CN103122452A - Surface metallization method for foamed plastic by adopting high-power pulse magnetron sputtering - Google Patents
Surface metallization method for foamed plastic by adopting high-power pulse magnetron sputtering Download PDFInfo
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Abstract
The invention relates to a surface metallization method for foamed plastic by adopting high-power pulse magnetron sputtering and belongs to the technical field of material surface engineering. The surface metallization method for the foamed plastic by adopting high-power pulse magnetron sputtering comprises the following steps of: firstly carrying out pre-treatment of surface sealing, cleaning, drying and distressing on the surface of foamed plastic, then loading samples, vacuumizing, and degassing; carrying out pre-sputtering to clean a foamed plastic workpiece and sputtering a target material; depositing a metal coating by adopting high-power pulse magnetron sputtering, wherein a metal coating with high ionization rate is deposited on the surface of the foamed plastic workpiece at a low temperature by controlling pulse configuration, frequency, charging voltage and sputtering/cooling time, and a metal coating with smooth surface, compact structure and high cohesion between film and substrate material is prepared; and finally cooling, taking away the foamed plastic workpiece, and inspecting properties of the metallized foamed plastic such as surface appearance, hardness and cohesion between film and substrate material. The surface metallization method for the foamed plastic by adopting high-power pulse magnetron sputtering has the advantages that the surface metallization method is applicable to various metallized coatings; the coating is smooth and compact in surface and high in cohesion between film and substrate material; the sputtering temperature and the deposition temperature are low, and a foamed plastic substrate can not deform; and the surface metallization method is safe and environment-friendly, and no chromic acid reagent which contains Cr<6+> and is related in a chemical plating process is used.
Description
Technical field
The present invention relates to porous plastics high-power impulse magnetron sputtering method for surface metallation, belong to the material surface engineering field.
Background technology
Nineteen forty-six, the U.S. starts to carry out metallization of plastic surface production, metallization of plastic surface can increase substantially the plastics performance, enlarge the use range of plastics, therefore plastic-metal production obtains very fast development, and nowadays the plastic-metal component have been widely used in automotive industry, instrument industry, shipbuilding, electronic industry and Aeronautics and Astronautics industry.Plastic-metal metallization processes application purpose is developed into and is utilized its feature performance benefit to substitute difficult-to-machine metal part, simplified processing process, saving precious metal and prolongation part work-ing life etc. by initial simple beautiful decoration.The plastic matrix material that is usually used in surface metalation has: polyester, nylon, polypropylene etc.Can, to the plastics processing of foaming, prepare porous plastics by physics or chemical process.Metallization can make Foam Plastic Surface have physicals, elimination static, reduction porous plastics air penetrability, the raising humidity resistance of institute's metallizing, and improve the mechanical property of porous plastics simultaneously, make heat-drawn wire rising 70～88.5%, tension stress performance raising 10～30%, impact resistance increase by 15～20%, the anti-tortuous power of porous plastics increase by 12%～20%, its good solubility-resistence can also increase.
Metallization of plastic surface technique is divided into wet processing and dry process two classes, and wet processing comprises electroless plating and liquid phase spraying etc., and dry process comprises vacuum evaporation, magnetron sputtering and gas phase spraying etc.The principle of electroless plating metallization of plastic surface technique is: do not apply external power, and utilize reductive agent that the metal ion in solution is reduced and be deposited on the body surface with catalytic activity, make it to form metallic coating.Its technical process is: surface preparation, oil removing, neutralization, chemical roughen, sensitization, distillation washing, activation, electroless plating, cleaning, plating.Wherein chemical roughen, sensitization, activation and electroless plating are crucial process procedures.2007, the Chinese patent of Na Lusikeweixiwusi etc. " frosting plates the method (CN101255584A) of attached metal ", by the Cryo-etching frosting, frosting is carried out to chemical roughen, improve chemical plating technology applicable plastic sill scope, and strengthen bonding force and the wear resisting property of coating.2010, the Chinese patent of Yin Weixin " a kind of method of electroplating copper on plastic surface (CN102383158A) ", add additive take sulfuric acid and copper sulfate in main electroplate liquid, improve homogeneity, film-substrate cohesion and the surface smoothness of frosting copper metallization coating.Electroless plating metallization of plastic surface technique can be carried out at low temperatures, be difficult for making plastic deformation, and equipment is simple, with low cost, but its metallizing kind is limited and technical process is complicated, use poisonous chemical reagent, that especially in the chemical roughen process, uses contains Cr
6+chromic acid, environmental pollution is very big.
Magnetron sputtering metallization of plastic surface technique is one and has high speed, low temperature, low damage, low-work voltage, and the physical gas phase deposition technology of advantages of environment protection, its simple process easy handling, produce the consumptive material utilization ratio high, consume less and environmental pollution little.By in vacuum, being filled with rare gas element, and apply electromagnetic field between plastic substrate and metallic target, the electron excitation rare gas element produced by glow discharge, produce plasma body, plasma body hits the atom of metal targets, is deposited on plastic substrate, completes sputter deposition process.1984, the United States Patent (USP) of Sartor etc. " Method For Metalizing Carbon Fiber Reinforced Plastic Members(US4455207) ", on the carbon fiber reinforced plastics surface, by gas phase deposition technology metallizing coating, before vapour deposition, use plasma bombardment to carry out the workpiece surface pre-treatment to improve the bonding force of metallic coating and carbon fiber reinforced plastics.Nineteen ninety-five, the European patent of Brule etc. " Process for the metallization of articles of plastic material(EP0539260B1) ", use alkali metal hydroxide to carry out the chemical roughen processing to plastic substrate, and the surface after using plasma bombardment to alligatoring activated, finally use cathode sputtering technology metal refining coating on plastic substrate.2009, the Chinese patent of Zhang Haozhi etc. " a kind of production method for sputtering aluminum foil on surface of plastic (CN1020941177A) ", use magnetron sputtering technique to prepare aluminium foil at pretreated frosting, aluminum foil thickness prepared by the method is even, smooth finish good, high with the plastic substrate bonding strength.In recent years, relevant dry method plastic-metal patent using plasma gas phase deposition technology, particularly magnetron sputtering technique more and more both at home and abroad.Tradition magnetic control spattering target particle ionization level is lower, generally only has 5～15%, causes the magnetron sputtering deposition coating quality still on the low side, and coating mostly is, and columnar crystal structure and the large film base binding performance of residual stress in coating loose porous, that vertically run through are poor.Therefore, improving the plasma body ionization level is the important channel of improving coating quality.Calendar year 2001, the United States Patent (USP) of Kouznetsov etc. " Method and apparatus for magnetically enhanced sputtering(US6296742) ", realize that on conventional magnetron sputtering target peak power reaches the impulsive discharge of MW level, obtain the Cu ionization level up to 70% plasma body, propose thus high-power impulse magnetron sputtering (High Power Pulsed Magnetron Sputtering) new technology.High-power impulse magnetron sputtering metallization of plastic surface technique is compared with traditional magnetron sputtering metallization of plastic surface technique, it effectively improves the plasma body ionization level by impulsive discharge, be accompanied by the raising of plasma body ionization level, plasma body strengthens the bombardment effect of plastic substrate, coating is changed into fine and closely woven equiax crystal structure and is strengthened plasma body transportation mechanism by columnar crystal structure, significantly improving around the plating ability of sputtering particle, make to be deposited on the densification of plastic workpiece surface coating structure, film-substrate cohesion is strong, coating ability to the Special plastic workpiece surface improves, in addition by reasonably formulating deposition and process for cooling time, can effectively control porous plastics workpiece working temperature lower than its heat-drawn wire, guarantee that workpiece does not deform because of overheated in deposition process, realization in Foam Plastic Surface at a high speed, low temperature depositing pure metal or multi-element alloy coat.
The advantage of porous plastics high-power impulse magnetron sputtering method for surface metallation is: be applicable to metalized coated kind extensive, and can be in plastic foam surface deposition pure metal coating or multi-element metal coating; Low temperature depositing, coatingsurface smooth finish and matrix are close and even thickness is controlled; Safety and environmental protection, do not used the Cr that contains used containing chemical plating technology
6+or other toxic effect huge sum of money composition chemical reagent.
Summary of the invention
The invention provides a kind of high-power impulse magnetron sputtering technology bubble metallization of plastic surface method, use metallized plastic prepared by the method to there is the advantages such as metallic coating compact structure, smooth surface, wear-resistant and film-substrate cohesion are strong and but the present invention's metallizing kind is extensive, processing step is easy, safety and environmental protection, do not use chemical plating technology related contain Cr
6+or other toxic effect huge sum of money composition chemical reagent.
The technical scheme that the present invention proposes is: the step that a kind of porous plastics high-power impulse magnetron sputtering method for surface metallation adopts is as follows:
A) porous plastics workpiece surface pre-treatment
Foam Plastic Surface is sealed, cleaned and dry, destressing processing;
B) piece installing, vacuumize, degasification
To be placed in vacuum chamber through the porous plastics of surface preparation, be vacuumized, be evacuated to base vacuum degree 2 * 10
-4pa～8 * 10
-3pa, and pass into rare gas element in backward vacuum chamber, being generally argon gas, gas flow is 40～100sccm, now the vacuum chamber internal gas pressure maintains 6 * 10
-2pa～2 * 10
-1pa, the degasification time is 20～60min;
C) pre-sputtering is cleaned porous plastics workpiece and sputtering target material
First the porous plastics workpiece is carried out to sputter clean, use high power pulsed source apply-100 on the porous plastics workpiece～-400V bias voltage, dutycycle are 80～100%, frequency is that 80～150kHz, inert gas flow are that 40～100sccm, cleaning air pressure are that 1～3Pa, scavenging period are 15～30min, then sputter clean magnetic controlling target, use superpower modulating pulse power supply to apply voltage on magnetic controlling target to be-300～-600V, pulse duration τ
onwith τ interpulse period
offbe that 6～34 μ s, pulse width are that 500～1000 μ s, frequency are that 30～100Hz, inert gas flow are that 60～100sccm, cleaning air pressure are that 0.1～1Pa, scavenging period are 3～5min;
D) high-power impulse magnetron sputtering metal refining coating
Using single target or many targets sputtering sedimentation coating, superpower modulating pulse power supply applies voltage and is-300 on magnetic controlling target～-600V, pulse duration τ
onwith τ interpulse period
offbe 6～14 μ s, pulse width is 500～3000 μ s, frequency is 10～100Hz, inert gas flow is 40～100sccm, it is 0.1～1Pa that work is pressed, peak point current is 10～250A, crest voltage is-350～-700V, peak power is 3～175kW, sedimentation rate is 1～180nm/min, the high-power impulse magnetron sputtering technology is the low-temperature physics gas phase deposition technology, before starting, sputtering sedimentation need not carry out heated baking to workpiece, in the long-time continuous sputter deposition process, workpiece temperature can be increased to 300～550 ℃, in coating, residual thermal stress is crossed conference and is made coating come off in deposition process or ftracture, therefore in the deposited coatings process, be to guarantee that the porous plastics workpiece temperature is not higher than its melting temperature, formulate sectional type high-power impulse magnetron sputtering depositing time and cooling time according to the porous plastics characteristics, every sputtering sedimentation period is 30～1800s, be 30～1800s cooling time, the plastic foam workpiece temperature is controlled in 50～150 ℃ of scopes,
E) cooling, pickup, inspection
Until the porous plastics workpiece, after in vacuum chamber, being cooled to room temperature, take out, be 1～3 hour cooling time, after pickup, porous plastics carried out subsequent examination and the tests such as surface topography, hardness, bonding force;
The pre-treatment of described porous plastics workpiece surface comprises:
A) porous plastics workpiece surface sealing treatment: due to the Foam Plastic Surface porous, pore size differs, metallic coating is difficult to its surface hole defect is well covered, therefore need to carry out sealing treatment to its surface, make metal profiling mould according to porous plastics workpiece shape, mould is placed in after chamber type electric resistance furnace is heated above 20～30 ℃ of temperature of porous plastics fusing point with stove and takes out, by pack into mould put into after resistance furnace heats 3～15min and take out of porous plastics;
B) surface cleaning: use the organic washing agent to carry out the wiping cleaning to the porous plastics that is cooled to room temperature;
C) dry, destressing is processed: porous plastics is placed in to drying baker, and oven temperature is set to 20～80 ℃, constant temperature drying 3～8 hours.
Described method for surface metallation is for the pure metal coating of depositing electrically conductive, heat conducting coating Cu, Al or anti-corrosion coating Cr, for depositing the multi-element alloy coat of hard coat CrN or hard refractory coating TiAlN, TiAlSiN.
The charging voltage that described high power pulsed source adopts is 0～-200V, pulse-repetition are that 5～500kHz, dutycycle are 50～100%, the charging voltage that described superpower modulating pulse power acquisition is used is 0～-700V, peak current value reach that 350A, peak power reach 0.32MW, pulse-repetition is 5～500Hz, pulse width 50～3000 μ s, dutycycle 10～50%.
The invention has the beneficial effects as follows: at first the method carries out surface-closed, cleaning and drying, destressing pre-treatment to Foam Plastic Surface, then fills sample, vacuumizes, degasification; Pre-sputtering is cleaned porous plastics workpiece and sputtering target material; High-power impulse magnetron sputtering metal refining coating, by realizing at the high ionization level of porous plastics workpiece surface, low temperature depositing metallic coating setting pulse position shape, frequency, charging voltage and sputter/cooling time, the metallic coating of preparation smooth surface, compact structure, high film-substrate cohesion; The performances such as finally cooling, pickup, inspection metallization Foam Plastic Surface pattern, hardness and film-substrate cohesion.The advantage of the method is: be applicable to metalized coated kind extensive; The smooth densification of coatingsurface, film-substrate cohesion are strong; The sputtering sedimentation temperature is low, and the plastic foam matrix does not deform; Safety and environmental protection, do not use chemical plating technology related containing Cr
6+chromic acid reagent.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described, further illustrates the minutia of this patent:
Example 1. certain factory require deposition Cu film on the urethane foam workpiece, sedimentation rate 50nm/min, target film thickness 5 μ m.
A) porous plastics workpiece surface pre-treatment
1) porous plastics workpiece surface sealing treatment: according to urethane foam workpiece shape, make metal profiling mould, mould is placed in to chamber type electric resistance furnace and is heated to take out after 150 ℃ of temperature with stove, by porous plastics pack into mould and put into resistance furnace heating 3min after take out.
2) surface cleaning: use the organic washing agent to carry out the wiping cleaning to the urethane foam that is cooled to room temperature, first use acetone, rear use alcohol carries out wiping to the urethane foam workpiece.
3) dry, destressing is processed: urethane foam is placed in to drying baker, and oven temperature is set to 40 ℃, constant temperature drying 4 hours.
B) piece installing, vacuumize, degasification
Be evacuated to base vacuum degree 2 * 10
-4pa passes into argon gas in vacuum chamber, and gas flow is 80sccm, and the vacuum chamber internal gas pressure maintains 1.7 * 10
-1pa, the degasification time is 30min.
C) pre-sputtering is cleaned porous plastics workpiece and sputtering target material
At first the urethane foam workpiece is carried out to sputter clean, use that apply-350V of high power pulsed source bias voltage, dutycycle are 90%, frequency is 30min for 100kHz, argon flow amount 80sccm, cleaning air pressure for 2.5Pa, scavenging period on the porous plastics workpiece; The sputter clean magnetic controlling target, use superpower modulating pulse power supply applies voltage and is-420V, pulse duration τ on magnetic controlling target
onbe 6 μ s and interpulse period τ
offbe that 34 μ s, pulse width are that 1000 μ s, frequency are that 30Hz, argon flow amount are that 80sccm, cleaning air pressure are that 0.3Pa, scavenging period are 3min.
D) high-power impulse magnetron sputtering metal refining coating
Superpower modulating pulse power supply applies voltage on magnetic controlling target
onwith τ interpulse period
offbe 10 μ s and 12 μ s, pulse width be 1000 μ s, frequency be 35Hz, argon flow amount be 80sccm, work press for 0.3Pa, peak point current be 90A, crest voltage for-450V, peak power be that 30kW, sedimentation rate are 50nm/min, are respectively sectional type high-power impulse magnetron sputtering depositing time and cooling time 300s and 180s, deposition, cooling stages multiplicity are 25 times.
E) cooling, pickup, inspection
Be 2 hours cooling time, after pickup, urethane foam carried out the subsequent examination such as surface topography, bonding force.
Example 2. certain factory require depositing Al film on the poly fourfluoroplastics workpiece, sedimentation rate 50nm/min, target film thickness 10 μ m.
A) porous plastics workpiece surface pre-treatment
1) surface cleaning: use the organic washing agent to carry out the wiping cleaning to the poly fourfluoroplastics that is cooled to room temperature, first use acetone, rear use alcohol carries out wiping to the poly fourfluoroplastics workpiece.
2) dry, destressing is processed: poly fourfluoroplastics is placed in to drying baker, and oven temperature is set to 80 ℃, constant temperature drying 4 hours.
B) piece installing, vacuumize, degasification
Be evacuated to base vacuum degree 2 * 10
-4pa passes into argon gas in vacuum chamber, and gas flow is 80sccm, and the vacuum chamber internal gas pressure maintains 1.7 * 10
-1pa, the degasification time is 30min.
C) pre-sputtering is cleaned porous plastics workpiece and sputtering target material
At first the poly fourfluoroplastics workpiece is carried out to sputter clean, use that apply-350V of high power pulsed source bias voltage, dutycycle are 90%, frequency is 30min for 100kHz, argon flow amount 80sccm, cleaning air pressure for 2.5Pa, scavenging period on the porous plastics workpiece; The sputter clean magnetic controlling target, use superpower modulating pulse power supply applies voltage and is-420V, pulse duration τ on magnetic controlling target
onbe 6 μ s and interpulse period τ
offbe that 34 μ s, pulse width are that 1000 μ s, frequency are that 30Hz, argon flow amount are that 80sccm, cleaning air pressure are that 0.3Pa, scavenging period are 3min.
D) high-power impulse magnetron sputtering metal refining coating
Superpower modulating pulse power supply applies voltage on magnetic controlling target
onwith τ interpulse period
offbe 10 μ s and 12 μ s, pulse width be 1000 μ s, frequency be 35Hz, argon flow amount be 80sccm, work press for 0.3Pa, peak point current be 90A, crest voltage for-450V, peak power be that 30kW, sedimentation rate are 50nm/min, are respectively sectional type high-power impulse magnetron sputtering depositing time and cooling time 900s and 300s, deposition, cooling stages multiplicity are 17 times.
E) cooling, pickup, inspection
Be 2 hours cooling time, after pickup, poly fourfluoroplastics carried out the subsequent examination such as surface topography, bonding force.
Claims (4)
1. a porous plastics high-power impulse magnetron sputtering method for surface metallation, it is characterized in that: the step of employing is as follows:
A) porous plastics workpiece surface pre-treatment
Foam Plastic Surface is sealed, cleaned and dry, destressing processing;
B) piece installing, vacuumize, degasification
To be placed in vacuum chamber through the porous plastics of surface preparation, be vacuumized, be evacuated to base vacuum degree 2 * 10
-4pa～8 * 10
-3pa, and pass into rare gas element in backward vacuum chamber, being generally argon gas, gas flow is 40～100sccm, now the vacuum chamber internal gas pressure maintains 6 * 10
-2pa～2 * 10
-1pa, the degasification time is 20～60min;
C) pre-sputtering is cleaned porous plastics workpiece and sputtering target material
First the porous plastics workpiece is carried out to sputter clean, use high power pulsed source apply-100 on the porous plastics workpiece～-400V bias voltage, dutycycle are 80～100%, frequency is that 80～150kHz, inert gas flow are that 40～100sccm, cleaning air pressure are that 1～3Pa, scavenging period are 15～30min, then sputter clean magnetic controlling target, use superpower modulating pulse power supply to apply voltage on magnetic controlling target to be-300～-600V, pulse duration τ
onwith τ interpulse period
offbe that 6～34 μ s, pulse width are that 500～1000 μ s, frequency are that 30～100Hz, inert gas flow are that 60～100sccm, cleaning air pressure are that 0.1～1Pa, scavenging period are 3～5min;
D) high-power impulse magnetron sputtering metal refining coating
Using single target or many targets sputtering sedimentation coating, superpower modulating pulse power supply applies voltage and is-300 on magnetic controlling target～-600V, pulse duration τ
onwith τ interpulse period
offbe 6～14 μ s, pulse width be 500～3000 μ s, frequency be 10～100Hz, inert gas flow be 40～100sccm, work press be 0.1～1Pa, peak point current be 10～250A, crest voltage be-350～-700V, peak power are that 3～175kW, sedimentation rate are 1～180nm/min; Formulate sectional type high-power impulse magnetron sputtering depositing time and cooling time according to the porous plastics characteristics, every sputtering sedimentation period is that 30～1800s, cooling time are 30～1800s, and the plastic foam workpiece temperature is controlled in 50～150 ℃ of scopes;
E) cooling, pickup, inspection
Until the porous plastics workpiece, after in vacuum chamber, being cooled to room temperature, take out, be 1～3 hour cooling time, after pickup, porous plastics carried out subsequent examination and the tests such as surface topography, hardness, bonding force.
2. porous plastics high-power impulse magnetron sputtering method for surface metallation according to claim 1, it is characterized in that: the pre-treatment of described porous plastics workpiece surface comprises:
A) porous plastics workpiece surface sealing treatment: according to porous plastics workpiece shape, make metal profiling mould, mould is placed in after chamber type electric resistance furnace is heated above 20～30 ℃ of temperature of porous plastics fusing point with stove and takes out, by pack into mould put into after resistance furnace heats 3～15min and take out of porous plastics;
B) surface cleaning: use the organic washing agent to carry out the wiping cleaning to the porous plastics that is cooled to room temperature;
C) dry, destressing is processed: porous plastics is placed in to drying baker, and oven temperature is set to 20～80 ℃, constant temperature drying 3～8 hours.
3. porous plastics high-power impulse magnetron sputtering method for surface metallation according to claim 1, it is characterized in that: described method for surface metallation is for the pure metal coating of depositing electrically conductive, heat conducting coating Cu, Al or anti-corrosion coating Cr, for depositing the multi-element alloy coat of hard coat CrN or hard refractory coating TiAlN, TiAlSiN.
4. porous plastics high-power impulse magnetron sputtering method for surface metallation according to claim 1, it is characterized in that: the charging voltage that described high power pulsed source adopts is 0～-200V, pulse-repetition are that 5～500kHz, dutycycle are 50～100%, the charging voltage that described superpower modulating pulse power acquisition is used is 0～-700V, peak current value reach that 350A, peak power reach 0.32MW, pulse-repetition is 5～500Hz, pulse width 50～3000 μ s, dutycycle 10～50%.
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| CN104975265B (en) * | 2015-06-25 | 2018-11-30 | 苏州爱迪尔镀膜科技有限公司 | High molecular synthetic material corrosion-resistant coating treatment process |
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| CN110055501A (en) * | 2019-04-17 | 2019-07-26 | 厦门阿匹斯智能制造系统有限公司 | A kind of method of semidry method continuous type PVD plated film plastic metal temperature control |
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| CN110850609A (en) * | 2019-11-21 | 2020-02-28 | 中国电子科技集团公司第二十六研究所 | Low-stress acousto-optic device and preparation method thereof |
| CN111962034A (en) * | 2020-08-14 | 2020-11-20 | 深圳后浪电子信息材料有限公司 | Copper-clad plate and high-speed vacuum preparation method thereof |
| CN111962034B (en) * | 2020-08-14 | 2022-11-01 | 深圳后浪电子信息材料有限公司 | Copper-clad plate and high-speed vacuum preparation method thereof |
| CN112831767A (en) * | 2021-01-04 | 2021-05-25 | 中国航空制造技术研究院 | Composite processing method for metallized film on surface of composite material |
| CN113061859A (en) * | 2021-03-19 | 2021-07-02 | 成都齐兴真空镀膜技术有限公司 | Metal coating for X-ray tube anode target and preparation method thereof |
| CN114369798A (en) * | 2021-12-14 | 2022-04-19 | 核工业西南物理研究院 | Film plating method for low-temperature vacuum ion plating of plastic surface |
| CN117418207A (en) * | 2023-12-19 | 2024-01-19 | 山西农业大学 | Three-target high-power pulse magnetron co-sputtering method |
| CN117418207B (en) * | 2023-12-19 | 2024-02-20 | 山西农业大学 | Three-target high-power pulse magnetron co-sputtering method |
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