrasive particle improves 50%-200% with the cohesive force of resinoid bond than common plating nickel gold hard rock, nickel plating rate of body weight gain >=30% of nickel plating thorn abrasive particle.Described rate of body weight gain refers to that in nickel plating thorn abrasive particle, nickel metal content accounts for the per-cent of the gross weight of abrasive particle raw material and nickel;
The electroplating technology of the abrasive particle of coating surface nickel thorn provided by the invention, the electroplate liquid of abrasive particle nickel plating thorn, abrasive particle nickel plating thorn has following positive beneficial effect:
1, the electroplate liquid of nickel plating thorn abrasive particle provided by the invention: benzene sulfinic acid sodium salt and adding of aniline sulfonic acid serve negative smooth effect, along with the growth of plating time, grain surface nickel dam presents crest and trough, and with negative smooth effect, the nickel deposition speed of trough slows down, crest nickel deposition speed is accelerated, and produces needle prick shape nickel thorn.
2, in preparation method:
1) the present invention carries out electronickelling process on micron particles surface, and the growth that nickel is stung presents thorn-like.In this process, nickel metal on the even plating in each molecule surface should be kept, ensure the reunion not occurring between molecule to occur because of the growth of nickel metal again.For solving this difficult problem, contriver adopts following way through repeatedly repetition test: fully and the sensitization carrying out pre-treatment of science, activation, reduction process, cause each grain surface can attachment activity center; Adjustment current density and pH value, make nickel deposition speed controlled; Optimize stirring velocity, ensure that abrasive particle can fully mix in plating bottle, do not contact anode in the plating solution again and occur serious strip.The plating leakage very easily occurred in Ni-Speed and crystal stock bad phenomenon are shown in accompanying drawing 3 and accompanying drawing 4.
2) on electro-plating method: the pH value of the current density designed by the present invention, instrument rotating speed and plating solution, by affecting the discharge effect of nickel ion deposition, the nickel plating abrasive particle with nickel thorn meeting weightening finish and require is reached in conjunction with different Plating times.
Fixedly be no less than the magnet of 2 pieces in the surrounding of circle plating bottle uniformly, be preferably 4 pieces, make plating solution inside have the magnetic field environment of a stable and uniform.Introduce the action of a magnetic field in nickel plating thorn process, nickel metal is had an impact in the sedimentation velocity of grain surface and the pattern of grain surface nickel metal, make nickel thorn effect more obvious.Magnetic field is incorporated in galvanic deposit, utilize the interaction of itself and electric field, metal ion, will have an impact to several links such as the mass transfer in electrodeposition process, surface conversion, plating solution physicochemical property, improve galvanic deposit environment, for the deposition cell obtaining superperformance provides good precondition.The impact that the introducing in magnetic field creates in the sedimentation velocity of grain surface and the pattern of grain surface nickel metal nickel metal, makes nickel sting effect more obvious.
3, the abrasive particle obtained is stung in nickel plating of the present invention, has following characteristics:
1) bonding force: the nickel plating thorn abrasive particle utilizing technical solution of the present invention to prepare, described grain surface has a large amount of needle-like or bar-shaped nickel thorn, abrasive particle improves 50%-200% with the cohesive force of resinoid bond than common nickel plating abrasive particle, and the work-ing life of the resinoid bonded grinding tool utilizing product of the present invention to prepare significantly increases.
2), in structure: the needle prick shape nickel coating major axis of gained of the present invention is 2:1-10:1 with the ratio of minor axis, coating structure is fine and close, and intensity is high, is combined firmly with abrasive particle.
Accompanying drawing explanation
Fig. 1 is adamantine electron microscopic picture before nickel plating thorn;
Fig. 2 is the electron microscopic picture of diamond salable product after nickel plating thorn.
Fig. 3 is the electron microscopic picture that after nickel plating thorn, diamond crystal stock is serious;
Fig. 4 is the electron microscopic picture that after nickel plating thorn, cubic boron nitride plating leakage is serious.
Embodiment
Set forth the present invention further below in conjunction with embodiment, but do not limit content of the present invention.
The preparation method of embodiment 1:20 μm of nickel plating thorn diamond abrasive grain
Step 1, get diamond (single-crystal diamond) the abrasive particle 1000ct of granularity 20 μm, add the stannous chloride solution 1L of 1g/L, sensitized treatment 20min, cleaning, obtain the diamond of sensitization;
Add the palladium chloride solution 1L of 1g/L, activation treatment 20min, cleaning in step 2, the sensitization diamond that obtains in step 1, obtain the diamond of activation;
Add the ortho phosphorous acid sodium solution 1L of 20g/L, reduction treatment 20min, cleaning in step 3, the activation diamond that obtains in step 2, obtain the diamond of reduction;
Step 4, preparation pre-plating solution 4L, the concentration of each composition is: single nickel salt 25g/L, Trisodium Citrate 10g/L, sodium acetate 10g/L, inferior sodium phosphate 20g/L;
The diamond of reduction step 3 obtained is poured in pre-plating solution and is stirred, and temperature controls at 60 DEG C, continues plating time 30min, forms nickel preplating diamond;
Step 5, preparation electroplate liquid 1L, the concentration of each composition is: single nickel salt 200g/L, boric acid 30g/L, sodium-chlor 18g/L, aniline sulfonic acid 0.01g/L, benzene sulfinic acid sodium salt 0.5g/L, be uniformly mixed;
Plating bottle put into by the electroplate liquid that step 6, nickel preplating diamond step 4 obtained and step 5 obtain, and by bottled for described plating on rolling electroplating meter, electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor; Described plating bottle surrounding fixes four blocks of magnet, in electronickelling thorn process, produce uniform magnetic field effect;
Step 7, control nickel plating stage initial current are 2A; After 5h, electric current is tuned up 3A; 10h after-current tunes up 4A; Bath pH values is maintained, pH=3 with the dilution heat of sulfuric acid of 25% in Ni-Speed; Plating bottle rotating speed 8r/min; Nickel plating duration 24h;
Step 8, plating terminate rear to nickel plating thorn diamond collect, clean, dry.
The preparation method of embodiment 2:30 μm of nickel plating thorn cubic boron nitride abrasive grain
Step 1, get the cubic boron nitride abrasive grain 1000ct of granularity 30 μm, add the stannous chloride solution 2L of 0.5g/L, sensitized treatment 30min, cleaning, obtain sensitized cube boron nitride;
Add the palladium chloride solution 2L of 0.5g/L, activation treatment 30min, cleaning in step 2, the sensitized cube boron nitride that obtains in step 1, obtain activation cubic boron nitride;
Add the ortho phosphorous acid sodium solution 2L of 30g/L, reduction treatment 30min, cleaning in step 3, the activation cubic boron nitride that obtains in step 2, obtain reduction cubic boron nitride;
Step 4, preparation pre-plating solution 4L, the concentration of each composition is: single nickel salt 250g/L, Trisodium Citrate 100g/L, sodium acetate 100g/L, inferior sodium phosphate 200g/L;
Reduction cubic boron nitride step 3 obtained is poured in pre-plating solution and is stirred, and temperature controls at 80 DEG C, continues plating time 40min, forms nickel preplating cubic boron nitride;
Step 5, preparation electroplate liquid 1L, the concentration of each composition is: single nickel salt 270g/L, boric acid 25g/L, sodium-chlor 20g/L, aniline sulfonic acid 0.5g/L, benzene sulfinic acid sodium salt 0.01g/L, be uniformly mixed;
Plating bottle put into by the electroplate liquid that step 6, nickel preplating cubic boron nitride step 4 obtained and step 5 obtain, and by bottled for described plating on rolling electroplating meter, electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor; Described plating bottle surrounding fixes four blocks of magnet, in electronickelling thorn process, produce uniform magnetic field effect;
Step 7, control nickel plating stage initial current are 0.5A; After 24h, electric current is tuned up 2A; After 24h, electric current tunes up 3A; Bath pH values is maintained, pH=4 with the dilution heat of sulfuric acid of 25% in Ni-Speed; Plating bottle rotating speed 10r/min; Nickel plating duration 106h;
Step 8, plating terminate rear to nickel plating thorn cubic boron nitride collect, clean, dry;
The preparation method of embodiment 3:50 μm of nickel plating thorn diamond abrasive grain
Step 1, get diamond (polycrystalline diamond) the abrasive particle 1000ct of granularity 50 μm, add the stannous chloride solution 1L of 1.5g/L, sensitized treatment 40min, cleaning, obtain the diamond of sensitization;
Add the palladium chloride solution 1L of 1.5g/L, activation treatment 40min, cleaning in step 2, the sensitization diamond that obtains in step 1, obtain the diamond of activation;
Add the ortho phosphorous acid sodium solution 1L of 30g/L, reduction treatment 40min, cleaning in step 3, the activation diamond that obtains in step 2, obtain the diamond of reduction;
Step 4, preparation pre-plating solution 4L, in often liter, the concentration of each composition is: single nickel salt 375g/L, Trisodium Citrate 150g/L, sodium acetate 150g/L, inferior sodium phosphate 300g/L;
The diamond of reduction step 3 obtained is poured in pre-plating solution and is stirred, and temperature controls at 60 DEG C, continues plating time 40min, forms nickel preplating diamond;
Step 5, preparation electroplate liquid 1L, the concentration of each composition is: single nickel salt 300g/L, boric acid 30g/L, sodium-chlor 18g/L, aniline sulfonic acid 0.2g/L, benzene sulfinic acid sodium salt 0.2g/L, be uniformly mixed;
Plating bottle put into by the electroplate liquid that step 6, nickel preplating diamond step 4 obtained and step 5 obtain, and by bottled for described plating on rolling electroplating meter, electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor; Described plating bottle surrounding fixes four blocks of magnet, in electronickelling thorn process, produce uniform magnetic field effect;
Step 7, control nickel plating stage initial current be 0.5A after 12h, electric current is tuned up 3A; After 72h, electric current is tuned up 4A; Bath pH values is maintained, pH=5 with the dilution heat of sulfuric acid of 25% in Ni-Speed; Plating bottle rotating speed 12r/min; Nickel plating duration 116h;
Step 8, plating terminate rear to nickel plating thorn diamond collect, clean, dry;
Experimental example 1: electron microscopic examination
Diamond product carries out scanning electronic microscope detection before the nickel plating thorn provided embodiment 1 and after nickel plating thorn:
Specifically see Fig. 1,2, wherein:
Fig. 1 result shows: under microstate, diamond particles regular shape before nickel plating thorn, smooth surface, even particle distribution;
Fig. 2 result shows: after nickel plating thorn, diamond particle surfaces is covered by nickel metal layer, and nickel metal presents a kind of needle-like or bar-shaped, rough degree becomes large, and specific surface area increases, and diamond particle surfaces does not have coating exposed and do not have crystal stock between diamond particles to occur.
Comparative example 1
The experimental technique of product of the present invention 15 μm of nickel plating thorn diamond abrasive grains:
Step 1-4 operation is with embodiment 1;
Step 5, preparation electroplate liquid 1L, in often liter, the concentration of each composition is: single nickel salt 200g/L, boric acid 30g/L, sodium-chlor 18g/L, sodium lauryl sulphate 0.5g/L, be uniformly mixed;
Plating bottle put into by the electroplate liquid that step 6, nickel preplating diamond step 4 obtained and step 5 obtain, and by bottled for described plating on rolling electroplating meter, electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor; Set instrument parameter;
Step 7, control nickel plating stage initial current are 0.5A; After 24h, electric current is tuned up 2A; Bath pH values is maintained, pH=3 with the dilution heat of sulfuric acid of 25% in Ni-Speed; Plating bottle rotating speed 4r/min; Nickel plating duration 120h;
Step 8, plating terminate rear to nickel plating thorn diamond collect, clean, dry;
Experimental result (see Fig. 3): the crystal stock phenomenon between nickel plating diamond particles is obvious; On nickel plating diamond particles, nickel thorn shape is not obvious, and smooth on some diamond surfaces do not have nickel to sting.
Comparative example 2
The experimental technique of product of the present invention 15 μm of nickel plating thorn cubic boron nitride abrasive grains:
Step 1-4 operation is with embodiment 1;
Step 5, preparation electroplate liquid 1L, in often liter, the concentration of each composition is: single nickel salt 200g/L, boric acid 30g/L, sodium-chlor 18g/L, Sodium dodecylbenzene sulfonate 0.5g/L, be uniformly mixed;
Plating bottle put into by the electroplate liquid that step 6, nickel preplating cubic boron nitride step 4 obtained and step 5 obtain, and by bottled for described plating on rolling electroplating meter, electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor; Set instrument parameter;
Step 7, control nickel plating stage initial current are 2A; After 24h, electric current is tuned up 4A; Bath pH values is maintained, pH=3 with the dilution heat of sulfuric acid of 25% in Ni-Speed; Plating bottle rotating speed 12r/min; Nickel plating duration 120h;
Step 8, plating terminate rear to nickel plating thorn cubic boron nitride collect, clean, dry;
Experimental result (see Fig. 4): the crystal stock phenomenon between nickel plating cubic boron nitride particle is obvious; Not exclusively, there is plating leakage phenomenon in cubic boron nitride surface nickel dam parcel; On nickel plating cubic boron nitride particle, nickel thorn shape is not obvious, and some cubic boron nitrides are smooth does not on the surface have nickel to sting.
Although above with general explanation, embodiment and test, the present invention is described in detail, and on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. produce an electroplate liquid for nickel plating thorn abrasive particle, it is the aqueous solution containing following composition: single nickel salt, boric acid, sodium-chlor, aniline sulfonic acid and benzene sulfinic acid sodium salt.
2. electroplate liquid according to claim 1, it is characterized in that, single nickel salt, the boric acid of 7-50g, the sodium-chlor of 5-25g, the aniline sulfonic acid of 0.01-0.5g, the benzene sulfinic acid sodium salt of 0.01-0.5g containing following composition: 50-300g in often liter of described electroplate liquid.
3. electroplate liquid according to claim 2, it is characterized in that, single nickel salt, the boric acid of 25-30g, the sodium-chlor of 18-20g, the aniline sulfonic acid of 0.01-0.5g, the benzene sulfinic acid sodium salt of 0.01-0.5g containing following composition: 200-300g in often liter of described electroplate liquid.
4. electroplate liquid according to claim 3, it is characterized in that, single nickel salt, the boric acid of 25-30g, the sodium-chlor of 18-20g, the aniline sulfonic acid of 0.1-0.5g, the benzene sulfinic acid sodium salt of 0.1-0.5g containing following composition: 200-300g in often liter of described electroplate liquid.
5. electroplate liquid according to claim 4, is characterized in that, single nickel salt, the boric acid of 30g, the sodium-chlor of 18g, the aniline sulfonic acid of 0.2g, the benzene sulfinic acid sodium salt of 0.2g containing following composition: 300g in often liter of described electroplate liquid.
6. a nickel plating thorn abrasive particle, it is characterized in that, it is prepared by following methods:
Step 1, get abrasive particle raw material 1000ct, add the stannous chloride solution 0.5-2L of 0.5-2g/L, sensitized treatment 10-40min, cleaning, obtain sensitization abrasive particle;
Add the palladium chloride solution 0.5-2L of 0.5-2g/L in step 2, the sensitization abrasive particle that obtains in step 1, activation treatment 10-40min, cleaning, obtains activation abrasive particle;
Add the ortho phosphorous acid sodium solution 0.5-2L of 10-50g/L in step 3, the activation abrasive particle that obtains in step 2, reduction treatment 10-40min, cleaning, obtains reduction abrasive particle;
Step 4, preparation 4L pre-plating solution, in often liter of pre-plating solution, the concentration of each component is: the single nickel salt of 25-375g/L, the citric acid of 10-150g/L are received, the sodium acetate of 10-150g/L, the inferior sodium phosphate of 20-300g/L, reduction abrasive particle step 3 obtained is poured in pre-plating solution and is stirred, temperature controls at 50-90 DEG C, continue plating time 20-60min, form nickel preplating abrasive particle;
Step 5, preparation 1L electroplate liquid, the proportioning of each composition, for described in any one of claim 1-5, mixes;
Step 6, nickel preplating abrasive particle step 4 obtained put into plating bottle, by bottled for described plating on rolling electroplating meter, add the electroplate liquid prepared in step 5; Electroplating meter anode is the nickel plate of 99.99%, and negative electrode is copper conductor;
Step 7, control nickel plating stage initial current are 0.5-2A; After 2-30h, electric current is tuned up 2A-3A; After 10-72h, electric current is tuned up 3-4A; Plating bottle rotating speed controls at 5-16r/min, and suitably adjusts according to current density change; Maintain bath pH values with the dilution heat of sulfuric acid of 25% in Ni-Speed, described pH value controls between 2 and 6; Nickel plating continued propagation 20-120h;
Step 8, plating terminate rear to nickel plating thorn abrasive particle collect, clean, dry, detect.
7. abrasive particle according to claim 6, is characterized in that, described abrasive particle raw material comprises diamond and/or cubic boron nitride, described diamond be preferably in single-crystal diamond, polycrystalline diamond one or both.
8. abrasive particle according to claim 6, is characterized in that, described abrasive particle raw material granularity is tested at laser particle analyzer, D50 >=10 μm.
9. abrasive particle according to claim 6, is characterized in that, has also carried out following setting: described plating bottle is fixed with magnet, magnet number >=2 piece, in electronickelling thorn process, produces uniform magnetic field effect plating bottle.
10. the abrasive particle according to any one of claim 6-9, is characterized in that, its surface has a large amount of nickel thorn, described nickel thorn to present form be major axis is 2:1-10:1 needle prick shape with the ratio of minor axis; Described nickel plating thorn abrasive particle improves 50%-200% with the cohesive force of resinoid bond than common plating nickel gold hard rock, nickel plating rate of body weight gain >=30% of nickel plating thorn abrasive particle.
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Cited By (7)
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| CN105904351A (en) * | 2016-04-25 | 2016-08-31 | 珠海大象磨料磨具有限公司 | Diamond brushed piece and preparation method thereof |
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| CN113848151A (en) * | 2021-09-24 | 2021-12-28 | 长沙岱勒新材料科技股份有限公司 | Method for detecting weight gain ratio of electroplated diamond |
| CN116005157A (en) * | 2022-12-13 | 2023-04-25 | 苏州圆格电子有限公司 | Neodymium iron boron surface pretreatment method and system |
| CN116005157B (en) * | 2022-12-13 | 2023-12-19 | 苏州圆格电子有限公司 | Neodymium iron boron surface pretreatment method and system |
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