CN109576687A - A kind of formula and technique of diadust chemical nickel plating - Google Patents
A kind of formula and technique of diadust chemical nickel plating Download PDFInfo
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- CN109576687A CN109576687A CN201910052823.1A CN201910052823A CN109576687A CN 109576687 A CN109576687 A CN 109576687A CN 201910052823 A CN201910052823 A CN 201910052823A CN 109576687 A CN109576687 A CN 109576687A
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- diadust
- nickel plating
- chemical nickel
- ammonium hydroxide
- citric acid
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000007747 plating Methods 0.000 title claims abstract description 96
- 239000000126 substance Substances 0.000 title claims abstract description 60
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 126
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 47
- 239000001509 sodium citrate Substances 0.000 claims abstract description 35
- 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 abstract description 35
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 32
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000001230 potassium iodate Substances 0.000 claims abstract description 13
- 229940093930 potassium iodate Drugs 0.000 claims abstract description 13
- 235000006666 potassium iodate Nutrition 0.000 claims abstract description 13
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims abstract description 12
- 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 abstract description 9
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims abstract description 9
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 9
- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000010432 diamond Substances 0.000 claims description 28
- 229910003460 diamond Inorganic materials 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 206010070834 Sensitisation Diseases 0.000 claims description 3
- 230000008313 sensitization Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 claims 3
- 230000013016 learning Effects 0.000 claims 1
- 239000001488 sodium phosphate Substances 0.000 claims 1
- 229910000162 sodium phosphate Inorganic materials 0.000 claims 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims 1
- 239000008139 complexing agent Substances 0.000 abstract description 19
- 239000011248 coating agent Substances 0.000 abstract description 15
- 238000000576 coating method Methods 0.000 abstract description 15
- 230000008021 deposition Effects 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 13
- 239000003795 chemical substances by application Substances 0.000 abstract description 7
- 230000001965 increasing effect Effects 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000008236 heating water Substances 0.000 abstract description 2
- 235000019786 weight gain Nutrition 0.000 description 28
- 230000037396 body weight Effects 0.000 description 18
- 239000002270 dispersing agent Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000003381 stabilizer Substances 0.000 description 12
- 230000004584 weight gain Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 235000005979 Citrus limon Nutrition 0.000 description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 239000003446 ligand Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 244000248349 Citrus limon Species 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 244000131522 Citrus pyriformis Species 0.000 description 2
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910021205 NaH2PO2 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation 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
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- 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)
- Chemically Coating (AREA)
Abstract
The invention discloses the formulas and technique of a kind of diadust chemical nickel plating, form as follows: nickel sulfate hexahydrate 20-30g/L, sodium hypophosphite 30-35g/L, citric acid 15-25g/L, ammonium hydroxide 12.5-22.5g/L, sodium citrate 12.5-17.5g/L, thiocarbamide 1-5mg/L, Potassiumiodate 2-10mg/L, Macrogol 4000 0.1-1.5g/L, dodecyl benzene sulfonic acid 0.1-1.5g/L.The diadust that useful load is 2~10g is placed in 400mL plating solution, carries out chemical nickel plating under 75~90 DEG C of heating water baths and 120r/min mixing speed after ultrasonic disperse 5min.The present invention increases citric acid and ammonium hydroxide on the basis of sodium citrate, the coating resistance to corrosion that the more single complexing agent of compound complex agent obtains is strong, fills the gap of single complex compound using compound complex agent, structure is even closer, complex compound just becomes stable, and deposition velocity is increased.
Description
Technical field
The invention belongs to diadust field of surface treatment, more particularly to matching for diadust chemical nickel plating
Side and process.
Background technique
With the rapid development of semiconductor information technology and photovoltaic technology, to the valuable hard brittle material such as monocrystalline silicon, jewel
Cutting processing requires increasingly precision, and the joint-cutting of diamond fretsaw processing is narrow, thickness is uniform, angularity is lower, and application is got over
Come more extensive.Diadust has hardness high, and wear-resistant, corrosion resistant excellent performance can be fabricated to cutting, grinding, probing
Equal diamond tools；Meanwhile it is there is also oxidizable, graphitization is heated, with the height between most metals, alloy, bonding agent
The shortcomings that interface energy, loss easy to fall off in actual use causes the service life of diamond tool short, processing efficiency
It is low.Domestic and international researcher is surface-treated diadust using various methods for a long time, with improve itself and matrix it
Between binding force, and chemical plating is widely used due to easy to operate, at low cost.It can be in Buddha's warrior attendant using the method for chemical plating
One layer of metallic film of stone particle surface plating enhances itself and matrix to reduce the thermal damage under hot environment to diamond particles
Between binding force, reduce diamond drop-off prolong to improve the utilization rate of diamond particles and the processing efficiency of diamond tool
The service life of its long product.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides the formula and technique of a kind of diadust chemical nickel plating
Method.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of formula of diadust chemical nickel plating forms as follows: nickel sulfate hexahydrate 20-30g/L, sodium hypophosphite
30-35g/L, citric acid 15-25g/L, ammonium hydroxide 12.5-22.5g/L, sodium citrate 12.5-17.5g/L, thiocarbamide 1-5mg/L, iodine
Sour potassium 2-10mg/L, Macrogol 4000 0.1-1.5g/L, dodecyl benzene sulfonic acid 0.1-1.5g/L.
The formula of the diadust chemical nickel plating forms as follows: nickel sulfate hexahydrate 25g/L, sodium hypophosphite
33g/L, citric acid 20g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L, Potassiumiodate 8mg/L, poly- second two
4000 1g/L of alcohol, dodecyl benzene sulfonic acid 1g/L.
The formula of the diadust chemical nickel plating forms as follows: nickel sulfate hexahydrate 25g/L, sodium hypophosphite
33g/L, citric acid 20g/L, ammonium hydroxide 12.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L, Potassiumiodate 8mg/L, poly- second two
4000 1g/L of alcohol, dodecyl benzene sulfonic acid 1g/L.
The formula of the diadust chemical nickel plating forms as follows: nickel sulfate hexahydrate 25g/L, sodium hypophosphite
33g/L, citric acid 25g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L, Potassiumiodate 8mg/L, poly- second two
4000 1g/L of alcohol, dodecyl benzene sulfonic acid 1g/L.
The technique that diadust chemical nickel plating is carried out using the formula, steps are as follows: being 2~10g by useful load
Diadust be placed in 400mL plating solution, after ultrasonic disperse 5min 75~90 DEG C of heating water baths and 120r/min stirring speed
Degree is lower to carry out chemical nickel plating.
The useful load of the diamond is 6g.
The water bath heating temperature when chemical nickel plating is 80~85 DEG C.
Pre-treatment is carried out before the diadust chemical nickel plating.
The process of the diadust pre-treatment is as follows: oil removing → washing → hydrophiling → washing → sensitization → washing →
Activation → washing.
Beneficial effects of the present invention: sodium citrate is added in the plating solution as complexing agent, can control for the free of reaction
The concentration of nickel ion increases bath stability, improves deposition velocity, and the present invention increases citric acid on the basis of sodium citrate
And ammonium hydroxide, the coating resistance to corrosion that the more single complexing agent of compound complex agent obtains is strong, and the present invention uses ternary built complexing agent, shape
It is that ternary complexes provide possibility at mixed ligand, due to the similar and same metal ion of the hardness of similar ligand
The stability constant for the single complex compound being respectively formed is close, therefore, is added in same solution, their competitiveness is suitable, easy shape
At stable ternary complexes.Once being formed, its stability is formed by ternary complexes than cognate ligand and metal ion
Binary complex stability is big, because the first ligand of ternary complexes is usually the multidentate ligand of macromolecular, it and metal
The chelate that ion is formed by has certain space structure, and the remaining co-ordination positions of metal ion will be accounted for by the second ligand
With the gap of originally complex compound is filled, and structure is even closer, and complex compound just becomes stable, to improve the densification of coating
Degree and resistance to corrosion.
Stabilizer is added in the plating solution can stablize plating solution, improve plating speed, and it is existing that addition dispersing agent can improve particle agglomeration
As sodium citrate is basis, and weight gain can be reduced by removing sodium citrate；Citric acid and ammonium hydroxide are for adjusting pH, and pH value is 4 left
Right available close coating；Using compound complex agent, the advantages of can not only integrating single complexing agent, exempt its defect, and
Play its advantage more preferable.Stable ternary complexes can be formed using compound complex agent, obtain the gap of single complex compound
Filling, structure is even closer, and complex compound just becomes stable, and deposition velocity is increased.So the optimal proportion of complexing agent is
Citric acid 25g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L.
Detailed description of the invention
The SEM image (12000 ×) of plating diamond when Fig. 1 is different citric acid contents, a, b, c are respectively that citric acid contains
The SEM image of plating diamond when measuring 15g/L, 20g/L, 25g/L.
Fig. 2 is influence of the citric acid content to chemical plating rate of body weight gain.
Fig. 3 is the relationship of ammonium hydroxide content and deposition rate.
Fig. 4 is the relationship of ammonium hydroxide content and rate of body weight gain.
The SEM image (12000 ×) of plating diamond when Fig. 5 is different ammonium hydroxide contents, a, b are respectively ammonium hydroxide content
SEM image when 12.5mL/L, 22.5mL/L.
Fig. 6 is the SEM image (3000 ×) for the plating diamond for being not added with dispersing agent and adding dispersing agent, and a, b are respectively
SEM image when polyethylene glycol and sodium dodecyl benzene sulfonate content are 0g/L, 1g/L.
Fig. 7 is the relationship of diamond useful load and rate of body weight gain.
Nickel slag is generated when Fig. 8 diamond useful load 2g.
There is plating leakage when Fig. 9 diamond useful load 8g.
Figure 10 is the relationship of temperature and rate of body weight gain.
Specific embodiment
Combined with specific embodiments below, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The person skilled in the art of the range of invention and is not intended to limit the present invention, the field can make one according to the content of foregoing invention
A little nonessential modifications and adaptations.
Embodiment 1
The formula of the present embodiment diadust chemical nickel plating forms as follows: nickel sulfate hexahydrate 25g/L, sodium hypophosphite
33g/L, citric acid 20g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L, Potassiumiodate 8mg/L, poly- second two
4000 1g/L of alcohol, dodecyl benzene sulfonic acid 1g/L.
The technique that diadust chemical nickel plating is carried out using above-mentioned formula, steps are as follows: diadust pre-treatment
Process is as follows: oil removing → washing → hydrophiling → washing → sensitization → washing → activation → washing.
The diadust that useful load is 6g is placed in 400mL plating solution, in 80~85 DEG C of water-baths after ultrasonic disperse 5min
Chemical nickel plating is carried out under heating and 120r/min mixing speed.
Embodiment 2
The formula of the diadust chemical nickel plating of the present embodiment forms as follows: nickel sulfate hexahydrate 25g/L, ortho phosphorous acid
Sodium 33g/L, citric acid 20g/L, ammonium hydroxide 12.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L, Potassiumiodate 8mg/L, poly- second
4000 1g/L of glycol, dodecyl benzene sulfonic acid 1g/L.
Embodiment 3
The formula of the diadust chemical nickel plating of the present embodiment forms as follows: nickel sulfate hexahydrate 25g/L, ortho phosphorous acid
Sodium 33g/L, citric acid 25g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L, Potassiumiodate 8mg/L, poly- second
4000 1g/L of glycol, dodecyl benzene sulfonic acid 1g/L.
Comparative example 1
The citric acid 25g/L, ammonium hydroxide 0g/L, sodium citrate 0g/L of the present embodiment, remaining formula is the same as embodiment 3.
Comparative example 2
The citric acid 0g/L, ammonium hydroxide 17.5g/L, ammonium hydroxide 0g/L of the present embodiment, remaining formula is the same as embodiment 3.
Comparative example 3
The citric acid 0g/L, ammonium hydroxide 0g/L, sodium citrate 12.5g/L of the present embodiment, remaining formula is the same as embodiment 3.
Comparative example 4
The citric acid 0g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L of the present embodiment, remaining formula is the same as embodiment 3.
Comparative example 5
The citric acid 25g/L, ammonium hydroxide 0g/L, sodium citrate 12.5g/L of the present embodiment, remaining formula is the same as embodiment 3.
Comparative example 6
The citric acid 25g/L, ammonium hydroxide 17.5g/L, sodium citrate 0g/L of the present embodiment, remaining formula is the same as embodiment 3.
Comparative example 1-6 experimental result is as follows
1, influence of the complexing agent content to chemical plating result
Sodium citrate is added in the plating solution as complexing agent, can control the concentration of the free nickel ion for reaction, increase
Bath stability improves deposition velocity, and the coating resistance to corrosion that the more single complexing agent of compound complex agent obtains is strong, so in lemon
Citric acid and ammonium hydroxide are increased on the basis of lemon acid sodium, complexing agent in solution (citric acid, citric acid are probed into using orthogonal experiment
Sodium, ammonium hydroxide) to chemical plating weight gain influence, the results are shown in Table 1.
Orthogonal test table of 1 complexing agent content of table to chemical plating increase heavy influence result
By 1 range analysis of table it is found that complexing agent content sorts to the primary and secondary of chemical plating increase heavy influence are as follows: citric acid > ammonium hydroxide >
Sodium citrate, the optimal proportion of weight gain are as follows: citric acid 20g/L, sodium citrate 12.5g/L, ammonium hydroxide 17.5mL/L, this proportion are filling
The weight gain obtained when carrying capacity is 6g is 1.008g, more maximum more than No. 3 than increasing weight in orthogonal test, thus the proportion be weight gain most
Excellent proportion.
1) influence of the citric acid content to chemical plating result
On the basis of complexing agent optimal proportion, change citric acid content (15~25g/L), gained plating outcome such as Fig. 1 and
Shown in Fig. 2.
As shown in Figure 1, as citric acid content increases, the nickel crystallite of diamond particle surfaces deposition first becomes larger to become smaller afterwards,
And in 20g/L, nickel crystallite is maximum, nickel crystallite is minimum when 25g/L (bath pH value 4) and plated layer compact, cause in Fig. 2 with
Citric acid content increases, and weight gain takes the lead in becoming smaller after becoming larger, and the rate of body weight gain highest in 20g/L.When citric acid content is lower than 20g/L
When, content increases smaller on the influence of chemical plating rate of body weight gain；When its content is higher than 20g/L, solution acidification aggravation, H2PO2 -'s
Reproducibility weakens, and chemomotive force reduces, and the fluctuation of plating speed is small during chemical plating, and uniform cause can be obtained while causing rate of body weight gain to decline
Coating close, plating leakage is few.So citric acid concentration should be chosen at 20g/L from rate of body weight gain；In terms of plated layer compact situation, lemon
Lemon acid concentration should be chosen at 25g/L；And chemical plating rate of body weight gain is related with size of nickel crystallite.
2) influence of the ammonium hydroxide content to chemical plating result
The palladium for being attached to diamond particle surfaces plays catalytic action in plating process, and the position for having palladium to depend on first generates
Nickel layer, and subsequent fill up is not carried out by chemomotive force by the surface that palladium depends on.It is different that chemomotive force difference will lead to coating stress
The result of sample, chemical plating is just different.The cause for influencing diadust surface chemical plating result is known as complexing agent, and stabilizer disperses
Agent, useful load, temperature etc., these factors affect chemomotive force and deposition rate.Relationship is available between deposition rate r and each factor
Following formula indicates:
R=k0[NiSO4·6H2O]a[NaH2PO2·H2O]b[C6H8O7·H2O]c[NH3·H2O]d[C6H5Na3O7·2H2O]e
[stabilizer]f[dispersing agent]gexp(-Ea/RT)
Wherein, a~g is kinetic parameter corresponding to each factor, and Ea is the apparent activation energy of electroless nickel deposition reaction.
Above formula both sides take logarithm, arrange the relationship that can be obtained in plating solution between ammonium hydroxide content and deposition rate are as follows:
Wherein p indicates that other than the substance withdrawl syndrome of ammonium hydroxide is as variable, remaining variables remain unchanged, and ammonium hydroxide substance
Amount concentration and deposition rate between logarithmic relationship curve be straight line (as shown in Figure 4), straight slope be kinetic parameter d value.
On the basis of complexing agent optimal proportion, change ammonium hydroxide content (12.5~22.5g/L), gained plating outcome such as Fig. 5
With shown in Fig. 6.As shown in Figure 5, as ammonium hydroxide content increases, rate of body weight gain increases.On the one hand, as shown in Figure 4, with ammonium hydroxide substance
Amount concentration increase, deposition rate improves, and weight gain in same time is caused to become more；On the other hand, it will be appreciated from fig. 6 that with ammonium hydroxide
Content increases, and nickel crystallite becomes larger, and uneven coating is even, plating leakage, and reaction is not easy to control, and ammonium hydroxide content is 12.5mL/L (plating solution pH
Value for 4) when coating is uniform, plating leakage is few；Further, since ammonium hydroxide increases, pH value of solution becomes larger, H2PO2 -Reproducibility enhancing, chemistry is dynamic
Power increases, and rate of body weight gain is caused to rise always.So ammonia concn should be chosen at 22.5mL/L from rate of body weight gain；It is caused from coating
Close situation sees that ammonia concn should be chosen at 12.5mL/L.
3) influence that the content of sodium citrate increases weight to chemical plating
By orthogonal result it is found that the content of sodium citrate has certain influence to chemical plating weight gain, increase weight after removing sodium citrate
For 0.653g, 1.008g when compared with optimal proportion is few.
PH value available close coating when being 4.It can be seen from the above, there are two the formulas that pH value is 4: a: citric acid 25g/
L, sodium citrate 12.5g/L, ammonium hydroxide 17.5mL/L；B: citric acid 20g/L, sodium citrate 12.5g/L, ammonium hydroxide 12.5mL/L, but a
The weight gain of formula is formulated greater than b, so comprehensively considering, the optimal proportion of complexing agent is citric acid 25g/L, ammonium hydroxide 17.5g/L, lemon
Lemon acid sodium 12.5g/L.
2, the influence of stabilizer and dispersant to chemical plating result
Stabilizer is added in the plating solution can stablize plating solution, improve plating speed, and it is existing that addition dispersing agent can improve particle agglomeration
As being formulated based on complexing agent optimal proportion, thiocarbamide and Potassiumiodate are as stabilizer, Macrogol 4000 and detergent alkylate
Sodium sulfonate probes into the influence of stabilizer and dispersant to chemical plating result, the results are shown in Table 2 as dispersing agent.
The influence of 2 stabilizer of table and dispersant to chemical plating result
As shown in Table 2, when not adding thiocarbamide and Potassiumiodate as stabilizer, there is nickel slag raw in solution after reaction
At, and when additive amount is excessive, can inhibit reaction to carry out, if increasing the amount of dispersing agent at this time, nonreactive solution can be made normally to occur
Reaction.The addition of dispersing agent can improve crystal stock phenomenon, as shown in fig. 7, but additional amount is excessive will lead to foam mistake in reaction process
It is more, cause diamond and part solution to overflow beaker and waste.The optimum content of experimental study resulting stabilizer and dispersing agent
Are as follows: thiocarbamide content should be 1.4mg/L, and acid iodide potassium content is 8mg/L, polyethyleneglycol content 1g/L, neopelex
Content is 1g/L.
3, influence of the process conditions to diadust chemical plating result
The process conditions for influencing diadust chemical plating result have useful load, temperature, ultrasound, repeatedly plating etc., beg for below
Influence by useful load and temperature to diadust chemical plating result.
1) influence of the useful load to chemical plating result
Plating solution used in chemical plating is 400mL, and diamond useful load is 2~10g, probes into diamond useful load to plating outcome
Influence (as shown in FIG. 8 and 9).
As shown in Figure 8, as diamond useful load becomes larger, rate of body weight gain is reduced.This is because the useful load when diamond is
When < 6g, the total surface area of the diamond as matrix is small, and the chemomotive force for acting on unit area increases, and cannot carry completely
The nickel simple substance restored in solution, leads to the generation of nickel slag, causes rate of body weight gain virtual height, and crystal stock is serious；And when diamond loads
When measuring > 6g, the chemomotive force for acting on unit area is reduced by dispersion, leads to plating leakage, and rate of body weight gain is caused to reduce.So dress
Carrying capacity is preferably 6g.
2) influence of the temperature to chemical plating result
As shown in Figure 10, as temperature increases, rate of body weight gain becomes larger.This is because when 80 DEG C of temperature <, ion activity and
Diffusion velocity is small, and chemomotive force is insufficient, and the deposition velocity of nickel is small, and reaction is slow not to react even, is hardly formed coating；As temperature >
At 85 DEG C, the nickel ion dissociation of complexing is fast, and chemomotive force increases, and the deposition velocity of nickel becomes faster, but the reunion of particle tends at this time
Greatly, coating is loose, and plating solution is unstable, and reaction is not easy to control.So temperature should be chosen at 80~85 DEG C, in this temperature range
It can get crystal stock and lack the few plating diamond of plating leakage.
(1) complexing agent sorts to the primary and secondary of chemical plating increase heavy influence are as follows: citric acid > ammonium hydroxide > sodium citrate increases weight optimal match
Than are as follows: citric acid 20g/L, sodium citrate 12.5g/L, ammonium hydroxide 17.5mL/L, weight gain, and plating solution pH can be reduced by removing sodium citrate
When being 4 or so, plating leakage can be obtained and lack the few plating diamond of crystal stock；Comprehensively consider, the optimal proportion of complexing agent is citric acid
25g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L.
(2) when not adding stabilizer in solution, the generation of nickel slag is had, and additive amount can excessively inhibit reaction to carry out,
If increasing the amount of dispersing agent at this time, nonreactive solution can be made normally to react；Stabilizer and dispersing agent optimum content are as follows:
Thiocarbamide content should be 1.4mg/L, and acid iodide potassium content is 8mg/L, polyethyleneglycol content 1g/L, sodium dodecyl benzene sulfonate content
For 1g/L.
(3) as diamond useful load becomes larger, rate of body weight gain is reduced；Useful load has the generation of nickel slag, useful load when being < 6g
Plating leakage is had when > 6g, so useful load is preferably 6g.
(4) as temperature increases, rate of body weight gain becomes larger；When 80 DEG C of temperature <, reaction is slow, is hardly formed coating；Work as temperature
At 85 DEG C of >, coating is loose, and plating solution is unstable.So the optimum range of temperature is 80~85 DEG C.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (9)
1. a kind of formula of diadust chemical nickel plating, it is characterised in that composition is as follows: nickel sulfate hexahydrate 20-30g/L, secondary Asia
Sodium phosphate 30-35g/L, citric acid 15-25g/L, ammonium hydroxide 12.5-22.5g/L, sodium citrate 12.5-17.5g/L, thiocarbamide 1-
5mg/L, Potassiumiodate 2-10mg/L, Macrogol 4000 0.1-1.5g/L, dodecyl benzene sulfonic acid 0.1-1.5g/L.
2. the formula of diadust chemical nickel plating according to claim 1, it is characterised in that composition is as follows: six water sulfuric acid
Nickel 25g/L, sodium hypophosphite 33g/L, citric acid 20g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L,
Potassiumiodate 8mg/L, Macrogol 4000 1g/L, dodecyl benzene sulfonic acid 1g/L.
3. the formula of diadust chemical nickel plating according to claim 1, it is characterised in that composition is as follows: six water sulfuric acid
Nickel 25g/L, sodium hypophosphite 33g/L, citric acid 20g/L, ammonium hydroxide 12.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L,
Potassiumiodate 8mg/L, Macrogol 4000 1g/L, dodecyl benzene sulfonic acid 1g/L.
4. the formula of diadust chemical nickel plating according to claim 1, it is characterised in that composition is as follows: six water sulfuric acid
Nickel 25g/L, sodium hypophosphite 33g/L, citric acid 25g/L, ammonium hydroxide 17.5g/L, sodium citrate 12.5g/L, thiocarbamide 1.4mg/L,
Potassiumiodate 8mg/L, Macrogol 4000 1g/L, dodecyl benzene sulfonic acid 1g/L.
5. the technique for carrying out diadust chemical nickel plating using any formula of claim 1-4, it is characterised in that step
It is rapid as follows: the diadust that useful load is 2~10g to be placed in 400mL plating solution, in 75~90 DEG C of water after ultrasonic disperse 5min
Chemical nickel plating is carried out under bath heating and 120r/min mixing speed.
6. the technique of diadust chemical nickel plating according to claim 5, it is characterised in that: the loading of the diamond
Amount is 6g.
7. the technique of diadust chemical nickel plating according to claim 5, it is characterised in that: when the chemical nickel plating
Water bath heating temperature is 80~85 DEG C.
8. the technique of diadust chemical nickel plating according to claim 5, it is characterised in that: the diadust
Pre-treatment is carried out before learning nickel plating.
9. the technique of diadust chemical nickel plating according to claim 5, it is characterised in that: before the diadust
The process of processing is as follows: oil removing → washing → hydrophiling → washing → sensitization → washing → activation → washing.
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