CN108286064A - A kind of pulse electrodeposition Ni-W/B4C nano composite deposite preparation method - Google Patents
A kind of pulse electrodeposition Ni-W/B4C nano composite deposite preparation method Download PDFInfo
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- CN108286064A CN108286064A CN201810091697.6A CN201810091697A CN108286064A CN 108286064 A CN108286064 A CN 108286064A CN 201810091697 A CN201810091697 A CN 201810091697A CN 108286064 A CN108286064 A CN 108286064A
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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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
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
Abstract
The invention discloses a kind of pulse electrodeposition Ni W/B4C nano composite film coating preparation method, includes the following steps:The first step:The pretreatment of steel disc matrix;Second step:The preparation of electroplate liquid;Third walks:Matrix is put into prepared electroplate liquid and carries out electro-deposition;4th step:The post-processing of plating piece.Pulse electrodeposition of the present invention prepares Ni W/B4The method of C nano composite film coating, is effectively improved B4Dispersion stabilizations of the C in electroplate liquid, hence it is evident that improve the agglomeration traits of nano particle, while improving the deposition of nano particle in nanocomposite, and determine B in plating solution4The optimum add amount of C nano particle is 2g/L.Compared to Ni W coating, prepared Ni W/B4There are C nano composite material excellent corrosion-resistant, abrasion resistance properties and higher microhardness, comprehensive performance to be significantly improved.
Description
Technical field
The invention belongs to electroplating technologies, and in particular to a kind of pulse electrodeposition preparation Ni-W/B4C nano composite film coating
Method.
Background technology
The compact structure of nickel-tungsten (Ni-W) alloy coating, hardness is high, heat-resist, wear-resistant at high temperature, anti-oxidant,
Showing excellent self-lubricating and corrosion resisting property, corrosion resistance is also very excellent especially in the environment containing halogen, and
And environmental pollution is small, is commonly used for nickel-base alloy coating, thus be increasingly valued by people in engineer application;However it utilizes and passes
When the direct current electrode position technique of system prepares Ni-W plated films, usually there is deposition rates slowly, electro-chemical activity site is few, current efficiency
The problems such as low and serious hydrogen evolution phenomenon so that the plated film of preparation occurs that residualinternal stress is excessive, crystal crystal boundary is apparent and crystal grain
The problems such as coarse or even coated surface generate the defects of dew point and micro-crack, eventually lead to local corrosion in practical applications
Occur, to influence the properties of plated film, reduces the actual life of Ni-W plated films.
Although had been introduced into Ni-W electrodeposition process as:Silicon carbide(SiC), titanium dioxide (TiO2), alundum (Al2O3)
(Al2O3), the nano materials such as PTFE with other mechanical performances such as the corrosion resistances, microhardness or wearability that improve Ni-W coating,
But it all has some limitations, such as:SiC is with obvious effects to the wearability for improving coating, to improving the micro- hard of Ni-W coating
It is poor to spend effect;PTFE is excellent to the self-lubricating effect for improving coating, to improving the microhardness and corrosion resistance of Ni-W coating
Effect is poor etc..
Invention content
The present invention is directed to deficiencies of the prior art, provides a kind of pulse electrodeposition preparation Ni-W/B4C nano is multiple
The method of condensation material, by introducing pulse plating techniques and by B4C nano particle mixes in plated film, utilizes its hardness and Buddha's warrior attendant
Stone is suitable, while having low-density, high elastic modulus and a series of wear-resisting and corrosion-resistant etc. excellent properties, can not only solve straight
The problem of galvanic electricity is plated, moreover it is possible to using the synergistic effect of the characteristic and material multiple elements design of solid particle itself, further
Effectively improve the wearability, corrosion resistance and microhardness of Ni-W plated films.
To achieve the above object, the technical solution adopted by the present invention to solve the technical problems is as follows.
(1) pre-treatment of matrix:Steel disc is finally carried out using sand paper polishing derusting then using oil removing is cleaned by ultrasonic
Acid-wash activation.The solution each group that oil removing is carried out to matrix is divided into:Sodium hydroxide 50g/L, sodium carbonate 40g/L, sodium phosphate 40g/L,
OP-10 emulsifiers 5ml/L, temperature 70 C, time 10min;Acid-wash activation:With the dilute sulfuric acid of 1mol/L, carried out under room temperature, the time
For 30s.
(2) preparation of electroplate liquid:Ni-W composite plating bath each groups are divided into:Trisodium citrate 0.5mol/L, sodium tungstate
0.14mol/L, sodium bromide 0.15mol/L, ammonium chloride 0.5mol/L, surfactant 0.1g/L, B4C nano particle 2g/L;
After the completion of electroplate liquid is prepared, magnetic agitation 30min is carried out to it first, then carries out ultrasonic agitation 30min, keeps nano particle equal
It is even to be dispersed stably in plating solution.
(3) electrodeposition process:The matrix of pre-treatment is put into prepared electroplate liquid and carries out electro-deposition;In deposition process
Control 75 DEG C of temperature, pH7.5, current density 5A/dm2;Applying pulse power supply is connected, pulse electrodeposition is proceeded by;It has been electroplated
Ultrasonic cleaning processing is carried out using ethyl alcohol and pure water at rear, obtains finished product;Technological parameter during pulse plating is:Pulse frequency
Rate is 1000Hz, duty ratio 0.8, time 60min, magnetic agitation speed 200rmp, the citric acid that mass concentration is 25%
The pH value that solution adjusts mixed solution is 7.0-7.5.
(4) post-processing of plating piece:Plating piece surface is cleaned by ultrasonic using ethyl alcohol, pure water successively, removes plating piece surface
The plating solution and nano particle of absorption.
Pulse electrodeposition of the present invention prepares Ni-W/B4The method of C nano composite film coating has following several beneficial
Effect.
(1) impulse electrodeposition technology preparation method is easy to operate, at low cost, and current efficiency is high, reduces plated film porosity, can
Effectively to inhibit hydrogen evolution phenomenon, improve the performance of plated film.
(2)B4For C nano particle since surface energy is larger, agglomeration is serious, passes through the surfactant added in solution
And electrodeposition process uses ultrasonic disperse and magnetic agitation simultaneously, is effectively improved B4Stably dispersings of the C in electroplate liquid
Property, hence it is evident that the agglomeration traits of nano particle are improved, while improving the deposition of nano particle in nanocomposite.
(3) Ni-W-B prepared by4C composite has the micro- of excellent corrosion-resistant, abrasion resistance properties and superelevation
The comprehensive performance of hardness, coating is significantly improved.
Description of the drawings
Fig. 1 is the experimental provision schematic diagram that the present invention uses.
Fig. 2 is the B that the present invention uses4Surface microscopic topographic under 5000 times of C nano particle.
Fig. 3 is Ni-W/B prepared by the present invention4(wherein a is sample to surface microscopic topographic under 3000 times of C nano composite film coating
Product 1:Ni-W;B-f is sample 2,3,4,5,6:Ni-W-(1、2、3、4、5g/L)B4C)。
Fig. 4 is the section BS-SEM images of sample 1 and sample 3 prepared by the present invention.
Fig. 5 is the EDS elements of sample 3 prepared by the present invention(Ni、W、B、C)Scan image.
Fig. 6 is the XRD diagram picture of all samples prepared by the present invention.
Fig. 7 is the microhardness of all samples prepared by the present invention.
Fig. 8 is the polarization curve of all samples prepared by the present invention.
Fig. 9 is the friction curve of sample 1 and sample 3 prepared by the present invention.
Figure 10 is sample 1 and pattern after the friction of sample 3 prepared by the present invention.
Specific implementation mode
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that the present embodiment is served only for
Invention is further explained, should not be understood as limiting the scope of the invention, the person skilled in the art in the field
The protection model of the present invention should be belonged to according to some the nonessential modifications and adaptations made for the present invention of aforementioned present invention content
It encloses.
Embodiment 1
Ni-W plates the preparation method of membrane sample 1, includes the following steps.
(1) pre-treatment of matrix:Steel disc is finally carried out using sand paper polishing derusting then using oil removing is cleaned by ultrasonic
Acid-wash activation.The solution each group that oil removing is carried out to matrix is divided into:Sodium hydroxide 50g/L, sodium carbonate 40g/L, sodium phosphate 40g/L,
OP-10 emulsifiers 5ml/L, temperature 70 C, time 10min;Acid-wash activation:With the dilute sulfuric acid of 1mol/L, carried out under room temperature, the time
For 30s.
(2) preparation of electroplate liquid:Ni-W composite plating bath each groups are divided into:Trisodium citrate 0.5mol/L, sodium tungstate
0.14mol/L, sodium bromide 0.15mol/L, ammonium chloride 0.5mol/L, surfactant 0.1g/L;After the completion of electroplate liquid is prepared,
Magnetic agitation 30min is carried out to it first, then carries out ultrasonic agitation 30min, nano particle is made uniformly and stably to be dispersed in plating
In liquid, the B of use is tested4The microscopic appearance of C nano particle is shown in Fig. 2.
(3) electrodeposition process:The matrix of pre-treatment is put into prepared electroplate liquid and carries out electro-deposition;In deposition process
Control 75 DEG C of temperature, pH7.5, current density 5A/dm2;Applying pulse power supply is connected, pulse electrodeposition is proceeded by;It has been electroplated
Ultrasonic cleaning processing is carried out using ethyl alcohol and pure water at rear, obtains finished product;Technological parameter during pulse plating is:Pulse frequency
Rate is 1000Hz, duty ratio 0.8, time 60min, magnetic agitation speed 200rmp;Experimental provision schematic diagram such as attached drawing 1
It is shown.
Embodiment 2
Ni-W/B4The preparation method of C nano composite film coating sample 2, sample 3, sample 4, sample 5, sample 6, includes the following steps.
(1) pre-treatment of matrix:Steel disc is finally carried out using sand paper polishing derusting then using oil removing is cleaned by ultrasonic
Acid-wash activation;The solution each group that oil removing is carried out to matrix is divided into:Sodium hydroxide 50g/L, sodium carbonate 40g/L, sodium phosphate 40g/L,
OP-10 emulsifiers 5ml/L, temperature 70 C, time 10min;Acid-wash activation:With the dilute sulfuric acid of 1mol/L, carried out under room temperature, the time
For 30s.
(2) preparation of electroplate liquid:Ni-W/B4C composite plating bath each groups are divided into:Trisodium citrate 0.5mol/L, sodium tungstate
0.14mol/L, sodium bromide 0.15mol/L, ammonium chloride 0.5mol/L, surfactant 0.1g/L, B4C nano particle dosage is distinguished
For 1,2,3,4,5g/L;After the completion of electroplate liquid is prepared, mechanical agitation 30min is carried out to it first, is then stirred by ultrasonic
30min makes nano particle uniformly and stably disperse in the plating solution.
(3) electrodeposition process:The matrix of pre-treatment is put into prepared electroplate liquid and carries out electro-deposition;In deposition process
Control 75 DEG C of temperature, pH7.5, current density 5A/dm2;Applying pulse power supply and ultrasonic generator are connected, it is auxiliary to proceed by ultrasound
Help pulse electrodeposition;Ultrasonic cleaning processing is carried out using ethyl alcohol and pure water after the completion of plating, obtains finished product;Ultrasonic wave added pulse electricity
Technological parameter during plating is:Pulse frequency is 1000Hz, duty ratio 0.8, ultrasonic power 100W, time 60min,
Magnetic agitation speed is 200rmp;Experimental provision schematic diagram is as shown in Fig. 1.
Experimental example
BS-SEM, micro-hardness testing, polarization test, friction testing are measured the comprehensive performance of plated film;Experimental result table
B under the conditions of bright ultrasonic wave added4C is dispersed in Ni-W plated films, effectively improves coated surface pattern, has refined crystal grain ruler
It is very little.The Ni-W/B of preparation4C nano composite film coating has excellent corrosion-resistant, wear-resisting property, and improves the aobvious of composite material
Microhardness.
(1) coated surface pattern.
The surface topography that plated film is observed using JSM-7500F types scanning electron microscope (SEM), is as a result shown in attached drawing 3, compound
Plated film section BS-SEM figures are shown in attached drawing 4.
(a) is the surface microscopic topographic figure of sample 1 in Fig. 2, as shown, being not added with B4The Ni-W of C nano particle preparation
For coating without apparent crystal boundary, coating surface is coarse and uneven;With B4The addition of C nano particle, the Ni-W/B of preparation4C nano is multiple
Closing the surface topography of plated film (figure (b)-(f)) gradually becomes uniform, fine and close, and crystal boundary disappears, and coated surface becomes more smooth light
It is sliding;It can intuitively be observed from figure (c), 3 composite film coating of sample prepared under this condition has minimum cell configuration, and
Without apparent appearance of reuniting;Fig. 4 is respectively the section BS-SEM figures of 3 composite film coating material of sample 1 and sample;By figure (a) it is found that not
Add B4The Ni-W coating of C nano particle shows coarse and uneven, and schemes the Ni-W-B in (b)4C Surface flat smooth;It is above-mentioned
As a result illustrate B4C nano particle increases the compactness and homogenieity of composite film coating so that coated surface pattern dense uniform.
(2) plated film element composition and content.
The element composition and content that test compound plated film is analyzed by INCA energy disperse spectroscopies (EDS), the results are shown in Table 1.
Fig. 4 is that the EDS elements of sample 3 form scanning figure, as seen from the figure, B4C successes deposit in coating, and point
Cloth is uniform;As shown in table 1, with B4The increase of C nano particle content in the plating solution, the B deposited in coating4C content also gradually increases
Add.
(3) plated film crystal structure and size.
Using XPert PRO MPD types X-ray diffractometers (XRD), with Cu K α radiations, scanning range is 20-80 degree, is ground
The crystal structure and crystallite dimension for studying carefully analysis composite film coating, are as a result shown in attached drawing 5 and table 2.
The Ni-W/B shown in fig. 5 prepared for the embodiment of the present invention4The XRD spectra of C nano composite film coating, analysis it is found that
Add B4After C nano particle, the absorption peak of Ni-W coating is substantially reduced;It can be seen that in conjunction with table 2, nanometer B4C particles are in electro-deposition
Cheng Zhong can effectively inhibit the growth of composite deposite structure cell, as the B in electroplate liquid4When C granule densities are 2g/L, it is formed by plating
Film crystallite dimension is 12nm, far smaller than the crystallite dimension 30nm of Ni-W coating;This also illustrates B4C can effectively reduce coating
Crystallite dimension improves the pattern of coating, this also matches with SEM results.
(4) micro-hardness testing.
By the microhardness of DUH-W20 microhardness tester test compound plated films, load as 100g, time 10s,
As a result see attached drawing 6;As seen from the figure, the microhardness of Ni-W coating is 550HV or so, Ni-W- (2g/L) B4The microhardness of C is
1180HV or so;Obviously, by adulterating B in coating4C nano particle can effectively improve the microhardness of coating.
(5) corrosion resistance is tested.
By using the corrosion resistance of the prepared composite film coating of CorrTest-310 type electrochemical workstations research, make
With typical three-electrode system, wherein working electrode is No. 45 carbon steels for being plated with the nano combined plated films of Ni-W/B4C, significant surface
Product is 15mm × 25mm, and auxiliary electrode is platinum electrode, and reference electrode is saturated calomel electrode (SEM), and corrosive medium is 3.5% chlorine
Change sodium solution, as a result sees attached drawing 7 and table 3.
By Fig. 7 and table 3 it is found that the corrosion potential of composite film coating is by -0.49V up to -0.36V, corrosion electric current density from
3.69μA/cm2It is minimum to be down to 0.21 μ A/cm2, corrosion rate is down to 0.002357mm/a by 0.04344mm/a;Show in Ni-
B is added in W coating4C nano particle can significantly improve the corrosion resistance of coating.
(6) wear-resisting test.
By the East China friction coefficient of MS-T3000 spin friction instrument test compound plated films, load 10N, rotating speed is
As a result 300r/min, testing time 30min are shown in attached drawing 8 and attached drawing 9;(a) is gained sample 1 in embodiment 1 in wherein Fig. 9,
(b) it is gained sample 3 in embodiment 3;By Fig. 8 and Fig. 9 it is found that the Ni-W-B prepared4The friction coefficient of C composite film coatings is obviously low
The wear scar width of coated surface narrows after Ni-W coating, frictional experiment, and Wear track depth reduces.
Claims (2)
1. a kind of pulse electrodeposition Ni-W/B4The preparation method of C nano composite film coating includes the following steps:(1) steel disc matrix is pre-
The processes such as processing, including polishing derusting, ultrasonic cleaning oil removing, surface active:By steel disc using sand paper polishing derusting, then utilize
It is cleaned by ultrasonic oil removing, finally carries out acid-wash activation;The solution each group that oil removing is carried out to matrix is divided into:Sodium hydroxide 50g/L, carbonic acid
Sodium 40g/L, sodium phosphate 40g/L, OP-10 emulsifier 5ml/L, temperature 70 C, time 10min;Acid-wash activation:It is dilute with 1mol/L
Sulfuric acid carries out under room temperature, time 30s;(2) configuration of electroplate liquid, Ni-W/B4C composite plating bath each groups are divided into:Trisodium citrate
0.5mol/L, sodium tungstate 0.14mol/L, sodium bromide 0.15mol/L, ammonium chloride 0.5mol/L, surfactant 0.1g/L, B4C
Nano particle(0g/L、1g/L、2g/L、3g/L、4g/L、5g/L);After the completion of electroplate liquid is prepared, magnetic force is carried out to it first and is stirred
30min is mixed, ultrasonic agitation 30min is then carried out, nano particle is made uniformly and stably to disperse in the plating solution;(3) electrodeposition process:
Pretreated matrix is put into prepared electroplate liquid and carries out electro-deposition;70-75 DEG C of temperature, pH7.0- are controlled in the process
7.5, current density 5A/dm2;Bath temperature is controlled using temperature control system, connects applying pulse power supply, opens magnetic agitation
Device proceeds by pulse electrodeposition;Technological parameter during pulse plating is:Pulse frequency is 800Hz, duty ratio 0.8,
Time is 60min, magnetic agitation speed 200rmp;(4) post-processing of plating piece:Ethyl alcohol, pure water are used successively to plating piece surface
It is cleaned by ultrasonic.
2. the pulse electrodeposition Ni-W/B that the method as described in claim 1 is prepared4C nano composite film coating.
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Cited By (6)
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CN112410852A (en) * | 2020-10-30 | 2021-02-26 | 中冶赛迪技术研究中心有限公司 | Nano composite electroplating equipment and electroplating process |
CN112894639A (en) * | 2021-03-01 | 2021-06-04 | 长沙理工大学 | Method for preparing electroplated diamond grinding wheel |
CN113061945A (en) * | 2021-03-16 | 2021-07-02 | 西南石油大学 | Pulse electrodeposition Ni-B/B4Preparation method of C nano composite coating |
CN113106521A (en) * | 2021-04-14 | 2021-07-13 | 西南石油大学 | Ni-W-ZrC microcrystal coating, plating solution and preparation method thereof |
CN113943957A (en) * | 2021-11-29 | 2022-01-18 | 西南石油大学 | Ni-W-WS2Nano composite coating and preparation method thereof |
CN115216626A (en) * | 2022-06-10 | 2022-10-21 | 杭州航天电子技术有限公司 | Ultrasonic nickel leaching device and method for aluminum alloy surface treatment |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112410852A (en) * | 2020-10-30 | 2021-02-26 | 中冶赛迪技术研究中心有限公司 | Nano composite electroplating equipment and electroplating process |
CN112894639A (en) * | 2021-03-01 | 2021-06-04 | 长沙理工大学 | Method for preparing electroplated diamond grinding wheel |
CN113061945A (en) * | 2021-03-16 | 2021-07-02 | 西南石油大学 | Pulse electrodeposition Ni-B/B4Preparation method of C nano composite coating |
CN113106521A (en) * | 2021-04-14 | 2021-07-13 | 西南石油大学 | Ni-W-ZrC microcrystal coating, plating solution and preparation method thereof |
CN113106521B (en) * | 2021-04-14 | 2022-05-20 | 西南石油大学 | Ni-W-ZrC microcrystal coating, plating solution and preparation method thereof |
CN113943957A (en) * | 2021-11-29 | 2022-01-18 | 西南石油大学 | Ni-W-WS2Nano composite coating and preparation method thereof |
CN115216626A (en) * | 2022-06-10 | 2022-10-21 | 杭州航天电子技术有限公司 | Ultrasonic nickel leaching device and method for aluminum alloy surface treatment |
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