CN106048610A - Method for preparing nano-ceramic coating interface on surface of ABS product - Google Patents
Method for preparing nano-ceramic coating interface on surface of ABS product Download PDFInfo
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- CN106048610A CN106048610A CN201610666401.XA CN201610666401A CN106048610A CN 106048610 A CN106048610 A CN 106048610A CN 201610666401 A CN201610666401 A CN 201610666401A CN 106048610 A CN106048610 A CN 106048610A
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- abs
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/36—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including layers graded in composition or physical properties
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention discloses a method for preparing a nano-ceramic coating interface on the surface of an ABS product. The method comprises the following steps: carrying out surface degreasing, surface hydrophilic treatment, surface roughening treatment, surface neutralizing treatment, pre-impregnating treatment, palladium immersion, peptizing, alkaline nickel plating, cleaning, drying, gas plasma cleaning pre-treatment and metal plasma high-energy injection pre-treatment; and after metal ion high-energy pre-treatment is completed, gradually and slowly reducing ion energy, and continuously and slowly charging a reaction gas until an interface blend layer continuously transiting to ceramic from metal is formed. According to the method disclosed by the invention, the surface of the ABS product is treated by virtue of the advantages of a metal plasma source, the defect of no high-temperature resistance of ABS plastic is overcome with the adoption of the method of alkaline low-temperature nickel plating, and then metal epitaxial growth and film coating, and metal film surface ceramization are carried out to complete preparation for a high-hardness ceramic coating with a high binding force on the ABS product; and meanwhile, the appearance needs of smoothness and the like of the surface ceramic coating can be met.
Description
Technical field
The present invention relates to a kind of method preparing nano ceramic coat interface at ABS product surface.
Background technology
Along with the development of society, pottery occupies an important position in a lot of fields, and is recognized by a lot of consumers
Can, the use environment of pottery is sufficiently complex, in the environment of especially having high temperature, greatly reduces service life, increases cost,
So traditional ceramic material cannot meet day by day harsh job requirement, exploitation has high temperature resistant, corrosion-resistant, anti-impact
Hit, resist tired and anti abrasive advanced composite material (ACM) to have become as the important topic of material science research.
At present, deposition technique based on vacuum is generally used to form the thin layer of conductive coating or ceramic material.Such as, exist
Electricity device in photovoltaic art often deposits the thin layer of transparent material such as tin indium oxide.Need the thinnest coating of deposition with
Obtain the electric current of more preferable optical transparence and across-layer.Some methods depositing this type coating used at present include chemistry gas
Deposition (CVD), physical vapour deposition (PVD) (PVD), laser assisted pyrolytic deposition and electro beam physics vapour deposition mutually.
ABS is acrylonitrile, butadiene and cinnamic terpolymer, and A represents acrylonitrile, and B represents butadiene, and S represents
Styrene.But, through actually used discovery: ABS substrate plastic cement products, not sulfuric acid corrosion resistant, meet sulphuric acid and rupture with regard to comminuted,
And ABS plastic can not be high temperature resistant, poor to the affinity of ceramic coating, how on plastic material shell, to prepare high-bond
High hard ceramic coating just become a problem in the urgent need to address.
Summary of the invention
It is an object of the invention to overcome weak point of the prior art, it is provided that one prepares nanometer on ABS material surface
The method at ceramic coating interface, to realize to prepare on plastic material shell the high hard ceramic coating of high-bond.
It is an object of the invention to be achieved through the following technical solutions:
A kind of method preparing nano ceramic coat interface at ABS product surface, comprises the following steps,
Oils and fats is removed on S1: surface, removes the greasy dirt that ABS goods attach;
S2: surface hydrophilic processes, abundant moistening ABS product surface;
S3: surface coarsening processes;
S4: surface neutralisation treatment;
S5: pre-preg, the ABS goods after neutralizing immerse in predip solution, and room temperature soaks 2min;
S6: heavy palladium, utilizes colloid palladium activation method palladium ion is adsorbed in surface of the work and is reduced into active palladium metal;
S7: dispergation, the ABS goods after being processed by above-mentioned heavy palladium are in the solution containing chemical pure hydrochloric acid 80~120mL/L
Dispergation processes;
S8: alkalescence nickel plating, the ABS goods after being processed by above-mentioned heavy palladium are containing NiSO422~30g/L, NaH2PO2·
H2O 22~30g/L, NH4Cl 20~30g/L, sodium citrate 10~15g/L mixed solution in carry out nickel chemical plating technology, molten
It is 40~60 DEG C that liquid temp controls;
S9: clean, uses ultrasonic wave water washing, and temperature controls between 50~60 DEG C, and scavenging period is 10min;
S10: dry;
S11: gaseous plasma cleans pretreatment, utilizes source gas plasma that ABS product surface is carried out place
Reason;
S12: metallic plasma high energy ion implantation pretreatment, carries out energetic ion injection process in the interface of ABS goods,
And then in ABS goods near surface about 200nm, form implanted layer;
S13: after metal ion high energy pretreatment is complete, the most slowly reduces ion energy, and is slowly introducing anti-continuously
Answer gas, until being formed by the interface blended layer of metal to pottery continuous transition.
The purpose of step S3 roughening treatment is to improve the surface hydrophilicity of ABS goods and form suitable roughness, to protect
Demonstrate,prove its coating and have good adhesive force.
Step S4 neutralisation treatment uses 80~120mL/L hydrochloric acid to be cleaned up by the Cr VI remaining in product surface, with
Exempt to pollute activator.
The preimpregnation of step S5 can strengthen the stability of activator, prevents activator to be diluted with water and hydrolyzes.
Step S6 utilizes colloid palladium activation method palladium ion is adsorbed in surface of the work and is reduced into active palladium metal, to follow-up
Chemical nickel plating plays catalytic action.
After palladium activation, the pallamine microgranule of ABS product surface absorption does not play catalytic action, because of palladium microgranule ambient absorption
There is the stannum hydrolysis glue-line of stable colloidal state effect.Palladium microgranule to be made plays the effect of catalytic active center, it is necessary to product surface
Carry out dispergation process.
One as such scheme is optional, also includes Jiao before cleaning with step S9 after described step S8 alkalescence nickel plating
Phosphate copper plating treatment, particularly as follows:
Pyrophosphate system is used to plate one layer of copper at ABS product surface.
Chemical Ni-plating layer is easily passivated, and directly is often being difficult to cover completely to its starting stage carrying out acidic copper-plating of bright
Lid, the dispersibility of pyrophosphate copper plating liquid and covering power are preferable, use pyrophosphate system first to plate a thin layer copper and are conducive to
Solve this problem.
Concrete, described employing pyrophosphate system at ABS product surface plating a thin layer copper particularly as follows: by above-mentioned ABS
Goods are containing Cu2P2O7·3H2O 50~70g/L, K4P2O7·3H2O 320~360g/L, mixing of ammonium citrate 20~25g/L
Close solution and carry out pyrophosphate copper plating process.
One as such scheme is optional, also includes at acidiccopper plating after described pyrophosphate copper plating processes
Reason, particularly as follows: by above-mentioned ABS goods containing CuSO4200~220g/L, chemical pure H2SO460~80g/L, chemical pure salt
The mixed solution of acid 70~80mg/L carries out acidiccopper plating process.
After copper facing, nickel coating can strengthen the corrosion resistance of coating again, preferred accordingly, as one, at described acidiccopper plating
Nickel Plating Treatment is also included after process, particularly as follows: by above-mentioned ABS goods containing NiSO4220~300g/L, NiCl235~
75g/L、H3BO3The mixed solution of 40~48g/L carries out Nickel Plating Treatment.
One as such scheme is optional, also includes that chromium plating processes after described acidiccopper plating processes, particularly as follows:
By above-mentioned ABS goods containing Cr2O3200~280g/L, chemical pure H2SO4The mixed solution of 2.0~2.8g/L carries out chromium plating
Process.
Chromium plating can strengthen hardness and the wearability of overall coating, and provides good matrix for Vacuum Deposition zirconium nitride.
Concrete, what described step S12 energetic ion injection processed concretely comprises the following steps:
ABS goods to be processed are arranged in columnar target origin system, under being passed through reacting gas, carry out HPPMS put
Electricity;
HPPMS electric discharge makes splash go out metal ion, and the cylinder interior that the atom of the non-ionization of sputter material limits, repeatedly
Sputtering and ionization, the metal ion of ionization is then drawn by extraction grid and is accelerated;
By the control of accelerating potential, it is achieved the matrix of the ion pair ABS goods of different-energy and coating carry out injecting or
Deposition.
HPPMS (abbreviation of High Power Puls Magnetron Sputtering, high energy pulse magnetron sputtering)
It is that a kind of peak power exceedes 2 magnitudes of mean power, the pulsed sputter technology of sputtering target material atom high ionization, by electricity etc.
Gas ions generating means short but extremely have the pulse of energy achieve coated microgranules before magnetron high from
Sonization density, it is close to reaching 100%.In the case of the sufficiently high pulse of energy, electric current quickly increases so that quickly experience
Glow discharge and the plasmoid of big electric current arc discharge (Arc) so that can be formed before magnetron and have very
The stable plasma of high carrier density.The present invention uses cylindrical target source structure to design, due to cylindrical shape inner periphery
Surface area (plane of i.e. discharging) is much larger than line removal cross-section area, and the ion after simultaneously drawing will be no longer by target surface nagative potential
Attraction, deposition efficiency is greatly improved.
The present invention has the following advantages and beneficial effect compared to existing technology:
1, the present invention utilizes the advantage of metal plasma source, processes ABS product surface, uses alkaline low-temperature plating
The method of nickel overcome ABS plastic can not resistant to elevated temperatures defect, and then carry out metal epitaxial growth plated film and metallic film surface pottery
Change, complete to prepare the high hard ceramic coating of high-bond on ABS goods, the fineness of surface ceramic coat can be met simultaneously
Etc. outward appearance demand, preparation has the potteries such as TiN, TiC, TiCN, DLC of the performance such as gorgeous color and high strong hardness, wear-resisting anti-corruption concurrently
Coating, meets the performance evaluatings such as film-substrate cohesion, surface smoothness, hardness, wear-and corrosion-resistant.
2, the present invention is by between pottery and metal level, preparation is without the transition zone at interface, and i.e. continuous print transition zone, whole
Plasma treatment procedure is uninterrupted, and all operations all slow quiet runs during plasma opens so can shape
Become by metal to pottery continuous print transition, effectively ensure adhesion.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
The ABS goods of the present invention include plastic workpiece or the product that the materials such as all kinds of ABS make.
The method preparing nano ceramic coat interface at above-mentioned ABS product surface comprises the steps:
(1) oils and fats is removed on surface: at Na3PO4、Na2CO3With cleaning treatment in NaOH mixed solution.In this step, mix molten
In liquid, each component concentration proportioning in different embodiments is shown in Table one:
Table one
(2) surface hydrophilic processes: at chemical pure H2SO4, abundant wetting articles surface in sodium soap mixed solution.This step
In Zhou, chemical pure H2SO4It is shown in Table two with sodium soap concentration proportioning in different embodiments:
Table two
(3) surface coarsening processes: at chemical pure H2SO4、Cr2O3Mixed solution is carried out.In this step, chemical pure H2SO4、
Cr2O3In concentration proportioning in different embodiments be shown in Table three:
Table three
(4) surface neutralisation treatment:: the plastic cement after being processed by surface coarsening is put in hydrochloric acid solution and is carried out.In this step, salt
Acid solution concentration proportioning in different embodiments is shown in Table four:
Table four
(5) pre-preg: immersed by the ABS goods after neutralisation treatment in predip solution, in this step, predip solution uses
Hydrochloric acid and the mixed solution of pre dip salt, hydrochloric acid and pre dip salt concentration proportioning in different embodiments are shown in Table five:
Table five
(6) heavy palladium processes: containing palladium activator, pre dip salt, chemical pure hydrochloric acid mixed solution in carry out, this step
In, in mixed solution, each component concentration proportioning in different embodiments is shown in Table six:
Table six
(7) dispergation processes: carrying out in chemical pure hydrochloric acid solution, in this step, chemical pure hydrochloric acid is in different embodiments
Concentration proportioning be shown in Table seven:
Table seven
(8) alkalescence Nickel Plating Treatment: containing NiSO4、NaH2PO2·H2O、NH4Cl, sodium citrate mixed solution in enter
OK, in this step, in mixed solution, each component concentration proportioning in different embodiments is shown in Table eight:
Table eight
(9) pyrophosphate copper plating processes: containing Cu2P2O7·3H2O、K4P2O7·3H2O, the mixed solution of ammonium citrate
In carry out, in this step, in mixed solution, each component concentration proportioning in different embodiments is shown in Table nine:
Table nine
(10) acidiccopper plating processes: containing CuSO4, chemical pure H2SO4, chemical pure hydrochloric acid mixed solution in carry out,
In this step, in mixed solution, each component concentration proportioning in different embodiments is shown in Table ten:
Table ten
(11) Nickel Plating Treatment: containing NiSO4、NiCl2、H3BO3Mixed solution in carry out, in this step, mixed solution
In each component concentration proportioning in different embodiments be shown in Table 11:
Table 11
(12) chromium plating processes: containing Cr2O3, chemical pure H2SO4Mixed solution in carry out, in this step, mixed solution
In each component concentration proportioning in different embodiments be shown in Table 12:
Table 12
(12) clean: using ultrasonic wave water washing, temperature controls between 50~60 DEG C, and scavenging period is 10min;
(13) dry: the moisture residuing in product surface can affect quality of coating, as easy to fall off in plated film or produce green mold etc..
Therefore needing to use to force stoving process, temperature is 65 DEG C, and the time is 40min.
(14) gaseous plasma cleans pretreatment: residuing in the impurity such as the oxide of product surface, Organic substance can affect
Film-substrate cohesion, need to utilize source gas plasma to be carried out ABS product surface processing, on the one hand cleaning oxide on surface
And Organic substance, on the other hand activating surface;
(15) metallic plasma high energy ion implantation pretreatment: carry out energetic ion injection process in the interface of ABS goods,
And then in ABS goods near surface about 200nm, form implanted layer, particularly as follows:
ABS goods to be processed are arranged in columnar target origin system, under being passed through reacting gas, carry out HPPMS put
Electricity;
HPPMS electric discharge makes splash go out metal ion, and the cylinder interior that the atom of the non-ionization of sputter material limits, repeatedly
Sputtering and ionization, the metal ion of ionization is then drawn by extraction grid and is accelerated;
By the control of accelerating potential, it is achieved the matrix of the ion pair ABS goods of different-energy and coating carry out injecting or
Deposition.
(16), after the pretreatment of metal ion high energy is complete, the most slowly reduces ion energy, and be slowly introducing anti-continuously
Answer gas, until being formed by the interface blended layer of metal to pottery continuous transition.
Owing to cylindrical shape inner circumferential surface long-pending (plane of i.e. discharging) is much larger than line removal cross-section area, after drawing simultaneously
Ion will no longer be attracted by target surface nagative potential, and deposition efficiency is greatly improved.
The method of the employing present invention compared with prior art, is tied after ABS product surface prepares nano ceramic coat interface
Fruit is as shown in table 13:
Table 13
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (7)
1. the method preparing nano ceramic coat interface at ABS product surface, it is characterised in that comprise the following steps,
Oils and fats is removed on S1: surface, removes the greasy dirt that ABS goods attach;
S2: surface hydrophilic processes, abundant moistening ABS product surface;
S3: surface coarsening processes;
S4: surface neutralisation treatment;
S5: pre-preg, the ABS goods after neutralizing immerse in predip solution, and room temperature soaks 2min;
S6: heavy palladium, utilizes colloid palladium activation method palladium ion is adsorbed in surface of the work and is reduced into active palladium metal;
S7: dispergation, the ABS goods dispergation in the solution containing chemical pure hydrochloric acid 80~120mL/L after above-mentioned heavy palladium is processed
Process;
S8: alkalescence nickel plating, the ABS goods after being processed by above-mentioned heavy palladium are containing NiSO422~30g/L, NaH2PO2·H2O 22
~30g/L, NH4Cl 20~30g/L, sodium citrate 10~15g/L mixed solution in carry out nickel chemical plating technology, solution temperature
Degree control is 40~60 DEG C;
S9: clean, uses ultrasonic wave water washing, and temperature controls between 50~60 DEG C, and scavenging period is 10min;
S10: dry;
S11: gaseous plasma cleans pretreatment, utilizes source gas plasma to be carried out ABS product surface processing;
S12: metallic plasma high energy ion implantation pretreatment, carries out energetic ion injection process in the interface of ABS goods, and then
Implanted layer is formed in ABS goods near surface about 200nm;
S13: after metal ion high energy pretreatment is complete, the most slowly reduces ion energy, and is slowly introducing reaction gas continuously
Body, until being formed by the interface blended layer of metal to pottery continuous transition.
The method preparing nano ceramic coat interface at ABS product surface the most according to claim 1, it is characterised in that
Also include that pyrophosphate copper plating processes before cleaning with step S9 after described step S8 alkalescence nickel plating, particularly as follows:
Pyrophosphate system is used to plate one layer of copper at ABS product surface.
The method preparing nano ceramic coat interface at ABS product surface the most according to claim 1, it is characterised in that
Described employing pyrophosphate system at ABS product surface one layer of copper of plating particularly as follows: by above-mentioned ABS goods containing Cu2P2O7·
3H2O 50~70g/L, K4P2O7·3H2O 320~360g/L, the mixed solution of ammonium citrate 20~25g/L carries out pyrophosphate
Copper plating treatment.
The method preparing nano ceramic coat interface at ABS product surface the most according to claim 2, it is characterised in that
After described pyrophosphate copper plating processes, also include that acidiccopper plating processes, particularly as follows: contained by above-mentioned ABS goods
CuSO4200~220g/L, chemical pure H2SO460~80g/L, the mixed solution of chemical pure hydrochloric acid 70~80mg/L carries out sulphuric acid
Salt copper plating treatment.
The method preparing nano ceramic coat interface at ABS product surface the most according to claim 4, it is characterised in that
Nickel Plating Treatment is also included after described acidiccopper plating processes, particularly as follows: by above-mentioned ABS goods containing NiSO4220~
300g/L、NiCl235~75g/L, H3BO3The mixed solution of 40~48g/L carries out Nickel Plating Treatment.
The method preparing nano ceramic coat interface at ABS product surface the most according to claim 2, it is characterised in that
After described acidiccopper plating processes, also include that chromium plating processes, particularly as follows: by above-mentioned ABS goods containing Cr2O3200~
280g/L, chemical pure H2SO4The mixed solution of 2.0~2.8g/L carries out chromium plating process.
7. according to the method preparing nano ceramic coat interface at ABS product surface described in any one of claim 1~6, its
Being characterised by, what described step S12 energetic ion injection processed concretely comprises the following steps:
ABS goods to be processed are arranged in columnar target origin system, under being passed through reacting gas, carry out HPPMS electric discharge;
HPPMS electric discharge makes splash go out metal ion, and the cylinder interior that the atom of the non-ionization of sputter material limits, and repeatedly sputters
And ionization, the metal ion of ionization is then drawn by extraction grid and is accelerated;
By the control of accelerating potential, it is achieved the matrix of the ion pair ABS goods of different-energy and coating carry out injecting or depositing.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108588651A (en) * | 2017-12-29 | 2018-09-28 | 深圳市旺鑫精密工业有限公司 | A kind of pulsed sputter coating process |
CN109160501A (en) * | 2018-11-06 | 2019-01-08 | 中山大学 | The method for preparing transition metal phosphide with microwave plasma CVD |
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CN1256717A (en) * | 1997-05-21 | 2000-06-14 | 瑞士铝业技术及管理有限公司 | Packaging material |
CN102337571A (en) * | 2011-11-03 | 2012-02-01 | 厦门建霖工业有限公司 | Method for electroplating plastic base material |
CN103938166A (en) * | 2013-01-23 | 2014-07-23 | 香港生产力促进局 | High-energy pulse-type magnetron sputtering method and magnetron sputtering device |
CN104626448A (en) * | 2015-01-15 | 2015-05-20 | 温兵 | Manufacturing process of shell |
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CN1150180A (en) * | 1995-11-15 | 1997-05-21 | 哈尔滨工业大学 | Plasma immersion ion implantation apparatus for material surface modifying |
CN1256717A (en) * | 1997-05-21 | 2000-06-14 | 瑞士铝业技术及管理有限公司 | Packaging material |
CN102337571A (en) * | 2011-11-03 | 2012-02-01 | 厦门建霖工业有限公司 | Method for electroplating plastic base material |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108588651A (en) * | 2017-12-29 | 2018-09-28 | 深圳市旺鑫精密工业有限公司 | A kind of pulsed sputter coating process |
CN109160501A (en) * | 2018-11-06 | 2019-01-08 | 中山大学 | The method for preparing transition metal phosphide with microwave plasma CVD |
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