CN108930031A - A kind of preparation method of diamond surface Electroless Ni-W-P coating - Google Patents
A kind of preparation method of diamond surface Electroless Ni-W-P coating Download PDFInfo
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- CN108930031A CN108930031A CN201810825665.4A CN201810825665A CN108930031A CN 108930031 A CN108930031 A CN 108930031A CN 201810825665 A CN201810825665 A CN 201810825665A CN 108930031 A CN108930031 A CN 108930031A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1889—Multistep pretreatment with use of metal first
Abstract
The invention discloses a kind of preparation methods of diamond surface Electroless Ni-W-P coating, the preparation method passes through in diamond particle surfaces coated graphite alkene layer, after graphene layer oxidation a large amount of oxygen-containing groups can be formed in diamond surface, the oxygen-containing functional group can effectively adsorb palladium active particles, and as complexant during plating, be conducive to Ni-W Base Metal effectively to deposit in diamond surface, finally obtain with good quality and combine fine and close uniform Ni-W-P coating with diamond.
Description
Technical field
The present invention relates to electroless plating technology field more particularly to a kind of preparations of diamond surface Electroless Ni-W-P coating
Method.
Background technique
Diamond itself also has excellent optics, sound in addition to the excellent properties such as high, anticorrosive, wearability with hardness
The properties such as, calorifics and electricity.Since over half a century, the production of diamond and the development of application technology are advanced by leaps and bounds,
It has reached in quantity, quality and many performances and has been even more than natural diamond.Diamond and its product are not only answered extensively
For mechanical, metallurgy, each industrial technical field such as build work, traffic, national defence, it is extended to high performance heat-resistant piece, anti-corrosion
The key areas such as part, heat conducting element and chip.Superhard material based on diamond etc. has become the basic of Modern Manufacturing Technology
Means play support and facilitation to state-owned pillar industry and national defense industry.It is counted according to external authoritative sources, world's diamond
Demand be just incremented by with average 8% or so annual growth rate, carbonado 50% or so is for manufacturing processing of stone at present
Tool.It is contemplated that the material progress of the mankind will attain a yet higher goal, or even peak after diamond product is universal, into
Enter the eternal diamond epoch.
Currently, the interface between diamond and basis material is generally reduced using the method for surface metallization both at home and abroad
Can, the infiltration of diamond and various metals material is realized, so that the bond strength of diamond and matrix is improved, in favor of sufficiently sending out
Wave the performance of diamond.Diamond surface coating technology is divided into chemical method (such as chemical plating and plating, chemical vapor deposition), object
Logos (the micro- vapor deposition of such as magnetron sputtering, physical vapour deposition (PVD), vacuum, powder covering sintering) and salt bath process.In these methods, chemistry
The method of plating have it is easily operated, it is at low cost, can mass production, the low advantage of plating temperature, and can be in the micro- of any shape
Plating is carried out on powder, overcomes other methods because of the non-uniform phenomenon of clad caused by granule-morphology, thus it is answered extensively
For plating Ni, Co, Cu and its alloy etc..
Electroless Plating Ni diamond amount accounts for about the half of entire plating diamond amount, and market capacity is considerable, is simultaneously
Increase Ni coating performance (such as wearability, corrosion resistance and solderability), usually during plating Ni Composite Coatings P, Electroless Plating Ni-
One of the reason of P alloying technology is widely used is that its coating has excellent corrosion resisting property, with the development of society, certain applications
Field can hardness to Ni coating and corrosion resistance have higher requirement, chemical Ni-P plating will not be able to satisfy at this time.At this moment, chemical
In plating Ni-W-P coating, the co-deposition of W changes Coating, so that its thermal stability and corrosion resistance are plated compared to Ni-P
Layer has comparable promotion, and either under plated state or after Overheating Treatment, the binding force of Ni-W-P coating is all higher than Ni-
P coating, therefore Ni-W-P coating possesses higher hardness and more excellent corrosion resistance, can in harsher corrosive environment,
It is used as protective coating, especially in acidic environment to protect matrix from corrosion.
And existing various diamond surface plating Ni-W-P techniques are still undesirable, such as there is Plating times length, coating surface
The problems such as pattern is not smooth enough, coating became uneven and coating and diamond interface bond strength are inadequate, there is room for improvement,
So improving existing plating Ni-W-P technique, developing more advanced plating Ni-W-P technique seems significant.
Summary of the invention
The problem of based on background technique, the invention proposes a kind of diamond surface Electroless Ni-W-P coatings
Preparation method, the preparation method is by the way that in diamond particle surfaces coated graphite alkene layer, which can be in gold after aoxidizing
Hard rock surface forms a large amount of oxygen-containing groups, which can effectively adsorb palladium active particles, and in plating mistake
In journey be used as complexant, be conducive to Ni-W Base Metal and effectively deposited in diamond surface, finally obtain with good quality and and
Diamond combines fine and close uniform Ni-W-P coating.
A kind of preparation method of diamond surface Electroless Ni-W-P coating proposed by the present invention, includes the following steps:
S1, the diadust that partial size is 50-200 μm is added in dilution heat of sulfuric acid, impregnates 1- at 60-80 DEG C
3h, is 20-30 μm of iron powder with partial size after filtering and partial size is that 1-5 μm of nickel powder mixes, in 0.1-1 × 10-3The vacuum condition of Pa
Under be warming up to 1200-1300 DEG C, obtain powder after insulation reaction 1-2h, after removing iron nickel powder superfluous in powder, be put into dilute sulphur
1-3h is impregnated in acid solution, is filtered, and washing after drying, obtains the diadust of surface coated graphite alkene；
S2, it will be mixed in the diadust addition concentrated sulfuric acid solution of coated graphite alkene in surface obtained in S1, in ice water
It is stirred to react 0.3-0.5h after the lower addition potassium permanganate of bath, the hydrogen peroxide that content is 3-6wt% is added and is stirred to react 0.1-
0.3h, filtering, being washed to pH value is 6-7, after drying, obtains the diadust that surface has oxygen-containing functional group；
S3, the surface that S2 is obtained is placed in sensitization-activated water solutions with the diadust of oxygen-containing functional group and is stirred
5-10min distills water washing after filtering, is then added to ortho phosphorous acid sodium water solution stirring 2-4min and carries out dispergation reduction, distillation
It is dried after water washing, obtains the diadust that surface has catalytic activity palladium；
S4, there is the diadust of catalytic activity palladium to be added in chemical plating fluid the surface that S3 is obtained, at 60-80 DEG C
Lower carry out chemical plating, during plating, adjusting bath pH value is 8-10, stirring rate 150-300r/min, Plating times
For 0.5-1h, plating is stood after the completion, is washed, vacuum drying, then be heat-treated 1-5h at 300-500 DEG C, is obtained coating surface
There is the diadust of Ni-W-P coating.
Preferably, in S1, diadust is added in dilution heat of sulfuric acid and is impregnated, further include to after immersion after filtering
Diadust washed, specifically, being first washed with distilled water, then be cleaned by ultrasonic with acetone, then washed with dehydrated alcohol
It washs.
Preferably, in S1, diadust is 2-5:1:1 with the weight ratio of iron powder and nickel powder.
Preferably, in S2, the additional amount of potassium permanganate is the 1- of the diadust of the surface coated graphite alkene
5wt%, the additional amount of hydrogen peroxide are the 1-10wt% of the diadust of the surface coated graphite alkene.
Preferably, in S3, the sensitization-activated water solutions include palladium chloride 0.3-0.6g/L, stannic chloride 1-5g/L, dense salt
Sour 30-50ml/L, sodium chloride 60-80g/L.
Preferably, in S3, the ortho phosphorous acid sodium water solution includes 15-20g/L sodium hypophosphite.
Preferably, in S4, the chemical plating fluid includes: nickel sulfate hexahydrate 8-16g/L, sodium hypophosphite 10-20g/L, tungsten
Sour sodium 1-3g/L, sodium citrate 20-50g/L, lactic acid 5-10mL/L, ammonium sulfate 20-30g/L, saccharin 0.5-1g/L, succinic acid 5-
15g/L, potassium iodide 10-20mg/L.
In a kind of preparation method of diamond surface Electroless Ni-W-P coating proposed by the invention, firstly, by Buddha's warrior attendant
Stone micro mist and iron powder, nickel powder pyroreaction, can be such that diamond is graphitized during the high temperature treatment process, thus in diamond
Surface grows equally distributed multi-layer graphene nanometer layer；Hereafter the diadust of the surface coated graphite alkene is subjected to oxygen
Change, graphene is largely oxidized to oxygen-containing functional group, thus forms a large amount of oxygen-containing groups in diamond surface；When should
When diadust is added in sensitization-activated water solutions, the diadust hydrophilicity which is oxidized is greatly improved,
It can thus be stabilized in the solution, simultaneously because the oxygen-containing group on its surface can be to Pd2+It is effectively adsorbed, lower
In sensitization-activated water solutions of concentration, it can in a large amount of metallic palladium particles of diamond surface deposition reaction, i.e. palladium particle；Most
The diadust with a large amount of catalytic activity palladiums is added in chemical plating fluid afterwards and carries out chemical plating, diadust by
In surface, distribution largely has the palladium particle for having catalytic activity for deposited metal Ni-W, ensure that the Ni-W Base Metal in Buddha's warrior attendant
Effective deposition on stone surface, and the oxygen-containing group that diamond surface has also is also used as complexant, makes the performance of plating solution
It is more stable while metal lining can also effectively be adsorbed, plating solution reaction and coating deposition rate are further speeded up, most
Gained Ni-W-P coating is in conjunction with diadust densification eventually, and coating is thicker, smooth, smooth, uniform, cladding is complete, also
With higher hardness and more excellent corrosion resistance.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of diamond surface Electroless Ni-W-P coating, includes the following steps:
S1, the diadust that partial size is 50 μm is added in dilution heat of sulfuric acid, 1h is impregnated at 80 DEG C, is used after filtering
Water washing is distilled, then is cleaned by ultrasonic with acetone, is then washed with dehydrated alcohol, with partial size is 30 μm of iron powders and partial size after drying
It is uniformly mixed for 1 μm of nickel powder, diadust is 5:1:1 with the weight ratio of iron powder and nickel powder, 0.1 × 10-3The vacuum of Pa
Under the conditions of be warming up to 1300 DEG C, obtain powder after insulation reaction 1h, after removing iron nickel powder superfluous in powder, it is molten to be put into dilute sulfuric acid
3h is impregnated in liquid, is filtered, and washing after drying, obtains the diadust of surface coated graphite alkene；
S2, it will be mixed in the diadust addition concentrated sulfuric acid solution of coated graphite alkene in surface obtained in S1, in ice water
0.3h is stirred to react after the lower addition potassium permanganate of bath, the additional amount of potassium permanganate is that the diamond of the surface coated graphite alkene is micro-
The 5wt% of powder adds the hydrogen peroxide that content is 3wt% and is stirred to react 0.3h, and the additional amount of hydrogen peroxide is surface cladding
The 1wt% of the diadust of graphene, filtering, being washed to pH value is 7, after drying, obtains surface with oxygen-containing functional group
Diadust；
S3, the surface that S2 is obtained is placed in sensitization-activated water solutions with the diadust of oxygen-containing functional group and is stirred
5min, the sensitization-activated water solutions include palladium chloride 0.6g/L, stannic chloride 1g/L, concentrated hydrochloric acid 50ml/L, sodium chloride 60g/L,
Water washing is distilled after filtering, is then added to ortho phosphorous acid sodium water solution stirring 4min and is carried out dispergation reduction, the sodium hypophosphite
Aqueous solution includes 15g/L sodium hypophosphite, is dried after distilling water washing, and it is micro- to obtain diamond of the surface with catalytic activity palladium
Powder；
S4, there is the diadust of catalytic activity palladium to be added in chemical plating fluid the surface that S3 is obtained, the chemistry
Plating solution include: nickel sulfate hexahydrate 16g/L, sodium hypophosphite 10g/L, sodium tungstate 3g/L, sodium citrate 20g/L, lactic acid 10mL/L,
Ammonium sulfate 20g/L, saccharin 1g/L, succinic acid 5g/L, potassium iodide 20mg/L, carry out chemical plating at 60 DEG C, during plating,
Adjusting bath pH value is 10, stirring rate 150r/min, Plating times 1h, is stood after the completion of plating, washing, and vacuum is dry
It is dry, then it is heat-treated 5h at 300 DEG C, obtain the diadust that coating surface has Ni-W-P coating.
Embodiment 2
A kind of preparation method of diamond surface Electroless Ni-W-P coating, includes the following steps:
S1, the diadust that partial size is 200 μm is added in dilution heat of sulfuric acid, 3h is impregnated at 60 DEG C, after filtering
Be washed with distilled water, then be cleaned by ultrasonic with acetone, then washed with dehydrated alcohol, after drying with partial size be 20 μm of iron powders and grain
Diameter is that 5 μm of nickel powders are uniformly mixed, and diadust is 2:1:1 with the weight ratio of iron powder and nickel powder, 1 × 10-3The vacuum of Pa
Under the conditions of be warming up to 1200 DEG C, obtain powder after insulation reaction 2h, after removing iron nickel powder superfluous in powder, it is molten to be put into dilute sulfuric acid
1h is impregnated in liquid, is filtered, and washing after drying, obtains the diadust of surface coated graphite alkene；
S2, it will be mixed in the diadust addition concentrated sulfuric acid solution of coated graphite alkene in surface obtained in S1, in ice water
0.5h is stirred to react after the lower addition potassium permanganate of bath, the additional amount of potassium permanganate is that the diamond of the surface coated graphite alkene is micro-
The 1wt% of powder adds the hydrogen peroxide that content is 6wt% and is stirred to react 0.1h, and the additional amount of hydrogen peroxide is surface cladding
The 10wt% of the diadust of graphene, filtering, being washed to pH value is 6, after drying, obtains surface with oxygen-containing functional group
Diadust；
S3, the surface that S2 is obtained is placed in sensitization-activated water solutions with the diadust of oxygen-containing functional group and is stirred
10min, the sensitization-activated water solutions include palladium chloride 0.3g/L, stannic chloride 5g/L, concentrated hydrochloric acid 30ml/L, sodium chloride 80g/
L distills water washing after filtering, is then added to ortho phosphorous acid sodium water solution stirring 2min and carries out dispergation reduction, the ortho phosphorous acid
Sodium water solution includes 20g/L sodium hypophosphite, is dried after distilling water washing, and it is micro- to obtain diamond of the surface with catalytic activity palladium
Powder；
S4, there is the diadust of catalytic activity palladium to be added in chemical plating fluid the surface that S3 is obtained, the chemistry
Plating solution includes: nickel sulfate hexahydrate 8g/L, sodium hypophosphite 20g/L, sodium tungstate 1g/L, sodium citrate 50g/L, lactic acid 5mL/L, sulphur
Sour ammonium 30g/L, saccharin 0.5g/L, succinic acid 15g/L, potassium iodide 10mg/L carry out chemical plating, plating process at 80 DEG C
In, adjusting bath pH value is 8, stirring rate 300r/min, Plating times 0.5h, is stood after the completion of plating, washing, vacuum
It is dry, then it is heat-treated 1h at 500 DEG C, obtain the diadust that coating surface has Ni-W-P coating.
Embodiment 3
A kind of preparation method of diamond surface Electroless Ni-W-P coating, includes the following steps:
S1, the diadust that partial size is 100 μm is added in dilution heat of sulfuric acid, 2h is impregnated at 70 DEG C, after filtering
Be washed with distilled water, then be cleaned by ultrasonic with acetone, then washed with dehydrated alcohol, after drying with partial size be 25 μm of iron powders and grain
Diameter is that 3 μm of nickel powders are uniformly mixed, and diadust is 3:1:1 with the weight ratio of iron powder and nickel powder, 0.5 × 10-3Pa's is true
It is warming up to 1250 DEG C under empty condition, powder is obtained after insulation reaction 1.5h, after removing iron nickel powder superfluous in powder, is put into dilute sulphur
2h is impregnated in acid solution, is filtered, and washing after drying, obtains the diadust of surface coated graphite alkene；
S2, it will be mixed in the diadust addition concentrated sulfuric acid solution of coated graphite alkene in surface obtained in S1, in ice water
0.4h is stirred to react after the lower addition potassium permanganate of bath, the additional amount of potassium permanganate is that the diamond of the surface coated graphite alkene is micro-
The 3wt% of powder adds the hydrogen peroxide that content is 4wt% and is stirred to react 0.2h, and the additional amount of hydrogen peroxide is surface cladding
The 5wt% of the diadust of graphene, filtering, being washed to pH value is 6, after drying, obtains surface with oxygen-containing functional group
Diadust；
S3, the surface that S2 is obtained is placed in sensitization-activated water solutions with the diadust of oxygen-containing functional group and is stirred
7min, the sensitization-activated water solutions include palladium chloride 0.4g/L, stannic chloride 3g/L, concentrated hydrochloric acid 40ml/L, sodium chloride 70g/L,
Water washing is distilled after filtering, is then added to ortho phosphorous acid sodium water solution stirring 3min and is carried out dispergation reduction, the sodium hypophosphite
Aqueous solution includes 17g/L sodium hypophosphite, is dried after distilling water washing, and it is micro- to obtain diamond of the surface with catalytic activity palladium
Powder；
S4, there is the diadust of catalytic activity palladium to be added in chemical plating fluid the surface that S3 is obtained, the chemistry
Plating solution include: nickel sulfate hexahydrate 12g/L, sodium hypophosphite 15g/L, sodium tungstate 2g/L, sodium citrate 30g/L, lactic acid 7mL/L,
Ammonium sulfate 25g/L, saccharin 0.8g/L, succinic acid 10g/L, potassium iodide 15mg/L carry out chemical plating, plating process at 70 DEG C
In, adjusting bath pH value is 9, stirring rate 200r/min, Plating times 0.7h, is stood after the completion of plating, washing, vacuum
It is dry, then it is heat-treated 3h at 400 DEG C, obtain the diadust that coating surface has Ni-W-P coating.
Embodiment 4
A kind of preparation method of diamond surface Electroless Ni-W-P coating, includes the following steps:
S1, the diadust that partial size is 200 μm is added in dilution heat of sulfuric acid, 1.5h is impregnated at 75 DEG C, filtered
After be washed with distilled water, then be cleaned by ultrasonic with acetone, then washed with dehydrated alcohol, with partial size be after drying 25 μm of iron powders and
Partial size is that 2 μm of nickel powders are uniformly mixed, and diadust is 3:1:1 with the weight ratio of iron powder and nickel powder, 0.6 × 10-3Pa's
It is warming up to 1250 DEG C under vacuum condition, powder is obtained after insulation reaction 2h, after removing iron nickel powder superfluous in powder, is put into dilute sulphur
1.2h is impregnated in acid solution, is filtered, and washing after drying, obtains the diadust of surface coated graphite alkene；
S2, it will be mixed in the diadust addition concentrated sulfuric acid solution of coated graphite alkene in surface obtained in S1, in ice water
0.3h is stirred to react after the lower addition potassium permanganate of bath, the additional amount of potassium permanganate is that the diamond of the surface coated graphite alkene is micro-
The 3wt% of powder adds the hydrogen peroxide that content is 4wt% and is stirred to react 0.2h, and the additional amount of hydrogen peroxide is surface cladding
The 6wt% of the diadust of graphene, filtering, being washed to pH value is 6, after drying, obtains surface with oxygen-containing functional group
Diadust；
S3, the surface that S2 is obtained is placed in sensitization-activated water solutions with the diadust of oxygen-containing functional group and is stirred
8min, the sensitization-activated water solutions include palladium chloride 0.5g/L, stannic chloride 2g/L, concentrated hydrochloric acid 45ml/L, sodium chloride 75g/L,
Water washing is distilled after filtering, is then added to ortho phosphorous acid sodium water solution stirring 2min and is carried out dispergation reduction, the sodium hypophosphite
Aqueous solution includes 18g/L sodium hypophosphite, is dried after distilling water washing, and it is micro- to obtain diamond of the surface with catalytic activity palladium
Powder；
S4, there is the diadust of catalytic activity palladium to be added in chemical plating fluid the surface that S3 is obtained, the chemistry
Plating solution include: nickel sulfate hexahydrate 10g/L, sodium hypophosphite 16g/L, sodium tungstate 2g/L, sodium citrate 40g/L, lactic acid 8mL/L,
Ammonium sulfate 28g/L, saccharin 0.7g/L, succinic acid 8g/L, potassium iodide 16mg/L carry out chemical plating, plating process at 70 DEG C
In, adjusting bath pH value is 9, stirring rate 250r/min, Plating times 0.8h, is stood after the completion of plating, washing, vacuum
It is dry, then it is heat-treated 2h at 450 DEG C, obtain the diadust that coating surface has Ni-W-P coating.
Comparative example 1
A kind of preparation method of diamond surface Electroless Ni-W-P coating, includes the following steps:
S1, the diadust that partial size is 100 μm is added in dilution heat of sulfuric acid, 2h is impregnated at 70 DEG C, after filtering
It is washed with distilled water, then is cleaned by ultrasonic with acetone, then washed with dehydrated alcohol, drying is placed in sensitization-activated water solutions
7min is stirred, the sensitization-activated water solutions include palladium chloride 0.4g/L, stannic chloride 3g/L, concentrated hydrochloric acid 40ml/L, sodium chloride
70g/L distills water washing after filtering, is then added to ortho phosphorous acid sodium water solution stirring 3min and carries out dispergation reduction, described time sub-
Sodium phosphate aqueous solution includes 17g/L sodium hypophosphite, is dried after distilling water washing, and the Buddha's warrior attendant that surface has catalytic activity palladium is obtained
Stone micro mist；
S2, there is the diadust of catalytic activity palladium to be added in chemical plating fluid the surface that S1 is obtained, the chemistry
Plating solution include: nickel sulfate hexahydrate 12g/L, sodium hypophosphite 15g/L, sodium tungstate 2g/L, sodium citrate 30g/L, lactic acid 7mL/L,
Ammonium sulfate 25g/L, saccharin 0.8g/L, succinic acid 10g/L, potassium iodide 15mg/L carry out chemical plating, plating process at 70 DEG C
In, adjusting bath pH value is 9, stirring rate 200r/min, Plating times 0.7h, is stood after the completion of plating, washing, vacuum
It is dry, then it is heat-treated 3h at 400 DEG C, obtain the diadust that coating surface has Ni-W-P coating.
Overlay coating chemical composition analysis is carried out to the diadust obtained in embodiment 1-4 and comparative example 1 respectively, is shown
Microhardness and corrosion resistance test, the dilution heat of sulfuric acid that the corrosive medium that corrosion resistance is selected when testing is 10% is to sample
It is impregnated, etching time 72h, uses the of poor quality as corrosion rate of experiment front and back unit time unit area sample,
The results are shown in Table 1:
The performance test results of diadust overlay coating in 1 embodiment 1-4 of table and comparative example 1
| Constituent content | Microhardness | Corrosion rate mg/ (cm2·h) | |
| Embodiment 1 | Ni86.05%, W1.35%, P12.60% | 633 | 0.0222 |
| Embodiment 2 | Ni86.11%, W1.06%, P12.83% | 621 | 0.0205 |
| Embodiment 3 | Ni86.03%, W1.62%, P12.35% | 649 | 0.0237 |
| Embodiment 4 | Ni85.98%, W1.48%, P12.54% | 638 | 0.0229 |
| To applying example 1 | Ni86.38%, W0.37%, P13.25% | 569 | 0.0878 |
The Ni-W-P coating on the diadust surface of 1-4 of embodiment of the present invention preparation is typical amorphous structure,
Surface is made of cellular content tissue, for the General N i-W-P coating in comparative example 1, cellular content is smaller, more evenly, cause
It is close；As seen from the above table, the microhardness of Ni-W-P coating surface is higher than the corresponding coating of comparative example 1 in embodiment 1-4, embodiment
The corrosion resistance of Ni-W-P coating compares and is improved for the coating in comparative example 1 in 1-4.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of diamond surface Electroless Ni-W-P coating, which comprises the steps of:
S1, the diadust that partial size is 50-200 μm is added in dilution heat of sulfuric acid, 1-3h, mistake is impregnated at 60-80 DEG C
It with partial size is 20-30 μm of iron powder after filter and partial size is that 1-5 μm of nickel powder mixes, in 0.1-1 × 10-3It heats up under the vacuum condition of Pa
To 1200-1300 DEG C, powder is obtained after insulation reaction 1-2h, after removing iron nickel powder superfluous in powder, is put into dilution heat of sulfuric acid
Middle immersion 1-3h is filtered, and washing after drying, obtains the diadust of surface coated graphite alkene；
S2, it will be mixed in the diadust addition concentrated sulfuric acid solution of coated graphite alkene in surface obtained in S1, under ice-water bath
It is stirred to react 0.3-0.5h after potassium permanganate is added, the hydrogen peroxide that content is 3-6wt% is added and is stirred to react 0.1-0.3h, mistake
Filter, being washed to pH value is 6-7, after drying, obtains the diadust that surface has oxygen-containing functional group；
S3, the surface that S2 is obtained is placed in sensitization-activated water solutions with the diadust of oxygen-containing functional group and stirs 5-
10min distills water washing after filtering, is then added to ortho phosphorous acid sodium water solution stirring 2-4min and carries out dispergation reduction, distilled water
It is dried after washing, obtains the diadust that surface has catalytic activity palladium；
S4, there is the diadust of catalytic activity palladium to be added in chemical plating fluid surface that S3 is obtained, at 60-80 DEG C into
Row chemical plating, during plating, adjusting bath pH value is 8-10, stirring rate 150-300r/min, and Plating times are
0.5-1h, plating are stood after the completion, are washed, vacuum drying, then are heat-treated 1-5h at 300-500 DEG C, and obtaining coating surface has
The diadust of Ni-W-P coating.
2. the preparation method of diamond surface Electroless Ni-W-P coating according to claim 1, which is characterized in that S1
In, diadust is added in dilution heat of sulfuric acid and is impregnated, further includes being washed to the diadust after immersion after filtering
It washs, specifically, being first washed with distilled water, then is cleaned by ultrasonic with acetone, is then washed with dehydrated alcohol.
3. the preparation method of diamond surface Electroless Ni-W-P coating according to claim 1 or 2, which is characterized in that
In S1, diadust is 2-5:1:1 with the weight ratio of iron powder and nickel powder.
4. the preparation method of diamond surface Electroless Ni-W-P coating according to claim 1-3, feature
It is, in S2, the additional amount of potassium permanganate is the 1-5wt% of the diadust of the surface coated graphite alkene, hydrogen peroxide
Additional amount is the 1-10wt% of the diadust of the surface coated graphite alkene.
5. the preparation method of diamond surface Electroless Ni-W-P coating according to claim 1-4, feature
It is, in S3, the sensitization-activated water solutions include palladium chloride 0.3-0.6g/L, stannic chloride 1-5g/L, concentrated hydrochloric acid 30-50ml/
L, sodium chloride 60-80g/L.
6. the preparation method of diamond surface Electroless Ni-W-P coating according to claim 1-5, feature
It is, in S3, the ortho phosphorous acid sodium water solution includes 15-20g/L sodium hypophosphite.
7. the preparation method of diamond surface Electroless Ni-W-P coating according to claim 1-6, feature
Be, in S4, the chemical plating fluid include: nickel sulfate hexahydrate 8-16g/L, sodium hypophosphite 10-20g/L, sodium tungstate 1-3g/L,
Sodium citrate 20-50g/L, lactic acid 5-10mL/L, ammonium sulfate 20-30g/L, saccharin 0.5-1g/L, succinic acid 5-15g/L, iodate
Potassium 10-20mg/L.
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| CN110904442A (en) * | 2019-11-27 | 2020-03-24 | 洛阳吉瓦新材料科技有限公司 | Diamond surface modification method |
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