CN106048610B - A method of nano ceramic coat interface is prepared in ABS product surface - Google Patents

A method of nano ceramic coat interface is prepared in ABS product surface Download PDF

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CN106048610B
CN106048610B CN201610666401.XA CN201610666401A CN106048610B CN 106048610 B CN106048610 B CN 106048610B CN 201610666401 A CN201610666401 A CN 201610666401A CN 106048610 B CN106048610 B CN 106048610B
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abs product
abs
ion
product surface
plating
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CN106048610A (en
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陈有贤
陈杰锋
谭平
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DONGGUAN WANGXIN PRECISION INDUSTRY Co.,Ltd.
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SHENZHEN WANGXIN PLASTIC TECHNOLOGY PRODUCT Co Ltd
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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
    • 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

Abstract

The invention discloses a kind of methods for preparing nano ceramic coat interface in ABS product surface, the following steps are included: after surface degreasing, surface hydrophilic processing, surface roughening treatment, surface neutralisation treatment, pre-preg, heavy palladium, dispergation, alkaline nickel plating, cleaning, drying, gaseous plasma cleaning pretreatment, the pretreatment of metallic plasma high energy ion implantation, the pretreatment of metal ion high energy finish, gradually slowly reduce ion energy, and it is continuously slowly introducing reaction gas, until forming the interface blended layer by metal to ceramic continuous transition.The present invention utilizes the advantages of metal plasma source, ABS product surface is handled, overcome ABS plastic cannot defect resistant to high temperature using the method for alkaline low-temperature nickel plating, and then carry out metal epitaxial growth plated film and metallic film surface ceramic, complete the hard ceramic coating of height that high-bond is prepared on ABS product, while the appearances demand such as finish that can satisfy surface ceramic coat.

Description

A method of nano ceramic coat interface is prepared in ABS product surface
Technical field
The present invention relates to a kind of methods for preparing nano ceramic coat interface in ABS product surface.
Background technique
With the development of society, ceramics occupy an important position in many fields, and recognized by many consumers Can, ceramic use environment is sufficiently complex, and in the environment of especially there is high temperature, service life is greatly reduced, increases cost, So traditional ceramic material can no longer meet increasingly harsh job requirement, exploitation has high temperature resistant, corrosion-resistant, anti-impact The important topic hit, tired and anti abrasive advanced composite material (ACM) is resisted to have become material science research.
Currently, generalling use the deposition technique based on vacuum to form the thin layer of conductive coating or ceramic material.For example, The thin layer of transparent material such as tin indium oxide is often deposited in electricity device in photovoltaic art.Need to deposit as thin as possible coating with Obtain better optical transparence and the electric current across layer.Some currently used methods for depositing this type coating include chemical gas Mutually deposition (CVD), physical vapour deposition (PVD) (PVD), laser assisted pyrolytic deposition and electro beam physics vapour deposition.
ABS is the terpolymer of acrylonitrile, butadiene and styrene, and A represents acrylonitrile, and B represents butadiene, and S is represented Styrene.However, by actual use discovery: ABS substrate plastic cement products, not sulfuric acid corrosion resistant meet sulfuric acid with regard to comminuted rupture, And ABS plastic is unable to high temperature resistant, and it is poor to the affinity of ceramic coating, how on plastic material shell to prepare high-bond The hard ceramic coating of height just become a problem in the urgent need to address.
Summary of the invention
The purpose of the present invention is overcoming shortcoming in the prior art, provide a kind of in ABS material surface preparation nanometer The method at ceramic coating interface, to realize the hard ceramic coating of height that can prepare high-bond on plastic material shell.
The purpose of the present invention is achieved through the following technical solutions:
A method of nano ceramic coat interface being prepared in ABS product surface, is included the following steps,
S1: surface degreasing removes the greasy dirt that ABS product attaches；
S2: surface hydrophilic processing sufficiently soaks ABS product surface；
S3: surface roughening treatment；
S4: surface neutralisation treatment；
S5: pre-preg immerses the ABS product after neutralization in predip solution, room temperature, impregnates 2min；
S6: palladium ion is adsorbed in workpiece surface using colloid palladium activation method and is reduced into active palladium metal by heavy palladium；
S7: dispergation, by above-mentioned heavy palladium treated ABS product in the solution containing 80~120mL/L of chemical pure hydrochloric acid Dispergation processing；
S8: alkaline nickel plating, by above-mentioned heavy palladium, treated that ABS product is containing NiSO422~30g/L, NaH2PO2· H222~30g/L of O, NH420~30g/L of Cl, 10~15g/L of sodium citrate mixed solution in carry out nickel chemical plating technology, it is molten The control of liquid temperature is 40~60 DEG C；
S9: cleaning, using ultrasonic wave water washing, temperature controls the scavenging period 10min between 50~60 DEG C；
S10: drying；
S11: gaseous plasma cleaning pretreatment carries out at cleaning ABS product surface using source gas plasma Reason；
S12: the pretreatment of metallic plasma high energy ion implantation carries out energetic ion injection processing in the interface of ABS product, And then implanted layer is formed in ABS product near surface 200nm；
S13: after the pretreatment of metal ion high energy finishes, gradually slowly reducing ion energy, and is continuously slowly introducing anti- Gas is answered, until forming the interface blended layer by metal to ceramic continuous transition.
The purpose of step S3 roughening treatment is to improve the surface hydrophilicity of ABS product and form roughness appropriate, to protect Demonstrate,proving its coating has good adhesive force.
Step S4 neutralisation treatment is cleaned up the Cr VI for remaining in product surface using 80~120mL/L hydrochloric acid, with Exempt to pollute activator.
Step S5 presoaks the stability that can enhance activator, and activator is prevented to be diluted with water and hydrolyze.
Palladium ion is adsorbed in workpiece surface using colloid palladium activation method and is reduced into active palladium metal by step S6, to subsequent Chemical nickel plating plays catalytic action.
After palladium activation, the pallamine particle of ABS product surface absorption does not play catalytic action, because of palladium particle ambient absorption Glue-line is hydrolyzed with the tin for stablizing colloidal state effect.Palladium particle is set to play the effect of catalytic active center, it is necessary to product surface Carry out dispergation processing.
One kind as above scheme is optional, further includes coke before cleaning after the step S8 alkalinity nickel plating with step S9 Phosphate copper plating treatment, specifically:
One layer of copper is plated in ABS product surface using pyrophosphate system.
Chemical Ni-plating layer is easily passivated, and is often difficult to cover completely in the initial stage for directly carrying out it acidic copper-plating of bright Lid, the dispersibility and covering power of pyrophosphate copper plating liquid are preferable, and a thin layer copper is first plated using pyrophosphate system and is conducive to Solve the problems, such as this.
Specifically, described plate a thin layer copper in ABS product surface using pyrophosphate system specifically: by above-mentioned ABS Product is containing Cu2P2O7·3H250~70g/L of O, K4P2O7·3H2320~360g/L's of O, 20~25g/L of ammonium citrate is mixed It closes solution and carries out pyrophosphate copper plating processing.
One kind as above scheme is optional, further includes at acidiccopper plating after pyrophosphate copper plating processing Reason, specifically: above-mentioned ABS product is being contained into CuSO4200~220g/L, the pure H of chemistry2SO460~80g/L, the pure salt of chemistry The mixed solution of 70~80mg/L of acid carries out acidiccopper plating processing.
Nickel coating can enhance the corrosion resistance of coating again after copper facing, therefore, as a preference, in the acidiccopper plating It further include Nickel Plating Treatment after processing, specifically: above-mentioned ABS product is being contained into NiSO4220~300g/L, NiCl235~ 75g/L、H3BO3The mixed solution of 40~48g/L carries out Nickel Plating Treatment.
One kind as above scheme is optional, further includes chromium plating process after acidiccopper plating processing, specifically: Above-mentioned ABS product is being contained into Cr2O3200~280g/L, the pure H of chemistry2SO4The mixed solution of 2.0~2.8g/L carries out chromium plating Processing.
Chromium plating can enhance the hardness and wearability of whole coating, and provide good matrix for Vacuum Deposition zirconium nitride.
Specifically, the specific steps of the step S12 energetic ion injection processing are as follows:
ABS product to be processed is mounted in the system of columnar target source, HPPMS is carried out in the case where being passed through reaction gas and is put Electricity；
HPPMS electric discharge make splash go out metal ion and the non-ionization of sputter material atom limitation cylinder interior, repeatedly Sputtering and ionization, and the metal ion of ionization then passes through extraction grid and draws and accelerate；
By the control of acceleration voltage, realize the matrix of the ion pair ABS product of different-energy and coating carry out injection or Deposition.
HPPMS (abbreviation of High Power Puls Magnetron Sputtering, high energy pulse magnetron sputtering) Be a kind of peak power it is more than 2 magnitudes of mean power, the pulsed sputter technology of sputtering target material atom high ionization, passes through electricity etc. Gas ions generating means short but extremely have the pulse of energy realize coated microgranules before magnetron it is high from Sonization density, it is close to reach 100%.In the case where energy sufficiently high pulse, electric current quickly increases, so that quickly experience The plasmoid of glow discharge and high current arc discharge (Arc), so that can be formed before magnetron has very The stable plasma of high carrier density.The present invention is designed using cylindrical target source structure, due to cylinder-shaped inner periphery Surface area (i.e. electric discharge plane) is much larger than line removal cross-section area, while the ion after extraction will be no longer by target surface negative potential Attraction, deposition efficiency greatly improves.
The present invention have the following advantages that compared with prior art and the utility model has the advantages that
1, the present invention utilizes the advantages of metal plasma source, handles ABS product surface, is plated using alkaline low-temperature The method of nickel overcome ABS plastic cannot defect resistant to high temperature, and then carry out metal epitaxial growth plated film and metallic film surface ceramics Change, completes the hard ceramic coating of height for preparing high-bond on ABS product, while can satisfy the finish of surface ceramic coat Etc. appearances demand, to have both TiN, TiC, TiCN, the DLC of performances such as gorgeous color and high strong hardness, wear-resisting anti-corruption etc. ceramic for preparation Coating meets the performance evaluatings such as film-substrate cohesion, surface smoothness, hardness, wear-and corrosion-resistant.
2, the present invention by ceramics and metal layer between prepare the transition zone without interface, i.e., continuous transition zone, entirely Plasma treatment procedure is uninterrupted, all operation slow quiet runs during plasma opens, in this way can shape , to the continuous transition of ceramics, effectively guarantee binding force at by metal.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
ABS product of the invention includes plastic workpiece made of the materials such as all kinds of ABS or product.
Include the following steps: in the method that above-mentioned ABS product surface prepares nano ceramic coat interface
(1) surface degreasing: in Na3PO4、Na2CO3With cleaning treatment in NaOH mixed solution.In this step, mix molten The concentration proportioning of each component in different embodiments is shown in Table one in liquid:
Table one
(2) surface hydrophilic is handled: in the pure H of chemistry2SO4, abundant wetting articles surface in sodium soap mixed solution.This step In rapid, the pure H of chemistry2SO4Two are shown in Table with the concentration proportioning of sodium soap in different embodiments:
Table two
(3) surface roughening treatment: in the pure H of chemistry2SO4、Cr2O3It is carried out in mixed solution.In this step, the pure H of chemistry2SO4、 Cr2O3In concentration proportioning in different embodiments be shown in Table three:
Table three
(4) surface neutralisation treatment:: the plastic cement after surface roughening treatment is put into hydrochloric acid solution and is carried out.In this step, salt The concentration proportioning of acid solution in different embodiments is shown in Table four:
Table four
(5) pre-preg: the ABS product after neutralisation treatment is immersed in predip solution, and in this step, predip solution is used The concentration proportioning of the mixed solution of hydrochloric acid and pre dip salt, hydrochloric acid and pre dip salt in different embodiments is shown in Table five:
Table five
(6) sink palladium processing: containing palladium activator, pre dip salt, chemical pure hydrochloric acid mixed solution in carry out, this step In, the concentration proportioning of each component in different embodiments is shown in Table six in mixed solution:
Table six
(7) dispergation is handled: being carried 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) alkaline Nickel Plating Treatment: containing NiSO4、NaH2PO2·H2O、NH4Cl, sodium citrate mixed solution in into It goes, in this step, the concentration proportioning of each component in different embodiments is shown in Table eight in mixed solution:
Table eight
(9) pyrophosphate copper plating is handled: containing Cu2P2O7·3H2O、K4P2O7·3H2O, the mixed solution of ammonium citrate Middle progress, in this step, the concentration proportioning of each component in different embodiments is shown in Table nine in mixed solution:
Table nine
(10) acidiccopper plating is handled: containing CuSO4, the pure H of chemistry2SO4, chemical pure hydrochloric acid mixed solution in carry out, In this step, the concentration proportioning of each component in different embodiments is shown in Table ten in mixed solution:
Table ten
(11) Nickel Plating Treatment: containing NiSO4、NiCl2、H3BO3Mixed solution in carry out, in this step, mixed solution The concentration proportioning of middle each component in different embodiments is shown in Table 11:
Table 11
(12) chromium plating process: containing Cr2O3, the pure H of chemistry2SO4Mixed solution in carry out, in this step, mixed solution The concentration proportioning of middle each component in different embodiments is shown in Table 12:
Table 12
(12) it cleans: using ultrasonic wave water washing, temperature controls the scavenging period 10min between 50~60 DEG C；
(13) dry: the moisture for remaining on product surface will affect quality of coating, such as plated film is easy to fall off or generates green mold. Therefore need to be using stoving process to be forced, temperature is 65 DEG C, time 40min.
(14) gaseous plasma cleaning pretreatment: remaining on the impurity such as oxide, the organic matter of product surface will affect Film-substrate cohesion need to start the cleaning processing ABS product surface using source gas plasma, on the one hand clear up oxide on surface And organic matter, another aspect activating surface；
(15) metallic plasma high energy ion implantation pre-processes: energetic ion injection processing is carried out in the interface of ABS product, And then implanted layer is formed in ABS product near surface 200nm, specifically:
ABS product to be processed is mounted in the system of columnar target source, HPPMS is carried out in the case where being passed through reaction gas and is put Electricity；
HPPMS electric discharge make splash go out metal ion and the non-ionization of sputter material atom limitation cylinder interior, repeatedly Sputtering and ionization, and the metal ion of ionization then passes through extraction grid and draws and accelerate；
By the control of acceleration voltage, realize the matrix of the ion pair ABS product of different-energy and coating carry out injection or Deposition.
(16) after the pretreatment of metal ion high energy finishes, ion energy is gradually slowly reduced, and is continuously slowly introducing anti- Gas is answered, until forming the interface blended layer by metal to ceramic continuous transition.
Since cylinder-shaped inner circumferential surface product (i.e. electric discharge plane) is much larger than line removal cross-section area, while after extraction Ion is by no longer by the attraction of target surface negative potential, deposition efficiency is greatly improved.
Using method of the invention after ABS product surface prepares nano ceramic coat interface compared with prior art, knot Fruit is as shown in table 13:
Table 13
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (6)

1. a kind of method for preparing nano ceramic coat interface in ABS product surface, which is characterized in that include the following steps,
S1: surface degreasing removes the greasy dirt that ABS product attaches；
S2: surface hydrophilic processing sufficiently soaks ABS product surface；
S3: surface roughening treatment；
S4: surface neutralisation treatment；
S5: pre-preg immerses the ABS product after neutralization in predip solution, room temperature, impregnates 2min；
S6: palladium ion is adsorbed in workpiece surface using colloid palladium activation method and is reduced into active palladium metal by heavy palladium；
S7: dispergation, by above-mentioned heavy palladium treated ABS product in the solution containing 80~120mL/L of chemical pure hydrochloric acid dispergation Processing；
S8: alkaline nickel plating, by above-mentioned heavy palladium, treated that ABS product is containing NiSO422~30g/L, NaH2PO2·H2O 22 ~30g/L, NH420~30g/L of Cl, 10~15g/L of sodium citrate mixed solution in carry out nickel chemical plating technology, solution temperature Degree control is 40~60 DEG C；
S9: cleaning, using ultrasonic wave water washing, temperature controls the scavenging period 10min between 50~60 DEG C；
S10: drying；
S11: gaseous plasma cleaning pretreatment starts the cleaning processing ABS product surface using source gas plasma；
S12: the pretreatment of metallic plasma high energy ion implantation carries out energetic ion injection processing in the interface of ABS product, in turn Implanted layer is formed in ABS product near surface 200nm；
S13: after the pretreatment of metal ion high energy finishes, ion energy is gradually slowly reduced, and be continuously slowly introducing reaction gas Body, until the interface blended layer by metal to ceramic continuous transition is formed,
ABS product to be processed is mounted in the system of columnar target source, HPPMS electric discharge is carried out in the case where being passed through reaction gas；
HPPMS electric discharge make splash go out metal ion and the non-ionization of sputter material atom limitation cylinder interior, sputter repeatedly And ionization, and the metal ion of ionization then passes through extraction grid and draws and accelerate；
By the control of acceleration voltage, realize that the matrix of the ion pair ABS product of different-energy and coating are injected or deposited.
2. the method according to claim 1 for preparing nano ceramic coat interface in ABS product surface, which is characterized in that It further include pyrophosphate copper plating processing before being cleaned after the step S8 alkalinity nickel plating with step S9, specifically:
One layer of copper is plated in ABS product surface using pyrophosphate system.
3. the method according to claim 1 for preparing nano ceramic coat interface in ABS product surface, which is characterized in that It is described that one layer of copper is plated in ABS product surface using pyrophosphate system specifically: above-mentioned ABS product is being contained into Cu2P2O7· 3H250~70g/L of O, K4P2O7·3H2The mixed solution of 320~360g/L of O, 20~25g/L of ammonium citrate carry out pyrophosphate Copper plating treatment.
4. the method according to claim 2 for preparing nano ceramic coat interface in ABS product surface, which is characterized in that It further include acidiccopper plating processing after pyrophosphate copper plating processing, specifically: above-mentioned ABS product is being contained CuSO4200~220g/L, the pure H of chemistry2SO4The mixed solution progress sulfuric acid of 60~80g/L, 70~80mg/L of chemical pure hydrochloric acid Salt copper plating treatment.
5. the method according to claim 4 for preparing nano ceramic coat interface in ABS product surface, which is characterized in that It further include Nickel Plating Treatment after acidiccopper plating processing, specifically: above-mentioned ABS product is being contained into NiSO4220~ 300g/L、NiCl235~75g/L, H3BO3The mixed solution of 40~48g/L carries out Nickel Plating Treatment.
6. the method according to claim 4 for preparing nano ceramic coat interface in ABS product surface, which is characterized in that It further include chromium plating process after acidiccopper plating processing, specifically: above-mentioned ABS product is being contained into Cr2O3200~ 280g/L, the pure H of chemistry2SO4The mixed solution of 2.0~2.8g/L carries out chromium plating process.
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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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Publication number Priority date Publication date Assignee Title
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
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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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