CN106498459A - A kind of electrodeposition of titanium method - Google Patents
A kind of electrodeposition of titanium method Download PDFInfo
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- CN106498459A CN106498459A CN201610955633.7A CN201610955633A CN106498459A CN 106498459 A CN106498459 A CN 106498459A CN 201610955633 A CN201610955633 A CN 201610955633A CN 106498459 A CN106498459 A CN 106498459A
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- 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
- C25D3/54—Electroplating: Baths therefor from solutions of metals not provided for in groups C25D3/04 - C25D3/50
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- 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
- C25D5/003—Electroplating using gases, e.g. pressure influence
Abstract
A kind of electrodeposition of titanium method, with plating metal as negative electrode, with simple substance titanium as anode, to add 0.146 ~ 0.208 moL of titanium sulfate, 0.07 ~ 0.176 moL of sodium sulfate, 0.003 ~ 0.008 moL of vanadate, 0.736 ~ 1.288moL of sulphuric acid, 10 ~ 25 g of surfactant to be formulated as electroplate liquid in every 1000mL water, electric current, voltage are set, implement electrodeposition of titanium.The electrodeposition of titanium method that the present invention is provided, have that processing speed is fast, short, forming efficiency is high to implement the time, simple to operation, breach the bottleneck of traditional electrodeposition of titanium method, thin film coating for neomorph provides a kind of new Method of Green Manufacture, provides a kind of new technological approaches for the manufacture production with coating material.
Description
Technical field
The invention belongs to metal electrodeposition field, is specifically related to a kind of electrodeposition of titanium method.
Background technology
Titanium is as a kind of strategic light metal, strong have the advantages that specific strength height, corrosion resistance, is usually used on submarine, aircraft,
Play a great role in navigation, aviation field, in metal surface, electrodeposition of titanium can play the corrosion-resistant effect of protection, can be applicable to as
Ocean, corrosive environment of sea water are medium.
The discharge potential of Titanium is low, realizes that the deposition of titanium is more difficult, while the immature also imperfection of the electroplating technology of titanium.Mesh
Front conventional method is as follows:One be electric arc ionization electro-plating method, using Titanium ionize in vacuum or noble gases be titanium from
Son and then bombarding cathode implement plating;Two is second-level titanizing method, first plates last layer active metal mainly on matrix(Such as
Magnesium), then cleaned with titanium tetrachloride solution, Titanium displaced by magnesium and be then plated on matrix;Three is fuse salt
Electro-plating method, with carbon oxygen titanium as anode, plating metal as negative electrode, fuse salt be electrolyte implement plating.But, electric arc ionization electricity
Electroplating method processing step is more, and energy resource consumption is high, and process is complicated, and operation difficulty is big;In second-level titanizing method, the electrode potential of magnesium is same
Sample is relatively low, and plating is difficult to;And fuse salt electro-plating method efficiency is low, cycle length, low cost, with certain limitation.
Content of the invention
The purpose of the present invention be that as solving the deficiencies in the prior art and provide a kind of easily shaping, high in machining efficiency, into
This low electrodeposition of titanium method.
The purpose of the present invention is realized in the following manner:
A kind of electrodeposition of titanium method, with plating metal as negative electrode, with simple substance titanium as anode, to add titanium sulfate in every 1000mL water
0.146 ~ 0.208 moL, 0.07 ~ 0.176 moL of sodium sulfate, 0.003 ~ 0.008 moL of vanadate, sulphuric acid 0.736 ~
1.288moL, 10 ~ 25 g of surfactant are formulated as electroplate liquid, arrange electric current, voltage, implement electrodeposition of titanium.
The plating metal is elemental metals, alloy material or solder.
The vanadate is vanadic acid sodium.
The surfactant is alkyl ether surfactant.
The alkyl ether surfactant be OP-10, polyoxyethylene lauryl ether, Polyethylene Glycol trimethyl nonyl ethers or
NPE.
The negative electrode and anode material are fixed on coating bath, and the spacing of cathode and anode is 20 ~ 25mm, and coating bath is isolation material.
The electrodeposition of titanium technological parameter is:0.5 ~ 5 A/dm of electric current density2, 3 ~ 10 V of voltage, electroplating solution temperature 35 ~
50 DEG C, 2 ~ 15 min of plating time.
The electrodeposition of titanium is carried out under noble gases or vacuum environment protection.
Beneficial effects of the present invention are as follows:1)Salt based on titanio sulfate, overcomes conventional arc ionization plating and two grades of plating
A kind of weak point of two methods, there is provided new method of electrodeposition of titanium;2)The electrodeposition of titanium method for being provided, not only can
Implement titanizing in monometallic, alloy surface, and in welding material ti coat on diamond, the preparation processing for neomorph solder provides one
Plant new approaches;3)Nonionic surfactant employed in electrodeposition of titanium plating solution not only can reduce between electrode and plating solution
Interfacial tension, but also there is leveling effect, cause cathode surface thickness of coating more uniform;4)Electrodeposition process is applied
Bath temperature is low, the time is short, with effect of energy;5)Electrodeposition of titanium is implemented under noble gases or vacuum environment protection,
The titanium coating cleanliness factor for depositing is high, does not contain any impurity, can prepare the titanium coating of high-quality.
The electrodeposition of titanium method that the present invention is provided, have the advantages that processing speed fast, implement that the time is short, forming efficiency is high,
Simple to operation, breach the bottleneck of traditional electrodeposition of titanium method, for neomorph thin film coating provide a kind of new green
Color manufacture method, provides a kind of new technological approaches for the manufacture production with coating material.
Specific embodiment
Embodiment 1
A kind of electrodeposition of titanium method, with plating metal as negative electrode, plating metal can be elemental metals, alloy material or solder(Such as
Ag-cu solder);With simple substance titanium as anode, negative electrode and anode material are fixed on coating bath, and coating bath is isolation material, between anode and cathode
Away from for 20 ~ 25mm, electroplate liquid is poured in coating bath;Then anode, cathode material are connected with the positive and negative electrode of plating power supply respectively
Connect, electric current, voltage are set, implement electrodeposition of titanium under noble gases or vacuum environment protection, after plating certain time, you can obtain
Obtain dense structure, equally distributed titanium electrodeposited coating.
To add 0.146 ~ 0.208 moL of titanium sulfate, 0.07 ~ 0.176 moL of sodium sulfate, vanadate in every 1000mL water
0.003 ~ 0.008 moL, 0.736 ~ 1.288moL of sulphuric acid, 10 ~ 25g of surfactant are formulated as electroplate liquid;Vanadate is preferably
Vanadic acid sodium;The surfactant is preferably alkyl ether surfactant, and further, alkyl ether surfactant is OP-
10th, any one in polyoxyethylene lauryl ether, Polyethylene Glycol trimethyl nonyl ethers, NPE.
Titanium sulfate deposits titanium coating for negative electrode and provides metal titanium ion as main salt in plating solution;Sodium sulfate is heavy as electricity
Additional salt in product titanium, can improve the electric conductivity of plating solution, reduce plating groove edge voltage, expand cathode-current density scope, improve
The dispersibility of plating solution;Vanadate is used as dispersant, it is possible to decrease the internal stress of coating, improves ductility of electrodeposited film, additionally it is possible to so that plating
Layer surface light;Sulphuric acid can improve the electric conductivity of plating solution as coating fining agent, can also refine coating crystal grain;Alkyl
Ether surfactant can reduce the interfacial tension between electrode and plating solution so that plating solution is easy to sprawl in electrode surface, while
There is leveling effect, cause cathode surface thickness of coating to be plated more uniform.
Plating power supply is D.C. regulated power supply;Electrodeposition of titanium technological parameter is preferably:0.5 ~ 5 A/dm of electric current density2, electricity
3 ~ 10 V of pressure, 35 ~ 50 DEG C of electroplating solution temperature, 2 ~ 15 min of plating time.Electrodeposition of titanium is preferably in noble gases or vacuum ring
Carry out under the protection of border, electrodeposition of titanium is implemented under noble gases or vacuum environment protection, and the titanium coating cleanliness factor for depositing is high, no
Containing any impurity, the titanium coating of high-quality can be prepared.
Embodiment 2
A kind of electrodeposition of titanium method, for BAg60Cu solders surface titanium deposition electrodeposited coating, comprises the following steps:
(1)Titanium sulfate 50 g/L is pressed first(0.208moL/L), 25 g/L of sodium sulfate(0.176moL/L), 1.5 g/L of vanadic acid sodium
(0.008moL/L), 70 ml/L of concentrated sulphuric acid that mass fraction is 98%(1.288moL/L), Polyethylene Glycol trimethyl nonyl ethers 25
G/L, 1000 ml of deionized water configure electroplate liquid, are stirred using EMS-15 magnetic stirring apparatuss;Liquid to be electroplated stirs
Afterwards, it is poured in PVC plastic coating bath;
(2)Simultaneously negative electrode BAg60Cu solders, anode material simple substance titanium are fixed on coating bath hanger, 25 mm of cathode and anode spacing;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In vacuum environment, 5 A/dm of electric current density is set2, 4.5 V of voltage, 50 DEG C of solution temperature, enforcement electrodeposition of titanium,
Electrodeposition of titanium is carried out in whipping process, 400 r/min of mixing speed, after 5 min of plating, you can on BAg60Cu solders surface
Obtain dense structure, be uniformly distributed, the titanium electrodeposited coating that thickness is 12 μm.
Embodiment 3
A kind of electrodeposition of titanium method, for red copper surface titanium deposition electrodeposited coating, comprises the following steps:
(1)Titanium sulfate 35 g/L is pressed first(0.146moL/L), 10 g/L of sodium sulfate(0.07moL/L), vanadic acid sodium 0.5g/L
(0.003moL/L), 40 ml/L of concentrated sulphuric acid that mass fraction is 98%(0.736moL/L), OP-10 10g/L, deionized water
1000 ml configure electroplate liquid, are stirred using EMS-15 magnetic stirring apparatuss;After liquid to be electroplated stirs, ABS is poured into
In plastic plating bath;
(2)Simultaneously negative electrode red copper, anode material simple substance titanium are fixed on coating bath hanger, 20 mm of cathode and anode spacing;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In vacuum environment, 4 A/dm of electric current density is set2, 3 V of voltage, 35 DEG C of solution temperature implement electrodeposition of titanium, electricity
Titanium deposition is carried out in whipping process, and 400 r/min of mixing speed, after plating 15min, you can organized in red copper surface
Fine and close, be uniformly distributed, the titanium electrodeposited coating that thickness is 30 μm.
Embodiment 4
A kind of electrodeposition of titanium method, for H62 brass surfaces titanium deposition electrodeposited coatings, comprises the following steps:
(1)Titanium sulfate 42 g/L is pressed first(0.175moL/L), 18 g/L of sodium sulfate(0.127moL/L), 1.0 g/L of vanadic acid sodium
(0.005moL/L), 55 ml/L of concentrated sulphuric acid that mass fraction is 98%(1.012moL/L), polyoxyethylene lauryl ether 18g/L,
1000 ml of deionized water configures electroplate liquid, is stirred using EMS-15 magnetic stirring apparatuss;After liquid to be electroplated stirs, will
Which is poured in ABS plastic coating bath;
(2)Simultaneously negative electrode H62 pyrite, anode material simple substance titanium are fixed on coating bath hanger, 22 mm of cathode and anode spacing;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In helium environmental protection, 0.5 A/dm of electric current density is set2, 10 V of voltage, 45 DEG C of solution temperature implement electricity heavy
Product titanium, electrodeposition of titanium are carried out in whipping process, and 400 r/min of mixing speed, after 10 min of plating, you can in H62 pyrite tables
Face obtain dense structure, be uniformly distributed, the titanium electrodeposited coating that thickness is 5 μm.
Embodiment 5
A kind of electrodeposition of titanium method, for BCu75SnNi solders surface titanium deposition electrodeposited coating, comprises the following steps:
(1)Titanium sulfate 38 g/L is pressed first(0.158moL/L), 16 g/L of sodium sulfate(0.113moL/L), vanadic acid sodium 1.2g/L
(0.007moL/L), 50 ml/L of concentrated sulphuric acid that mass fraction is 98%(0.92moL/L), NPE 15g/L,
1000 ml of deionized water configures electroplate liquid, is stirred using EMS-15 magnetic stirring apparatuss;After liquid to be electroplated stirs, will
Which is poured in epoxy resin coating bath;
(2)Simultaneously negative electrode BCu75SnNi solders, anode material simple substance titanium are fixed on coating bath hanger, cathode and anode spacing 20
mm;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In argon gas protection environment, 2 A/dm of electric current density is set2, 5 V of voltage, 40 DEG C of solution temperature implement electro-deposition
Titanium, electrodeposition of titanium are carried out in whipping process, and 400 r/min of mixing speed, after plating 12min, you can in BCu75SnNi prickers
Material surface obtain dense structure, be uniformly distributed, the titanium electrodeposited coating that thickness is 20 μm.
Embodiment 6
A kind of electrodeposition of titanium method, for pure nickel surface titanium deposition electrodeposited coating, comprises the following steps:
(1)Titanium sulfate 0.18moL/L, sodium sulfate 0.176moL/L, vanadic acid sodium 0.005moL/L, mass fraction are pressed first for 98%
Concentrated sulphuric acid 0.736moL/L, OP-10 20g/L, 1000 ml of deionized water configuration electroplate liquid, using EMS-15 magnetic stirring apparatuss
It is stirred;After liquid to be electroplated stirs, it is poured in PVC plastic coating bath;
(2)Simultaneously negative electrode pure nickel, anode material simple substance titanium are fixed on coating bath hanger, cathode and anode spacing 22mm;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In vacuum environment, 1 A/dm of electric current density is set2, 3 V of voltage, 40 DEG C of solution temperature implement electrodeposition of titanium, electricity
Titanium deposition is carried out in whipping process, and 400 r/min of mixing speed, after plating 4min, you can is obtained tissue on pure nickel surface and is caused
Close, be uniformly distributed, the titanium electrodeposited coating that thickness is 6 μm.
Embodiment 7
A kind of electrodeposition of titanium method, for red copper surface titanium deposition electrodeposited coating, comprises the following steps:
(1)Titanium sulfate 0.208moL/L, sodium sulfate 0.12moL/L, vanadic acid sodium 0.006moL/L, mass fraction are pressed first for 98%
Concentrated sulphuric acid 0.9moL/L, NPE 10g/L, 1000 ml of deionized water configuration electroplate liquid, using EMS-15 magnetic
Power agitator is stirred;After liquid to be electroplated stirs, it is poured in epoxy resin coating bath;
(2)Simultaneously negative electrode red copper, anode material simple substance titanium are fixed on coating bath hanger, cathode and anode spacing 25mm;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In argon gas protection environment, 3 A/dm of electric current density is set2, 6 V of voltage, 50 DEG C of solution temperature implement electro-deposition
Titanium, electrodeposition of titanium are carried out in whipping process, and 400 r/min of mixing speed, after plating 8min, you can obtained in red copper surface
Dense structure, be uniformly distributed, the titanium electrodeposited coating that thickness is 15 μm.
Embodiment 8
A kind of electrodeposition of titanium method, for BAg65Cu solders surface titanium deposition electrodeposited coating, comprises the following steps:
(1)Titanium sulfate 0.146moL/L, sodium sulfate 0.15moL/L, vanadic acid sodium 0.008moL/L, mass fraction are pressed first for 98%
Concentrated sulphuric acid 1.1moL/L, 25 g/L of Polyethylene Glycol trimethyl nonyl ethers, 1000 ml of deionized water configuration electroplate liquid, adopt
EMS-15 magnetic stirring apparatuss are stirred;After liquid to be electroplated stirs, it is poured in PVC plastic coating bath;
(2)Simultaneously negative electrode BAg65Cu solders, anode material simple substance titanium are fixed on coating bath hanger, 25 mm of cathode and anode spacing;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In helium environmental protection, 2.5 A/dm of electric current density is set2, 5 V of voltage, 45 DEG C of solution temperature implement electricity heavy
Product titanium, electrodeposition of titanium are carried out in whipping process, and 400 r/min of mixing speed, after 2 min of plating, you can in BAg65Cu prickers
Material surface obtain dense structure, be uniformly distributed, the titanium electrodeposited coating that thickness is 5 μm.
Embodiment 9
A kind of electrodeposition of titanium method, for Al55Cu alloy surface titanium deposition electrodeposited coatings, comprises the following steps:
(1)Titanium sulfate 0.19moL/L, sodium sulfate 0.07moL/L, vanadic acid sodium 0.003moL/L, mass fraction are pressed first for 98%
Concentrated sulphuric acid 1.288moL/L, 15 g/L of polyoxyethylene lauryl ether, 1000 ml of deionized water configuration electroplate liquid, using EMS-
15 magnetic stirring apparatuss are stirred;After liquid to be electroplated stirs, it is poured in ABS plastic coating bath;
(2)Simultaneously negative electrode Al55Cu alloys, anode material simple substance titanium are fixed on coating bath hanger, 22 mm of cathode and anode spacing;
(3)Then anode, cathode material is electric with the PS205 DC voltage-stabilizings plating of 20 V of rated voltage, 5 A of rated current respectively
The positive and negative electrode connection in source;
(4)In vacuum environment, 2.5 A/dm of electric current density is set2, 3.5 V of voltage, 35 DEG C of solution temperature implement electro-deposition
Titanium, electrodeposition of titanium are carried out in whipping process, and 400 r/min of mixing speed, after plating 6min, you can in Al55Cu alloy tables
Face obtain dense structure, be uniformly distributed, the titanium electrodeposited coating that thickness is 9 μm.
Above-described is only the preferred embodiment of the present invention, it is noted that for a person skilled in the art,
Under the premise of without departing from general idea of the present invention, some changes and improvements can also be made, these should also be considered as the present invention's
Protection domain.
Claims (8)
1. a kind of electrodeposition of titanium method, it is characterised in that:With plating metal as negative electrode, with simple substance titanium as anode, with every 1000mL
0.146 ~ 0.208 moL of titanium sulfate, 0.07 ~ 0.176 moL of sodium sulfate, 0.003 ~ 0.008 moL of vanadate, sulphuric acid is added in water
0.736 ~ 1.288moL, 10 ~ 25 g of surfactant are formulated as electroplate liquid, arrange electric current, voltage, implement electrodeposition of titanium.
2. electrodeposition of titanium method as claimed in claim 1, it is characterised in that:The plating metal is elemental metals, alloy material
Material or solder.
3. electrodeposition of titanium method as claimed in claim 1, it is characterised in that:The vanadate is vanadic acid sodium.
4. electrodeposition of titanium method as claimed in claim 1, it is characterised in that:The surfactant is lived for alkyl ether surface
Property agent.
5. electrodeposition of titanium method as claimed in claim 4, it is characterised in that:The alkyl ether surfactant be OP-10,
Polyoxyethylene lauryl ether, Polyethylene Glycol trimethyl nonyl ethers or NPE.
6. electrodeposition of titanium method as claimed in claim 1, it is characterised in that:The negative electrode and anode material are fixed on coating bath
On, the spacing of cathode and anode is 20 ~ 25mm, and coating bath is isolation material.
7. electrodeposition of titanium method as claimed in claim 1, it is characterised in that the electrodeposition of titanium technological parameter is:Electric current density
0.5~5 A/dm2, 3 ~ 10 V of voltage, 35 ~ 50 DEG C of electroplating solution temperature, 2 ~ 15 min of plating time.
8. electrodeposition of titanium method as claimed in claim 1, it is characterised in that:The electrodeposition of titanium is in noble gases or vacuum ring
Carry out under the protection of border.
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CN103046093A (en) * | 2012-12-21 | 2013-04-17 | 江苏大学 | Pulse electrodeposition method for improving surface abrasion resistance of high-speed steel roll |
CN105862096A (en) * | 2016-06-02 | 2016-08-17 | 烟台工程职业技术学院 | Method for preparing FHA bioactive coating through electrical brush-plating-sintering method |
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JPS5022493B1 (en) * | 1969-08-16 | 1975-07-31 | ||
JPS522842A (en) * | 1975-06-24 | 1977-01-10 | Gotou Seisakushiyo Kk | Method of producing metallic titanium |
SU1413157A1 (en) * | 1986-06-17 | 1988-07-30 | Киевское Производственное Объединение "Ювелирпром" | Titanium-plating electrolyte |
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