CN110438499A - A kind of non-metal material surface metalized article and its method for metallising - Google Patents
A kind of non-metal material surface metalized article and its method for metallising Download PDFInfo
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- CN110438499A CN110438499A CN201910696684.6A CN201910696684A CN110438499A CN 110438499 A CN110438499 A CN 110438499A CN 201910696684 A CN201910696684 A CN 201910696684A CN 110438499 A CN110438499 A CN 110438499A
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- metal
- metal layer
- metal material
- layer
- material surface
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- 239000007769 metal material Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910052755 nonmetal Inorganic materials 0.000 title claims abstract description 29
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- 239000002184 metal Substances 0.000 claims abstract description 148
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- 239000010949 copper Substances 0.000 claims description 48
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- 238000007747 plating Methods 0.000 claims description 34
- 238000004544 sputter deposition Methods 0.000 claims description 28
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- 238000001465 metallisation Methods 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 229910052723 transition metal Inorganic materials 0.000 claims description 11
- 150000003624 transition metals Chemical class 0.000 claims description 11
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 6
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- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 1
- 229940050410 gluconate Drugs 0.000 description 1
- 235000013905 glycine and its sodium salt Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229940001447 lactate Drugs 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000006263 metalation reaction Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
-
- 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
- C23C28/02—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 only coatings only including layers of metallic material
-
- 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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of non-metal material surface metalized article and its method for metallising, and the product includes at least one layer of non-metallic layer and at least one layer of metal layer;The metal layer is made of metal material, and the non-metallic layer is made of plastics and/or rubber;It has many advantages, such as non-metallic layer and metal layer binding strength height, excellent mechanical property.
Description
Technical field
The present invention relates to the surface metalation preparation sides of non-metal material surface metallizing art more particularly to a kind of plastics
Method and product.
Background technique
Non-metal material surface formed metal layer, as electromagnetic signal conduction access, be widely used in automobile, industry,
The fields such as computer, communication.
There are also vacuum vapour deposition, magnetron sputtering method, ion plating methods for the method for non-metal material surface painting coating metal layer.China
Patent CN85109145 discloses " plastic products and its manufacturing method that are coated with metal ", and coating method is using magnetron sputtering
Method.Chinese patent CN1117916 is disclosed " plastic products of metallization ", and coating method is sprayed using vacuum deposition or vacuum
Plating method.Chinese patent CN1162654 is disclosed " metal coat of thermoplastic ", coating method using gas phase spraying plating at
Reason or sputtering method.For the plastics of the low-surface-energies such as polypropylene, need to be chemically treated before coating, electric spark processing or low temperature
Corona treatment etc. pre-processes (surface dust, roughening, activation are simultaneously grafted).Metal vapor deposition inevitably causes surface to be damaged
Wound.There are still non-metallic layer and metal layer binding strength be not high and the disadvantages of mechanical property is poor for these methods.
For above situation, the present invention provides a kind of non-metal material surface metalized article and its method for metallising.
Summary of the invention
First aspect present invention provides a kind of non-metal material surface metalized article, and the product includes at least one layer of non-
Metal layer and at least one layer of metal layer;The metal layer is made of metal material, and the non-metallic layer is made of nonmetallic materials;
The metal material includes at least transition metal;The nonmetallic materials are plastics and/or rubber.
As one embodiment of the present invention, the transition metal be selected from chromium, manganese, iron, cobalt, nickel, copper, zinc, palladium, silver,
One of platinum, gold or mercury are a variety of.
As one embodiment of the present invention, the transition metal is in nickel, manganese, iron, cobalt, copper, chromium, silver or zinc
It is one or more.
As one embodiment of the present invention, the nonmetallic materials are plastics.
As one embodiment of the present invention, the nonmetallic materials are selected from polyethylene, polypropylene, polyvinyl chloride, gather
Styrene, acrylonitrile-butadiene-styrene (ABS) co-polymer, polymethacrylates, polyethylene terephthalate, poly- pair
One of butyl phthalate and polyurethane are a variety of.
As one embodiment of the present invention, the non-metallic layer is made of plastic film.
The second aspect of the present invention provides a kind of method for metallising for preparing above-mentioned non-metal material surface metalized article,
The method includes at least following steps:
It is metallized by the way of sputter coating;
It is metallized by the way of electroplated metallization.
As one embodiment of the present invention, described method includes following steps:
The method that S01 uses sputter coating, metallizes in non-metal layer surface, forms the first metal layer and the second gold medal
Belong to layer;
S02 forms third metal layer by the way of chemical plating, on the surface of second metal layer;
S03 forms the 4th metal layer by the way of electroplated metallization, on the surface of third metal layer.
As one embodiment of the present invention, the gold of the metal material of the third metal layer and the 4th metal layer
It is identical to belong to material.
As one embodiment of the present invention, the metal material of the third metal layer is copper.
The utility model has the advantages that
The present invention uses specific deposition technique and technique, prepares metal layer and non-metallic layer firm binding force, and have
Have the advantages that opaque;The present invention realizes the effective heavy of different metal by adjusting the technological parameter of actual deposition technology simultaneously
Product.
Specific embodiment
In conjunction with preferred implementation method of the invention below detailed description and including embodiment can be further understood that this hair
Bright content.Unless otherwise indicated, all technologies used herein and scientific term all have general with the application fields
Logical technical staff's is generally understood identical meaning.If mentioned in the definition and the application of the concrete term disclosed in the prior art
Any definition supplied is inconsistent, then term provided herein of being subject to defines.
It is used in the present context, unless being clearly dictated in context, otherwise without the spy of the single plural form of restriction
Sign is also intended to the feature including plural form.It will also be appreciated that term as used herein " by ... preparation " it is synonymous with "comprising",
" comprising ", " including ", " having ", "comprising" and/or " including " indicate stated group when used in this manual
Object, step, method, product or device are closed, but does not preclude the presence or addition of one or more of the other composition, step, method, system
Product or device.In addition, using " preferred ", " preferably ", " preferred " etc. to be when describing presently filed embodiment
Refer to, can provide the embodiment of the present invention of certain beneficial effects in some cases.However, under identical circumstances or other feelings
Under condition, other embodiments are also likely to be preferred.In addition to this, not dark to the statement of one or more preferred embodiments
Show that other embodiments are unavailable, is also not intended to exclude other embodiments except the scope of the present invention.
The present invention provides a kind of non-metal material surface metalized article, the product include at least one layer of non-metallic layer and
At least one layer of metal layer;The metal layer is made of metal material, and the non-metallic layer is made of nonmetallic materials.
The metal material includes at least transition metal, and the nonmetallic materials are plastics and/or plastics.
Metal layer
In the present invention, the metal layer refers to what the modes such as sputtering, chemical plating, plating of use were formed in non-metal layer surface
Metal surface.
As one embodiment of the present invention, the number of plies of the metal layer can be one layer, using sputter coating, chemistry
Any one of plated film and plating carry out plated film.
As one embodiment of the present invention, the number of plies of the metal layer be can be two layers, using sputter coating, chemistry
Any two in plated film and plating distinguish plated film.
As one embodiment of the present invention, the number of plies of the metal layer can be three layers, be respectively adopted sputter coating,
Plated film and plating difference plated film.
As one embodiment of the present invention, the number of plies of the metal layer can be greater than three layers.
Transition metal
Transition metal refers to a series of metallic elements in the area d in the periodic table of elements;In general, this region is arrived including 3
12 have the element of ten races altogether, but do not include the inner transition element in the area f.
As one embodiment of the present invention, the transition metal be selected from chromium, manganese, iron, cobalt, nickel, copper, zinc, palladium, silver,
One of platinum, gold or mercury are a variety of.
As a kind of preferred embodiment of the invention, the filtering metal is in nickel, manganese, iron, cobalt, copper, chromium, silver and zinc
It is one or more.
As more a kind of preferred embodiment of the present invention, the transition metal is selected from one of Ni, Co, Cu and Ag or more
Kind.
Non-metallic layer
In the present invention, the non-metallic layer is made of plastics and/or rubber material.
As one embodiment of the present invention, the non-metallic layer is made of plastics.
As one embodiment of the present invention, the plastics be selected from polyethylene, polypropylene, polyvinyl chloride, polystyrene,
Acrylonitrile-butadiene-styrene (ABS) co-polymer, polymethacrylates, polyethylene terephthalate, poly terephthalic acid
One of butyl ester or polyurethane are a variety of.
From the angle for the binding force for improving non-metallic layer and metal layer, the plastics be selected from polypropylene, polyethylene and
Polyvinyl chloride, one of polyethylene terephthalate, PA polybutyleneterephthalate and polyurethane.
From the light transmittance angle for reducing metalized article, the non-metallic layer is made of plastic film, the plastics
Film with a thickness of 2-1000 μm;It is more preferred with a thickness of 2-100 μm.
The second aspect of the present invention provides a kind of method for metallising for preparing above-mentioned non-metal material surface metalized article,
The method includes at least following steps:
It is metallized by the way of sputter coating;
It is metallized by the way of electroplated metallization.
As one embodiment of the present invention, the method for metallising of the non-metal material surface metalized article includes
Following steps:
The method that S01 uses sputter coating, metallizes in non-metal layer surface, forms the first metal layer and the second gold medal
Belong to layer;
S02 forms third metal layer by the way of chemical plating, on the surface of second metal layer;
S03 forms the 4th metal layer by the way of electroplated metallization, on the surface of third metal layer.
Sputter coating
Common sputter coating mode mainly includes d.c. sputtering, radio-frequency sputtering, magnetron sputtering and reactive sputtering.
In the present invention, the mode of the sputter coating can be known to the skilled in the art any sputter coating
Mode, illustrated with magnetron sputtering, the present invention in, the magnetron sputtering specific steps are as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film, to non-gold
Belong to material and carry out plated film, bias mains voltage sets 80-180V, and grid bias power supply duty ratio sets 30-50%, intermediate frequency power supply electric current
15A-25A is set, argon flow is set as 150-180Sccm, and reaction gas flow requires to be gradually added into according to membrane system, when plated film
Between setting required according to membrane system and film thickness, vacuum degree is down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product.
In the present invention, the metal layer for using sputter coating to be formed is the first metal layer and second metal layer.
The first metal layer is the metal layer being plated on non-metallic layer.
The first metal layer and the second metal are respective with a thickness of 1-200nm;More preferably 1-20nm.
The first metal layer and the metal material of second metal layer are following at least one metal or its compound: Ni,
Co, Cu and Ag.
Chemical plating
Chemical plating is also referred to as electroless plating or autocatalytic plating, is in the case where no impressed current by suitable reduction
Agent makes metal ion in plating solution be reduced into metal, and deposits to a kind of coating method of piece surface.
Electroless plating technology is that the deposition of metal is generated by controllable redox reaction under the catalytic action of metal
Process.Compared with plating, electroless plating technology is with coating is uniform, pin hole is small, is not required to DC power supply device, can sink on non-conductor
Accumulate and have the characteristics that certain properties.
As one embodiment of the present invention, the third metal layer that the chemical plating is formed is copper film.
As one embodiment of the present invention, the plating steps of the chemical plating include at least copper facing and following steps group
It is one or more in conjunction;
The step combination includes:
It is bulk, remove glue, neutralization, adjustment, activating pretreatment, activation, activating and reducing.
It is bulk
Bulk is that the precondition of a uniform, ideal hole wall is provided for subsequent step.
The leavening agent used in the present invention is made of water, bulk additive, pH correction agent;And every liter of leavening agent contains
The water of 849ml, the bulk additive of 150ml and the pH correction agent of 1ml.
The bulk additive is by the N-Methyl pyrrolidone of 30-100g/L, the sodium hydroxide of 40-60g/L and 30-
The DMF of 100g/L is formed.
The pH correction agent is the sodium hydroxide solution of 32wt%.
The bulk processing step is as follows:
Object to be processed is placed in bulk solution, standing time 45-110s, bulk solution temperature is that 70-80 is Celsius
Degree.
The bulk solution refers to the mixture of leavening agent and water, and the bulk addition in 1 liter of bulk solution containing 150ml
Agent.
The pH value of the bulk solution is 10-12.
Except glue
Except glue primarily to high-efficiency cleaning hole wall and perforating residue, effectively prevent hole wall to separate;It simultaneously can be effective
Increase the binding force of hole wall and substrate, reduces separation risk.
The adhesive remover used in the present invention is formed by water, except glue additive, pH adjusting agent;And every liter of leavening agent contains
The water of 770ml, 125ml except glue additive and 105ml pH adjusting agent.
The glue additive that removes is permanganate, compares preferably sodium permanganate.
The sodium hydroxide solution that the pH adjusting agent is 32%, 32% sodium hydroxide solution refer to 432g/L NaOH.
It is described except the processing step of glue is as follows:
Object to be processed is placed on except in sol solution, standing time 90-300s, removing sol solution temperature is that 75-85 is Celsius
Degree.
The mixture for referring to adhesive remover and water except sol solution, and 1 liter of glue that removes removed in sol solution containing 50g adds
Agent;1 liter except the NaOH containing 45g in sol solution.
It neutralizes
In the present invention, the neutralization is the acidic materials neutralized except during glue, improves binding force.
The neutralizer used in the present invention is made of water, sulfuric acid, hydrogen peroxide and neutralization additive;And every liter of neutralizer contains
There are the water of 860ml, the sulfuric acid of the 50wt% of 100ml and the 35wt%H of 15ml2O2。
The processing step of the neutralization is as follows:
Object to be processed is placed on and is neutralized in solution, standing time 35-60s, neutralizing solution temperature is that 25-35 is Celsius
Degree.
The neutralization solution refers to the mixture of neutralizer and water, the sulphur of the 50wt% containing 100ml in 1 liter of neutralization solution
Acid;The 35wt%H of 15ml2O2。
Adjustment
Heretofore described adjustment is the residue in order to effectively remove de-smear in hole, while adjusting pore wall charge, is made
The surface that hole wall becomes extremely strong adsorption capacity is obtained, provides ideal hole wall treatment effect for subsequent copper facing.
The regulator used in the present invention is made of water and adjustment additive;And every liter of regulator contains the water of 960ml,
The adjustment additive of 40ml.
The adjustment additive is selected from one kind of dopamine, Dopamine hydrochloride, pyrroles, hydramine or nitrate.
The processing step of the adjustment is as follows:
Object to be processed is placed in adjustment solution, standing time 60s, adjustment solution temperature is 50 degrees Celsius.
Activating pretreatment
In the present invention, the activating pretreatment is adjusted simultaneously primarily to the pollutant before activating in device to hole is handled
Economize on electricity lotus, prepares for subsequent activation.
In the present invention, the activating pretreatment agent is sodium chloride solution, and 980ml water is contained in every 1 liter of activating pretreatment agent
Sodium chloride, 10ml activating pretreatment additive with 10ml.
The activating pretreatment additive is tartrate, citrate, edetate, nitrilotriacetic acid salt, three
One of ethanol amine.
The processing step of the activating pretreatment is as follows:
Object to be processed is placed in activating pretreatment agent, standing time 20s, neutralizing solution temperature is 25 degrees Celsius.
Activation
Heretofore described activation processing, which refers to, activates the hole wall for having adjusted charge, to be copper facing below
Good covering provide optimal conditions.
The activator used in the present invention is made of water, activating additive and alkaline matter;And every liter of activator contains
The water of 774ml, the activating additive of 225ml and the sodium hydroxide solution of 1ml.
The concentration of the sodium hydroxide solution is 32wt%.
As one embodiment of the present invention:
The activating additive is main composition and adjuvant;The two weight ratio is 10:1.
The main composition is palladium sulfate, and the adjuvant is ethylenediamine tetra-acetic acid or ethylenediamine.
The processing step of the activation is as follows at this time:
Object to be processed is placed in activated solution, standing time 45s, activated solution temperature is 45 degrees Celsius;PH value
It is 10.0.
As another embodiment of the invention:
The activating additive is main composition and adjuvant;The two weight ratio is 10:1.
The main composition is silver nitrate, and the adjuvant is sodium hypophosphite or EDETATE SODIUM.
The processing step of the activation is as follows at this time:
Object to be processed is placed in activated solution, standing time 45s, activated solution temperature is 45 degrees Celsius;PH value
For 3-6.
Activating and reducing
Activating and reducing is primarily to catalysis accelerates later period copper-plated process.
The activating and reducing agent used in the present invention is made of water, boric acid and activating and reducing additive;And every liter activation also
Former agent contains the water of 990ml, the boric acid of 25g, the activating and reducing additive of 10mg.
The activating and reducing additive is potassium borohydride.
The processing step of the activating and reducing is as follows:
Object to be processed is placed in activating and reducing agent, standing time 35s, activating and reducing solution temperature is 35 Celsius
Degree;PH value is 6 or so.
Electroless copper
In the present invention, every 1 liter of chemical copper solution includes 852.5ml water, copper-based agent of 85ml, 2.5ml copper stabilizer, 45ml
Copper additives, 15ml copper reduction agent, 9g sodium hydroxide.
The copper-based agent is complexing agent, and the complexing agent is selected from preferably at least two or up to 10 carbon atoms
Amino acid, polycarboxylic acids, usually aminoacetic acid, such as nitrilotriacetic acid, alternatively, the usually poly- second of alkylen polyamine
Acid, it includes ethylenediamine tetra-acetic acid (EDTA), diethylenetriamine pentaacetic acid (DTPA), N-hydroxyethyl-ethylenediamine tetraacethyl, 1,
3- diamino -2- propyl alcohol-N, N, N ',-four acetic acid of N ', two acetic acid of dihydroxyphenyl ethylene diamine, four acetic acid of diaminocyclohexane
Or ethylidene glycol-bis- ((beta-aminoethyl ether)-N, N '-four acetic acid) and N, N, N ', N '-four-(2- hydroxypropyl) ethylene
Amine, citrate, tartrate, N, N-2- (ethoxy) glycine, gluconate, lactate, citrate, tartrate,
Coronal ether and/or cryptand.
The copper additives are copper sulphate.
The copper reduction agent is selected from one of vanillic aldehyde and formaldehyde, glyoxalic acid, sodium hypophosphite or elegreen or more
Kind.
The processing step of the electroless copper is as follows:
Object to be processed is placed in chemical copper solution, standing time 240-450s, chemical copper solution temperature is taken the photograph for 35
Family name's degree.
The liquid medicine service life: tank liquor produces area 100m2/ L or tank liquor specific gravity are more than 1.09g/cm3。
The third metal with a thickness of 0.05-3 μm.
Electroplated metallization
Plating is exactly to plate the process of the other metal or alloy of a thin layer on certain metal surfaces using electrolysis principle, is
The technique of the surface of metal or other materials product attachment layer of metal film is set to prevent metal oxygen to play using electrolysis
The effects of changing (as corroded), improving wearability, electric conductivity, reflective, corrosion resistance (copper sulphate etc.) and having improved aesthetic appearance.
Electroplate liquid used in the present invention includes the cupric sulfate pentahydrate of 60-90g/L;The sulfuric acid of 180-220g/L;40-
The chloride ion of 80ppm;The open cylinder agent of 8-12ml/L;The brightener of 3-5ml/L and the regulator of 0.1-0.5ml/L.
There is the chloride ion etc. in hydrochloric acid, acid mist or tap water in the source of chloride ion in the present invention.
The open cylinder agent is sulfonate, azacyclo- copolymer and surfactant.
The sulfonate be selected from one of dodecyl sodium sulfate, acyl methylamine alkane sulfonic acid sodium or paratoluenesulfonic acid sodium salt or
It is a variety of;The azacyclo- copolymer is poly- (vinyl imidazole -2- acrylamide-2-methyl propane sulfonic-methacrylic acid 18
Ester).The surfactant is selected from one of sodium isethionate, succinic acid dihexyl sodium sulfonate, lauryl sodium sulfate.
The brightener is mercaptopropanesulfonic acid sodium and N, and N- dimethyl disulfide is for formamide propane sulfonic acid sodium, ratio 2:
1。
The regulator is polyethylene glycol of the hydroxyl value in 8~14mg KOH/g.
The step of plating, is as follows:
01. plating solution opens cylinder
1, cylinder body cleans
A), clean cylinder body and each pipeline are washed with water;
B), cylinder body and filtration system 2-4 hours are impregnated with 5wt%NaOH;
C), 5wt%H is used after cleaning up cylinder body and each pipeline with clear water2SO4 impregnates 2-4 hours;
D), cylinder can be opened after washing with water clean cylinder body and each pipeline;
2, cylinder step is opened
A), the water of 2/3 cylinder volume is placed, filtering is opened and is inflated;
B), it is slowly added to the AR grade sulfuric acid of 200g/L;
C), 75g/L copper sulphate is added;
D), it is linked into cleaned copper anode, and changes cotton core after filtering 4 hours using carbon core and filters;
E), when temperature is cooled to 30 DEG C or less, 10ml/L open cylinder agent, 5ml/L brightener, 0.5ml/L regulator is added;
F), using 0.5-2.0ASD current density electrolysis 4-8 hours;
G), can be test-manufactured after test and chemical analysis adjustment each component to normal range (NR).
02 plating conditions are as follows:
Operating temperature: 20-30 degrees Celsius;Cathode-current density is 1-6A/dm2, voltage 1-3.5V;Anode is cupric
99.9% phosphorous copper balls or phosphor-copper angle (phosphorous 0.03-0.06wt%).Anode and cathode area ratio is 1:(1.5-2.5);Agitating mode
For air stirring (using low-pressure oil-free hair dryer and oily-water seperating equipment and filter device must be passed through) and movable cathode;Filtering
Mode is that 5-10 μm of cotton core or carbon core continuously filter.
03 plating solution maintenance:
1, because the plating solution of evaporation loss can be added with deionized water;
2, periodic analysis sulfuric acid copper content, sulfuric acid content and chloride content;
3, additive is adjusted according to hull trough test;
4, every operation 1000AH need to add brightener 200ml during normal production.
4th metal layer with a thickness of 100-50000nm.
Technology of the invention is described in detail combined with specific embodiments below.
Embodiment 1:
The present embodiment provides a kind of non-metal material surface metalized article, the product includes one layer of non-metallic layer and four
Layer non-metallic layer;
The non-metallic layer is polyethylene film, and the weight average molecular weight of the polyethylene film is 560000.
The film thickness is 50 μm.
Four layers of metal layer is respectively the first metal layer, second metal layer, third metal layer and the 4th metal layer.
The first metal layer and the second metal carry out plated film in a manner of sputtering, and third metal layer is in a manner of chemical plating
Carry out plated film;4th metal layer carries out plated film in a manner of being electroplated.
Wherein, the first metal layer is formed by Ni metal, and second metal layer is formed by Co metal, third metal layer and
Four metal layers have copper metal to be formed.
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 95V, and grid bias power supply duty ratio setting 35%, intermediate frequency power supply electric current is set
Determine 18A, argon flow is set as 160Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
15min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 150V, and grid bias power supply duty ratio setting 35%, intermediate frequency power supply electric current sets 22A, and argon flow is set
It is set to 150Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 9min, vacuum degree is down to
2.3×10-1Pa。
The first metal layer it is bimetallic with a thickness of 13nm with a thickness of 15nm,;
Chemical plating:
In the present invention, the chemical plating includes the following steps:
S001:
It is bulk: will to be placed in bulk solution by the product of sputter coating, standing time 60s, bulk solution temperature
It is 75 degrees Celsius;
S002:
Except glue: will be placed on by bulk processed product except in sol solution, standing time 120s removes sol solution temperature
Degree is 80 degrees Celsius;
S003
It neutralizes: it will be by being neutralized in solution except the processed product of glue is placed on, standing time 40s neutralizes solution temperature
Degree is 30 degrees Celsius;
S004:
Adjustment: the product crossed by neutralisation treatment being placed in regulator, standing time 60s, adjusts solution temperature
It is 50 degrees Celsius.
S005:
Activating pretreatment: will be adjusted processed product and be placed in activating pretreatment agent, standing time 20s,
Neutralizing solution temperature is 25 degrees Celsius.
S006:
Activation: the product crossed by activating pretreatment is placed in activator, standing time 45s, activated solution temperature
Degree is 45 degrees Celsius.
S007:
Activating and reducing: it will be placed in activating and reducing agent by the product being activated, standing time 35s, activation
Reducing agent temperature is 35 degrees Celsius.
S008:
Copper facing: it will be placed in chemical copper solution by the processed product of activating and reducing, standing time 315s, chemistry
Heavy copper liquid temperature is 35 degrees Celsius.
The leavening agent is made of water, bulk additive, pH correction agent;And every liter of leavening agent contains the water of 849ml,
The bulk additive of 150ml and the pH correction agent of 1ml.The pH correction agent is the sodium hydroxide solution of 32wt%.
The bulk additive of 150ml is by the N-Methyl pyrrolidone of 60g/L, the sodium hydroxide of 50g/L and 70g/L
DMF composition.
The adhesive remover is formed by water, except glue additive, pH adjusting agent;And every liter of adhesive remover contains the water of 770ml,
125ml except glue additive and 105ml pH adjusting agent.The glue additive that removes is sodium permanganate;The pH adjusting agent is
32% sodium hydroxide solution, 32% sodium hydroxide solution refer to 432g/L NaOH.
The neutralizer is made of water, sulfuric acid, hydrogen peroxide and neutralization additive;And every liter of neutralizer contains 885ml's
Water, the sulfuric acid of the 50wt% of 100ml and the 35wt%H of 15ml2O2。
The regulator is made of water and adjustment additive;And every liter of regulator contains the water of 960ml, the adjustment of 40mg
Additive.The adjustment additive is dopamine.
The activating pretreatment agent is sodium chloride solution, the chlorine containing 980ml water and 10ml in every 1 liter of activating pretreatment agent
Change sodium, 10ml triethanolamine.
The activator is made of water, activating additive and alkaline matter;And every liter of activator contains the water of 774ml,
The activating additive of 225ml and the sodium hydroxide solution of 1ml.The concentration of the sodium hydroxide solution is 32wt%.The activation
Additive is main composition and adjuvant;The two weight ratio is 10:1.
The main composition is palladium sulfate, and the adjuvant is ethylenediamine tetra-acetic acid.
The activating and reducing agent is made of water, boric acid;And every liter of activating and reducing agent contains the water of 990ml, the boron of 25g
Acid, the potassium borohydride of 10mg.
Every 1 liter of chemical copper solution adds comprising 852.5ml water, copper-based agent of 85ml, 2.5ml copper stabilizer, 45ml copper
Add agent, 15ml copper reduction agent, 9g sodium hydroxide.The copper-based agent, copper stabilizer, copper additives and copper reduction agent are bought from wide
East is large at Science and Technology Ltd..
The copper-based agent is N-hydroxyethyl-ethylenediamine tetraacethyl;The copper additives are copper sulphate;The copper reduction agent
For elegreen.
Plating
The step of plating, is as follows:
01. plating solution opens cylinder
1, cylinder body cleans
A), clean cylinder body and each pipeline are washed with water;
B), cylinder body and filtration system 3 hours are impregnated with 5wt%NaOH;
C), 5wt%H is used after cleaning up cylinder body and each pipeline with clear water2SO4 impregnates 2 hours;
D), cylinder can be opened after washing with water clean cylinder body and each pipeline;
2, cylinder step is opened
A), the water of 2/3 cylinder volume is placed, filtering is opened and is inflated;
B), it is slowly added to the AR grade sulfuric acid of 200g/L;
C), 75g/L copper sulphate is added;
D), it is linked into cleaned copper anode, and changes cotton core after filtering 4 hours using carbon core and filters;
E), when temperature is cooled to 30 DEG C or less, 10ml/L open cylinder agent, 5ml/L brightener, 0.5ml/L regulator is added;
F), using 1.5ASD current density electrolysis 6 hours;
G), can be test-manufactured after test and chemical analysis adjustment each component to normal range (NR).
02 plating conditions are as follows:
Operating temperature: 25 degrees Celsius;Cathode-current density is 4A/dm2, voltage 1.8V;Anode is cupric 99.9%
Phosphorous copper balls or phosphor-copper angle (phosphorous 0.03-0.06wt%).Anode and cathode area ratio is 1:2;Agitating mode is that air stirring (must be adopted
With low-pressure oil-free hair dryer and pass through oily-water seperating equipment and filter device) and movable cathode;Filter type is 5-10 μm of cotton core
Continuous filtering.
03 plating solution maintenance:
1, because the plating solution of evaporation loss can be added with deionized water;
2, periodic analysis sulfuric acid copper content, sulfuric acid content and chloride content;
3, additive is adjusted according to hull trough test;
4, every operation 1000AH need to add brightener 200ml during normal production.
Electroplate liquid used in the present embodiment includes the cupric sulfate pentahydrate of 80g/L;The sulfuric acid of 190g/L;The chlorine of 60ppm from
Son;The open cylinder agent of 9ml/L;The brightener of 4ml/L and the regulator of 0.3ml/L.There is hydrochloric acid in the source of chloride ion in the present embodiment.
The open cylinder agent is dodecyl sodium sulfate, poly- (vinyl imidazole -2- acrylamide-2-methyl propane sulfonic-methyl
Octadecyl acrylate), sodium isethionate, ratio 5:1:1.
The brightener is mercaptopropanesulfonic acid sodium and N, and N- dimethyl disulfide is for formamide propane sulfonic acid sodium, ratio 2:
1。
The regulator is polyethylene glycol of the hydroxyl value in 10mg KOH/g.
The third metal layer thickness is 1 μm;4th metal layer with a thickness of 300nm.
Embodiment 1-1:
The present embodiment and the difference of embodiment 1 are as follows, remaining is all the same:
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 95V, and grid bias power supply duty ratio setting 35%, intermediate frequency power supply electric current is set
Determine 18A, argon flow is set as 160Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
18min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 150V, and grid bias power supply duty ratio setting 35%, intermediate frequency power supply electric current sets 22A, and argon flow is set
It is set to 150Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 6min, vacuum degree is down to
2.3×10-1Pa。
Embodiment 2:
The present embodiment the difference from embodiment 1 is that, the metal of second metal layer is silver;And concrete operations parameter is as follows:
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 95V, and grid bias power supply duty ratio setting 35%, intermediate frequency power supply electric current is set
Determine 18A, argon flow is set as 160Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
15min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 160V, and grid bias power supply duty ratio setting 40%, intermediate frequency power supply electric current sets 21A, and argon flow is set
It is set to 160Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 10min, vacuum degree is down to
2.3×10-1Pa。
The bulk processing step is as follows:
Object to be processed is placed in bulk solution, standing time 80s, bulk solution temperature is 78 degrees Celsius.
Embodiment 3:
The present embodiment the difference from embodiment 1 is that, the metal of the first metal layer is Co metal, the metal of second metal layer
For Ni metal.
Operating parameter is same as Example 1, and unused operating parameter is as follows:
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 110V, and grid bias power supply duty ratio setting 31%, intermediate frequency power supply electric current is set
Determine 17A, argon flow is set as 166Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
13min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 160V, and grid bias power supply duty ratio setting 40%, intermediate frequency power supply electric current sets 20A, and argon flow is set
It is set to 160Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 8min, vacuum degree is down to
2.3×10-1Pa。
The bulk processing step is as follows:
Object to be processed is placed in bulk solution, standing time 70s, bulk solution temperature is 75 degrees Celsius.
It is described except the processing step of glue is as follows:
Object to be processed is placed on except in sol solution, standing time 110s, bulk solution temperature is 81 degrees Celsius.
Embodiment 3-1:
The present embodiment the difference from embodiment 1 is that, the metal of the first metal layer is Co metal, the metal of second metal layer
For Ni metal;And design parameter is same as Example 1.
Embodiment 4:
The present embodiment and the difference of embodiment 3 are that the metal of second metal layer is Ag metal.
Operating parameter is same as Example 3, and unused operating parameter is as follows:
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 110V, and grid bias power supply duty ratio setting 31%, intermediate frequency power supply electric current is set
Determine 17A, argon flow is set as 166Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
13min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 120V, and grid bias power supply duty ratio setting 45%, intermediate frequency power supply electric current sets 20A, and argon flow is set
It is set to 155Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 11min, vacuum degree is down to
2.3×10-1Pa。
The bulk processing step is as follows:
Object to be processed is placed in bulk solution, standing time 90s, bulk solution temperature is 75 degrees Celsius.
It is described except the processing step of glue is as follows:
Object to be processed is placed on except in sol solution, standing time 112s, bulk solution temperature is 81 degrees Celsius.
Embodiment 5:
The present embodiment and the difference of embodiment 4 are that the metal of the first metal layer is Ag metal;The metal of second metal layer
For Co metal.
Operating parameter is same as Example 4, and unused operating parameter is as follows:
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 170V, and grid bias power supply duty ratio setting 32%, intermediate frequency power supply electric current is set
Determine 20A, argon flow is set as 166Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
15min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 120V, and grid bias power supply duty ratio setting 45%, intermediate frequency power supply electric current sets 21A, and argon flow is set
It is set to 158Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 10min, vacuum degree is down to
2.3×10-1Pa。
The bulk processing step is as follows:
Object to be processed is placed in bulk solution, standing time 90s, bulk solution temperature is 75 degrees Celsius.
It is described except the processing step of glue is as follows:
Object to be processed is placed on except in sol solution, standing time 120s, bulk solution temperature is 80 degrees Celsius.
Embodiment 6:
The present embodiment and the difference of embodiment 5 are that the metal of second metal layer is Ni.
Operating parameter is same as Example 5, and unused operating parameter is as follows:
The mode of the sputtering is as follows:
S01. under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film is right
Nonmetallic materials carry out plated film, and bias mains voltage sets 170V, and grid bias power supply duty ratio setting 32%, intermediate frequency power supply electric current is set
Determine 20A, argon flow is set as 166Sccm, and reaction gas flow requires to be gradually added into according to membrane system, starts plated film time setting
15min, vacuum degree are down to 2.3 × 10-1Pa;
Various pump valves are successively closed according to magnetron sputtering coater operating instruction after plated film, deflating to open the door to take out produces
Product obtain the product for being coated with the first metal layer.
S02. according to S01 step, the product for being coated with the first metal layer is carried out to the metallization operations of second metal layer.
Wherein, the metallization operations parameter of second metal layer is as follows:
Under argon gas and reaction gas environment, grid bias power supply is opened, the intermediate frequency power supply of target needed for opening plated film starts to plate
Film, bias mains voltage set 125V, and grid bias power supply duty ratio setting 48%, intermediate frequency power supply electric current sets 20A, and argon flow is set
It is set to 150Sccm, reaction gas flow requires to be gradually added into according to membrane system, starts plated film time and sets 10min, vacuum degree is down to
2.3×10-1Pa。
The bulk processing step is as follows:
Object to be processed is placed in bulk solution, standing time 90s, bulk solution temperature is 75 degrees Celsius.
Embodiment 7:
The present embodiment the difference from embodiment 1 is that, sputter coating has only plated one layer of metal layer, i.e. Ni metal layer.
Embodiment 8:
The present embodiment the difference from embodiment 1 is that, a kind of non-metal material surface metallization system provided in this embodiment
Product do not contain third metal layer, i.e., without chemical deposit, only to sputter the two metal layers formed and be electroplated formed one
Layer metal layer.
Embodiment 9:
The present embodiment the difference from embodiment 1 is that, in the present embodiment in chemical plating without containing adjustment, activating pretreatment,
Activation and this four step of activating and reducing, only include it is bulk, except glue, neutralization and copper facing.
Embodiment 10:
The present embodiment the difference from embodiment 1 is that, the nonmetallic materials are polypropylene, and its weight average molecular weight is
30000。
Remaining operating parameter and embodiment 1 are consistent.
Embodiment 11:
The present embodiment the difference from embodiment 1 is that, the copper reduction agent be formaldehyde.
Embodiment 12:
The present embodiment the difference from embodiment 1 is that, it is described except glue additive be potassium permanganate.
Performance test:
1. extensibility
Test method: taking long 10cm × wide 10cm sample, go horizontal drawing with the strength of constant force 30N, until fracture, record
Elongate length.
Extensibility=(length at break -10)/10 × 100%.
2. binding force
Test method: taking long 10cm × wide 10cm sample, be sticked on sample with 3M adhesive tape, adhesive tape is uncovered, and observes sample
Whether the metal on product surface is taken off, changes the adhesive tape of different viscosity until the metal layer of sample surfaces is destroyed.Record adhesive tape
Sticky specification, sticky specification is related with power, and conversion obtains the size of corresponding power.
3. light transmittance
Using optical microphotograph sem observation sample, observe whether sample surfaces have luminous point.Have luminous point be it is unqualified, without luminous point
For qualification.
Test result:
At last it is pointed out that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not intended to limit the invention, it is all at this
Made any modifications, equivalent replacements, and improvements etc., should be included in protection model of the invention within the spirit and principle of invention
Within enclosing.
Claims (10)
1. a kind of non-metal material surface metalized article, which is characterized in that the product include at least one layer of non-metallic layer and
At least one layer of metal layer;The metal layer is made of metal material, and the non-metallic layer is made of plastics and/or rubber;
The metal material includes at least transition metal or its compound.
2. non-metal material surface metalized article described in claim 1, which is characterized in that the transition metal be selected from chromium,
One of manganese, iron, cobalt, nickel, copper, zinc, palladium, silver, platinum, gold or mercury are a variety of.
3. non-metal material surface metalized article as claimed in claim 2, which is characterized in that the transition metal be selected from nickel,
One of manganese, iron, cobalt, copper, chromium, silver or zinc are a variety of.
4. non-metal material surface metalized article described in claim 1, which is characterized in that the non-metallic layer is by plastics structure
At.
5. non-metal material surface metalized article as claimed in claim 4, which is characterized in that the plastics be selected from polyethylene,
Polypropylene, polystyrene, acrylonitrile-butadiene-styrene (ABS) co-polymer, polymethacrylates, gathers to benzene two polyvinyl chloride
One of formic acid glycol ester, PA polybutyleneterephthalate or polyurethane are a variety of.
6. non-metal material surface metalized article described in claim 1, which is characterized in that the non-metallic layer is thin by plastics
Film is constituted.
7. a kind of method for metallising of non-metal material surface metalized article described in any one of claims 1-6, feature
It is, the method includes at least following steps:
It is metallized by the way of sputter coating;
It is metallized by the way of electroplated metallization.
8. the method for metallising of non-metal material surface metalized article as claimed in claim 7, which is characterized in that the method
Include the following steps:
The method that S01 uses sputter coating, metallizes in non-metal layer surface, forms the first metal layer and the second metal
Layer;
S02 forms third metal layer by the way of chemical plating, on the surface of second metal layer;
S03 forms the 4th metal layer by the way of electroplated metallization, on the surface of third metal layer.
9. the method for metallising of non-metal material surface metalized article according to any one of claims 8, which is characterized in that the third
The metal material of metal layer is identical with the metal material of the 4th metal layer.
10. the method for metallising of non-metal material surface metalized article according to any one of claims 8, which is characterized in that described
The metal material of three metal layers is copper.
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