CN106435666B - A method of high-temperature alloy surface deposition layer is prepared using neutral platinum plating solution - Google Patents
A method of high-temperature alloy surface deposition layer is prepared using neutral platinum plating solution Download PDFInfo
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- CN106435666B CN106435666B CN201611046074.4A CN201611046074A CN106435666B CN 106435666 B CN106435666 B CN 106435666B CN 201611046074 A CN201611046074 A CN 201611046074A CN 106435666 B CN106435666 B CN 106435666B
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 51
- 238000007747 plating Methods 0.000 title claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 21
- 239000000956 alloy Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000007935 neutral effect Effects 0.000 title claims abstract description 13
- 230000008021 deposition Effects 0.000 title claims description 13
- 238000004070 electrodeposition Methods 0.000 claims abstract description 51
- 239000000243 solution Substances 0.000 claims abstract description 44
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910002621 H2PtCl6 Inorganic materials 0.000 claims abstract description 14
- 229910000397 disodium phosphate Inorganic materials 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000012360 testing method Methods 0.000 claims description 79
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000000151 deposition Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000009713 electroplating Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- 239000000356 contaminant Substances 0.000 claims description 4
- 238000005238 degreasing Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000003518 caustics Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002932 luster Substances 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 20
- 239000003513 alkali Substances 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 8
- 238000001994 activation Methods 0.000 description 7
- 238000000576 coating method Methods 0.000 description 5
- 238000005554 pickling Methods 0.000 description 5
- UUWCBFKLGFQDME-UHFFFAOYSA-N platinum titanium Chemical compound [Ti].[Pt] UUWCBFKLGFQDME-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000001141 propulsive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
- C25D5/40—Nickel; Chromium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
It is neutral electrolyte solution, and provides and the method with semi-transparent bright metal gloss, binding force and preferable, the in homogeneous thickness platinum electrodeposition of compactness is prepared in high-temperature alloy surface using the solution with high current efficiency, pH value the purpose of the present invention is to provide a kind of.The neutrality platinum plating solution is H2PtCl6·6H2O aqueous solution, Na2HPO4Or K2HPO4, deionized water mixed solution electrolyte solution, its pH value controls between 7.0~7.5, the neutral electrolyte solution is different from traditional acid or alkaline platinum plating solution, the compactness and metallic luster of the existing acid platinum plating solution of the platinum layer obtained after electro-deposition, and there is the characteristic of the good binding force of alkaline platinum plating solution.And the electrolyte solution preparation method is simple, is suitable for promoting and applying.
Description
Technical field
The invention belongs to surfaces to process, coatings art, in particular to platiniferous in a kind of high-temperature alloy surface antioxidant coating
It is prepared by the coating of element.
Background technique
Platinum, fusing point with higher, is applied in high temperature alloy, can form solid solution conduct with other metallic elements
The surface covering or adhesive layer of high-temperature component to effectively improve the use temperature of component, while enhancing matrix and other paintings
Cohesive force between layer.During preparing platiniferous high-temperature oxidation resistant coating, it is necessary first to one layer of platinum be electroplated in matrix surface.
Classify according to traditional pH value to platinum plating solution, acid and alkalinity can be classified as.Acidic bath (pH value range
Between 0.2~3.0) platinum layer prepared, surface porosity factor is low, and it is more bright, this is because being reduced in deposition process
Pt atom matrix surface grow it is comparatively dense, still, this also increases the internal stress between sedimentary and matrix, internal stress
Become larger with the increase of deposit thickness, sedimentary is easily made crack phenomenon occur, leads to the thickness of sedimentary tool in deposition
There is certain limitation, meanwhile, also reduce the binding force between sedimentary and matrix；Alkali plating solution (pH value range be 9.0~
Between 13.5) platinum layer prepared, the good bonding strength with matrix, this is because the pt atom being reduced is raw in matrix surface
Length is more dispersed, causes the surface of sedimentary there are certain hole, the presence of these holes can discharge sedimentary and matrix
Between internal stress, still, the sedimentary surface color that alkali plating solution is prepared is darker, without metallic luster.It can be seen that plating
The pH value of platinum liquid directly affects the quality of sedimentary, in addition, pH value be also influence electrolytic cell in cathode efficiency it is crucial because
The height of element, current efficiency directly affects the deposition efficiency of electroplate liquid.
Both there is high current the advantages of developing one kind while having acid and alkaline platinum plating solution concurrently based on these factors
Efficiency, but the electrolyte solution with good binding force and compactness is very important.
Summary of the invention
Have high current efficiency, pH value (7.0~7.5) for neutral electrolysis the object of the present invention is to provide a kind of
Matter solution, and provide and prepared in high-temperature alloy surface with semi-transparent bright metal gloss, binding force and densification using the solution
The method of property platinum electrodeposition preferable, in homogeneous thickness.
The present invention specifically provides a kind of neutral platinum plating solution, it is characterised in that: the neutrality platinum plating solution is H2PtCl6·
6H2O aqueous solution, Na2HPO4Or K2HPO4, deionized water mixed solution electrolyte solution, pH value control 7.0~7.5 it
Between, the neutrality platinum plating solution current efficiency with higher.
Wherein, H in the neutral platinum plating solution2PtCl6·6H2The mass percent of O is 20~40%, Na2HPO4Or
K2HPO4Concentration be 7~17g/L.
Pass through Na in the present invention2HPO4Or K2HPO4The electromotive force of Pt ion in electrolyte solution is improved, Pt ion is accelerated to exist
Cathode surface reduction, guarantees electrodeposition process current efficiency with higher, current efficiency is up to 38~60%.
The pH value of neutrality platinum plating solution of the present invention adjusts the solution used as H3PO4Or NH3·H2O, concentration are respectively
20~60% and 40~80%.
The present invention also provides the method for preparing high-temperature alloy surface deposition layer using the neutral platinum plating solution, features
It is, specific steps are as follows:
(1), by each surface grinding of high temperature alloy test piece, and edges and corners are ground into chamfering；
(2), blast processing is carried out to strip, it is desirable that each surface blast is uniform；
(3), test piece is cleaned by ultrasonic using organic solvent, removes surface and oil contaminant；
(4), the cleaning of alkali soluble propulsive cathode is respectively adopted and HCl solution etch carries out at surface degreasing cleaning and activation test piece
Reason；
(5), test piece is electroplated using the method for DC electrodeposition, test piece is as cathode, design parameter are as follows: electrolyte
The pH value of solution is 7.0~7.5, and electrolyte solution temperature is between 65~80 DEG C, and current density is 1~8A/dm2(ASD), electric
The plating time is 10~60min；
(6), the test piece after plating is cleaned with hot deionized water, washes away electrolyte solution remained on surface, is then placed in
It is dried in drying box.
Wherein, high temperature alloy substrate selected in step (1) is one of iron-based, Ni-based and cobalt-base alloys.
Solution used by removal surface and oil contaminant is the mixed solution of one of ethyl alcohol, acetone or both in step (3).
NaOH and HCl solution is respectively adopted in surface degreasing cleaning and activation processing in step (4), wherein NaOH solution is dense
Degree is 20~50%, and scavenging period is 2~10min；HCl solution concentration is 10~40%, and the processing time is 5~20s.
Test piece in step (6) after plating is cleaned using 50~80 DEG C of hot deionized waters, washes away electricity remained on surface
Electrolyte solution is then put into drying box and is dried, and drying temperature is 120~150 DEG C, and the time is 5~20min.
The present invention has the advantage that and the utility model has the advantages that
(1) platinum plating solution mentioned in the present invention is neutral (pH value 7.0~7.5) electrolyte solution, is different from traditional
Acid or alkaline platinum plating solution, the compactness and metallic luster of the existing acid platinum plating solution of the platinum layer of electro-deposition, and there is alkaline platinum plating
The characteristic of the good binding force of liquid is a kind of novel method for preparing platinum electrodeposition in high-temperature alloy surface.
(2) neutrality (pH value 7.0~7.5) platinum plating solution mentioned in the present invention, the electrolyte solution of selection are acid and nothing
The mixed liquor of machine salt, preparation method are simple.The electrolyte solution current efficiency of traditional inorganic solvent is 10~30%, and of the invention
The current efficiency of electrolyte solution can achieve 38~60%, can be heavy in high-temperature alloy surface by controlling electroplating parameter
Thickness is uniform out for product, and the sedimentary of surface compact.
Detailed description of the invention
Fig. 1 is the test piece macro surface after electro-deposition, is in semi-transparent bright metal color.
Fig. 2 is the test piece microcosmic surface observed under scanning electron microscope, and deposition layer surface is comparatively dense.
Fig. 3 is the thickness for the test piece section sedimentary observed under scanning electron microscope, the electro-deposition major parameter of selection are as follows: electricity
Current density 5A/dm2(ASD) 10min is deposited under.
Specific embodiment
Embodiment 1
(1), substrate prepares: a kind of nickel base superalloy (trade mark DD413) being selected to be used as substrate, the alloy that will have been cast
The test piece of 10 × 12 × 2mm is made of wire cutting machine for stick, and each surface of test piece is polished with 600# sand paper, and edges and corners are ground
Chamfering.
(2), blast is handled: using Al2O3Sand grains carries out blast to strip, and each surface blast is uniform.
(3), organic solvent is cleaned by ultrasonic: using acetone soln, is cleaned by ultrasonic to the test piece after blast, removes surface
Greasy dirt, ultrasonic frequency 280KHz, scavenging period 30min.
(4), alkali cleaning and pickling: the NaOH for being 30% with concentration carries out oil removing to test piece and cleans, time 5min；Use concentration
Surface activation process, time 20s are carried out to test piece for 10% HCl.
(5), it weighs before test piece electro-deposition: being 10 with exact value-4The balance of g weighs to test piece, records its electro-deposition
Preceding quality is 1.8992g.
(6), strip electro-deposition platinum layer: being electroplated using the method for DC electrodeposition, and test piece is as cathode, anode
Plate uses platinum titanium net, and preparing electrolyte solution used by electro-deposition platinum layer is H2PtCl6·6H2O、Na2HPO4And deionized water
Mixed solution, wherein H2PtCl6·6H2The mass percent of O is 20%, Na2HPO4Concentration be 7g/L, remaining for go from
Sub- water；Electrolyte solution is heated to 65 DEG C, measuring its pH value is 7.2, after powering on, and applies 5A/dm to test piece2(ASD)
Current density, stop after electroplating time 10min, test piece taken out from electrolytic cell.
(7), the test piece after plating is cleaned with 80 DEG C of hot deionized waters, washes away electrolyte solution remained on surface, then
It is put into 150 DEG C of drying boxes, dries 5min.
(8), it increases weight and calculates after test piece electro-deposition: being 10 with exact value-4The balance of g claims the test piece after electro-deposition
Weight, recording its quality is 1.9207g, and the increase quality for calculating test piece after electro-deposition is 0.0215g.
(9), its macro surface of post-depositional sample is the metallochrome (Fig. 1) of semi-transparent light, is seen under scanning electron microscope
It examines, microcosmic surface is comparatively dense (Fig. 2), and deposit thickness is about 3 μm (Fig. 3).
(10), electrolyte solution mentioned in the present invention can be gone out to post-depositional weight gain Mass Calculation by faraday's formula
Cathode efficiency (ηc%) and the thickness of deposition layer (δ):
By formula,
Calculate the cathode efficiency (η of electrolyte solutioncIt %) is about 43%.Wherein, m ' is to increase weight after electro-deposition
Quality；M is the calculated weight gain quality of Faraday's law；I is current strength；T is sedimentation time；K is chemical equivalent.
By formula,
The theoretic throat (δ) for calculating deposition layer is 3.1 μm, almost the same with microscopic measurement value.Wherein, icFor electric current
Density；K is chemical equivalent；T is sedimentation time；ε1For cathode efficiency；ρ is the density of platinum.
Embodiment 2
(1), preparation step is the same as embodiment 1 before test piece is electroplated.
(2), alkali cleaning and pickling: the NaOH for being 20% with concentration carries out oil removing to test piece and cleans, time 10min；With dense
Degree carries out surface activation process, time 5s to test piece for 40% HCl.
(3), it weighs before test piece electro-deposition: being 10 with exact value-4The balance of g weighs to test piece, records its electro-deposition
Preceding quality is 1.7336g.
(4), strip electro-deposition platinum layer: being electroplated using the method for DC electrodeposition, and test piece is as cathode, anode
Plate uses platinum titanium net, and preparing electrolyte solution used by electro-deposition platinum layer is H2PtCl6·6H2O、Na2HPO4And deionized water
Mixed solution, wherein H2PtCl6·6H2The mass percent of O is 30%, Na2HPO4Concentration be 14g/L, remaining for go from
Sub- water；Electrolyte solution is heated to 73 DEG C, measuring its pH value is 7.0, after powering on, and applies 3A/dm to test piece2(ASD)
Current density, stop after electroplating time 20min, test piece taken out from electrolytic cell.
(5), the test piece after plating is cleaned with 50 DEG C of hot deionized waters, washes away electrolyte solution remained on surface, then
It is put into 120 DEG C of drying boxes, dries 20min.
(6), it increases weight and calculates after test piece electro-deposition: being 10 with exact value-4The balance of g claims the test piece after electro-deposition
Weight, recording its quality is 1.7676g, and the increase quality for calculating test piece after electro-deposition is 0.034g.
(7), its macro surface of post-depositional sample is the metallochrome of semi-transparent light, is observed under scanning electron microscope,
Microcosmic surface is comparatively dense, and deposit thickness is about 4.8 μm, cathode efficiency (ηcIt %) is about 57%.
Embodiment 3
(1), preparation step is the same as embodiment 1 before test piece is electroplated.
(2), alkali cleaning and pickling: the NaOH for being 50% with concentration carries out oil removing to test piece and cleans, time 2min；Use concentration
Surface activation process, time 10s are carried out to test piece for 20% HCl.
(3), it weighs before test piece electro-deposition: being 10 with exact value-4The balance of g weighs to test piece, records its electro-deposition
Preceding quality is 1.7921g.
(4), strip electro-deposition platinum layer: being electroplated using the method for DC electrodeposition, and test piece is as cathode, anode
Plate uses platinum titanium net, and preparing electrolyte solution used by electro-deposition platinum layer is H2PtCl6·6H2O、Na2HPO4And deionized water
Mixed solution, wherein H2PtCl6·6H2The mass percent of O is 40%, Na2HPO4Concentration be 17g/L, remaining for go from
Sub- water；Electrolyte solution is heated to 80 DEG C, measuring its pH value is 7.5, after powering on, and applies 3A/dm to test piece2(ASD)
Current density, stop after electroplating time 20min, test piece taken out from electrolytic cell.
(5), the test piece after plating is cleaned with 70 DEG C of hot deionized waters, washes away electrolyte solution remained on surface, then
It is put into 130 DEG C of drying boxes, dries 10min.
(6), it increases weight and calculates after test piece electro-deposition: being 10 with exact value-4The balance of g claims the test piece after electro-deposition
Weight, recording its quality is 1.8279g, and the increase quality for calculating test piece after electro-deposition is 0.0358g.
(7), its macro surface of post-depositional sample is the metallochrome of semi-transparent light, is observed under scanning electron microscope,
Microcosmic surface is comparatively dense, and deposit thickness is about 5.1 μm, cathode efficiency (ηcIt %) is about 60%.
Embodiment 4
(1), preparation step is the same as embodiment 1 before test piece is electroplated.
(2), alkali cleaning and pickling: the NaOH for being 35% with concentration carries out oil removing to test piece and cleans, time 6min；Use concentration
Surface activation process, time 13s are carried out to test piece for 15% HCl.
(3), it weighs before test piece electro-deposition: being 10 with exact value-4The balance of g weighs to test piece, records its electro-deposition
Preceding quality is 1.9333g.
(4), strip electro-deposition platinum layer: being electroplated using the method for DC electrodeposition, and test piece is as cathode, anode
Plate uses platinum titanium net, and preparing electrolyte solution used by electro-deposition platinum layer is H2PtCl6·6H2O、K2HPO4With deionized water
Mixed solution, wherein H2PtCl6·6H2The mass percent of O is 25%, K2HPO4Concentration be 10g/L, remaining is deionization
Water；Electrolyte solution is heated to 76 DEG C, measuring its pH value is 7.1, after powering on, and applies 1A/dm to test piece2(ASD)
Current density stops after electroplating time 60min, test piece is taken out from electrolytic cell.
(5), the test piece after plating is cleaned with 75 DEG C of hot deionized waters, washes away electrolyte solution remained on surface, then
It is put into 140 DEG C of drying boxes, dries 8min.
(6), it increases weight and calculates after test piece electro-deposition: being 10 with exact value-4The balance of g claims the test piece after electro-deposition
Weight, recording its quality is 1.9643g, and the increase quality for calculating test piece after electro-deposition is 0.031g.
(7), its macro surface of post-depositional sample is the metallochrome of semi-transparent light, is observed under scanning electron microscope,
Microcosmic surface is comparatively dense, and deposit thickness is about 4.4 μm, cathode efficiency (ηcIt %) is about 52%.
Embodiment 5
(1), preparation step is the same as embodiment 1 before test piece is electroplated.
(2), alkali cleaning and pickling: the NaOH for being 40% with concentration carries out oil removing to test piece and cleans, time 4min；Use concentration
Surface activation process, time 8s are carried out to test piece for 30% HCl.
(3), it weighs before test piece electro-deposition: being 10 with exact value-4The balance of g weighs to test piece, records its electro-deposition
Preceding quality is 1.87g.
(4), strip electro-deposition platinum layer: being electroplated using the method for DC electrodeposition, and test piece is as cathode, anode
Plate uses platinum titanium net, and preparing electrolyte solution used by electro-deposition platinum layer is H2PtCl6·6H2O、K2HPO4With deionized water
Mixed solution, wherein H2PtCl6·6H2The mass percent of O is 35%, K2HPO4Concentration be 16g/L, remaining is deionization
Water；Electrolyte solution is heated to 68 DEG C, measuring its pH value is 7.4, after powering on, and applies 8A/dm to test piece2(ASD)
Current density stops after electroplating time 30min, test piece is taken out from electrolytic cell.
(5), the test piece after plating is cleaned with 60 DEG C of hot deionized waters, washes away electrolyte solution remained on surface, then
It is put into 125 DEG C of drying boxes, dries 15min.
(6), it increases weight and calculates after test piece electro-deposition: being 10 with exact value-4The balance of g claims the test piece after electro-deposition
Weight, recording its quality is 1.96g, and the increase quality for calculating test piece after electro-deposition is 0.09g.
(7), its macro surface of post-depositional sample is the metallochrome of semi-transparent light, is observed under scanning electron microscope,
Microcosmic surface is comparatively dense, and deposit thickness is about 12.8 μm, cathode efficiency (ηcIt %) is about 38%.
Electrolyte solution of the invention current efficiency with higher can be verified by example, it within a short period of time can be with
Deposit surface compact, coating in homogeneous thickness.
Examples detailed above is only illustrated a certain parameter in each parameter scope in the present invention, but the present invention
Design be not limited thereto, all changes that unsubstantiality is carried out using the invention belong to invade the scope of the present invention
Behavior.
Claims (7)
1. a kind of neutrality platinum plating solution, it is characterised in that: the neutrality platinum plating solution is H2PtCl6·6H2O aqueous solution, Na2HPO4Or
K2HPO4, deionized water mixed solution electrolyte solution, pH value is between 7.0~7.5；In the neutrality platinum plating solution
H2PtCl6·6H2The mass percent of O is 20~40%, Na2HPO4Or K2HPO4Concentration be 7~17g/L.
2. according to neutrality platinum plating solution described in claim 1, it is characterised in that: the pH value of the neutrality platinum plating solution adjusts the molten of use
Liquid is H3PO4Or NH3·H2O, concentration are respectively 20~60% and 40~80%.
3. a kind of using the method that neutrality platinum plating solution prepares high-temperature alloy surface deposition layer described in claim 1, feature exists
In specific steps are as follows:
(1), by each surface grinding of high temperature alloy test piece, and edges and corners are ground into chamfering；
(2), blast processing is carried out to strip, it is desirable that each surface blast is uniform；
(3), test piece is cleaned by ultrasonic using organic solvent, removes surface and oil contaminant；
(4), caustic dip and HCl solution etch is respectively adopted, surface degreasing cleaning and activation processing is carried out to test piece；
(5), test piece is electroplated using the method for DC electrodeposition, test piece is as cathode, design parameter are as follows: electrolyte solution
PH value be 7.0~7.5, electrolyte solution temperature be 65~80 DEG C between, current density be 1~8A/dm2, electroplating time is
10~60min；
(6), the test piece after plating is cleaned with hot deionized water, washes away electrolyte solution remained on surface, be then placed in drying
It is dried in case.
4. according to the method for preparing high-temperature alloy surface deposition layer using neutral platinum plating solution described in claim 3, feature exists
In: selected high temperature alloy substrate is one of iron-based, Ni-based and cobalt-base alloys.
5. according to the method for preparing high-temperature alloy surface deposition layer using neutral platinum plating solution described in claim 3, feature exists
In: solution used by removal surface and oil contaminant is the mixed solution of one of ethyl alcohol, acetone or both in step (3).
6. according to the method for preparing high-temperature alloy surface deposition layer using neutral platinum plating solution described in claim 3, feature exists
In: NaOH and HCl solution is respectively adopted in surface degreasing cleaning and activation processing in step (4), wherein NaOH solution concentration is 20
~50%, scavenging period is 2~10min；HCl solution concentration is 10~40%, and the processing time is 5~20s.
7. according to the method for preparing high-temperature alloy surface deposition layer using neutral platinum plating solution described in claim 3, feature exists
In: the test piece after plating is cleaned using 50~80 DEG C of hot deionized waters, is washed away electrolyte solution remained on surface, is then put
Enter in drying box and dried, drying temperature is 120~150 DEG C, and the time is 5~20min.
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|---|---|---|---|---|
| US2027358A (en) * | 1931-03-12 | 1936-01-07 | Johnson Matthey Co Ltd | Electrodeposition of metals of the platinum group |
| CN103492618A (en) * | 2011-01-12 | 2014-01-01 | 庄信万丰股份有限公司 | Improvements in coating technology |
| CN104040032A (en) * | 2012-01-12 | 2014-09-10 | 庄信万丰股份有限公司 | Improvements in coating technology |
| CN105671601A (en) * | 2015-12-31 | 2016-06-15 | 中国科学院深圳先进技术研究院 | Microelectrode surface modification method |
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| US2027358A (en) * | 1931-03-12 | 1936-01-07 | Johnson Matthey Co Ltd | Electrodeposition of metals of the platinum group |
| CN103492618A (en) * | 2011-01-12 | 2014-01-01 | 庄信万丰股份有限公司 | Improvements in coating technology |
| CN104040032A (en) * | 2012-01-12 | 2014-09-10 | 庄信万丰股份有限公司 | Improvements in coating technology |
| CN105671601A (en) * | 2015-12-31 | 2016-06-15 | 中国科学院深圳先进技术研究院 | Microelectrode surface modification method |
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