CN102121101A - Method for chemically plating copper without palladium on polyester film - Google Patents
Method for chemically plating copper without palladium on polyester film Download PDFInfo
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- CN102121101A CN102121101A CN 201110043365 CN201110043365A CN102121101A CN 102121101 A CN102121101 A CN 102121101A CN 201110043365 CN201110043365 CN 201110043365 CN 201110043365 A CN201110043365 A CN 201110043365A CN 102121101 A CN102121101 A CN 102121101A
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Abstract
The invention discloses a method for chemically plating copper without palladium on a polyester film, comprising the following steps: firstly removing oil on the polyester film, and optically grafting crylic acid onto the surface of the polyester film by a grafting method, so as to improve the hydrophilism and activity of the surface; then soaking by utilizing ammonia water and a nitric acid sliver solution for activating; and finally carrying out chemical copper plating to realize the metallization of the surface of the polyester film. The method is simple to operate and easy to realize. By utilizing the method, the plasma processing equipment and palladium chloride can be omitted, thereby being beneficial to lowering the cost; and the method can be applied to preparing metal line patterns by an addition process in the circuit board industry.
Description
Technical field
The invention belongs to the metallized technical field of non-metal material surface, relate to a kind of method of on polyester film, not having the palladium electroless copper.
Background technology
Polyester (polyethylene terephthalate, english abbreviation is PET), belong to general engineering plastic, nineteen forty-one has been since raw material makes fiber first by British J.R. Whenfield and J.T. Dikson with terephthalic acid and ethylene glycol, obtained gradually using widely, its membrane product (polyester film, PET film) owing to nontoxic, weathering resistance, chemical stability is good and have the favor that extremely excellent mechanical property is subjected to circuit-board industry, can be used for making flexible circuit board.
But because polyester film wetting ability difference and surface inertness must could carry out electroless copper on its surface through processing such as surface coarsening (as plasma treatment), activation.Use the most general activation method " two-step approach " and " single stage method " arranged." two-step approach " is exactly that the PET film is earlier at SnCl
2Carry out sensitization in the solution and handle, then at PdCl
2Activate in the solution; In order to reduce operation, develop " single stage method ", promptly use SnCl separately
2-PdCl
2The colloid activation solution.More than two kinds of methods, though can on PET, cause the deposition of copper, certain degree of difficulty is arranged, be difficult for deposition and go up copper.In addition, because the PdCl that uses
2Cost an arm and a leg, and relate to SnCl again
2Use, the activation system instability.
Summary of the invention
The objective of the invention is to overcome the deficiency that palladium catalyst costs an arm and a leg in the electroless copper, the apparatus for processing plasma cost is higher, a kind of method of not having the palladium electroless copper on polyester film is provided.Can realize the no palladium electroless copper of PET film, its technical process is as follows: PET film oil removing → PET film load light trigger → UV-light causes gas phase graft acrylic acid → activation → electroless copper.Concrete a kind of method of not having the palladium electroless copper on polyester film may further comprise the steps:
(1) PET film oil removing: put in dehydrated alcohol or the acetone PET film into ultrasonic cleaning 3～5 minutes, ultrasonic cleaning 2～3 minutes in distilled water is then taken out and is dried or dry for standby.
(2) PET film load light trigger: used light trigger is benzophenone (BP), and BP is dissolved in the acetone, and making concentration is the BP solution of 0.3～1.0g/L.The mode of load BP can be directly to coat BP solution on the PET film, dries then; Also can be the PET film to be put in the BP solution soaked 3～15 minutes under the normal temperature, take out then and dry.
(3) UV-light causes the gas phase graft acrylic acid: have the PET film of BP to put in the reaction unit load, the reaction unit synoptic diagram as shown in Figure 1, wherein 1 is acrylic acid solution, 2 is ultraviolet lamp, 3 for answering container, 4 is polyester film (PET film).Used ultraviolet lamp power is 9 watts or 15 watts, and predominant wavelength is 254nm.If the ultraviolet lamp that uses is 9 watts, then the PET film of BP and the distance of ultraviolet lamp are arranged is 1.0～2.0cm in load, and the time of UV-irradiation is 5～30 minutes; If the ultraviolet lamp that uses is 15 watts, then the PET film of BP and the distance of ultraviolet lamp are arranged is 1.0～5.0cm in load, and the time of UV-irradiation is 5～15 minutes.The massfraction of used acrylic acid solution is 10%～50%.
UV-light initiation grafting acrylic acid is a vapor phase process, promptly has load the PET film of BP to put in the reaction unit that is filled with the vinylformic acid steam, initiation grafting vinylformic acid under UV-irradiation.The vinylformic acid steam is by the mode of high pure nitrogen to the acrylic acid solution bubbling produced.
(4) activation: UV-light is caused PET film behind the gas phase graft acrylic acid put in the distilled water ultrasonic cleaning into 2～3 minutes, put the pH value then into and be that normal temperature soaked 10～20 seconds down in 11.50～12.00 the ammonia soln, put the AgNO that concentration is 0.5～1.0g/L again into
3Normal temperature soaked 10～30 seconds down in the solution, put in the distilled water under the normal temperature soaking and washing at last into 2～5 seconds.
(5) electroless copper: the PET film after will activating is put into and is carried out electroless copper in the chemical bronze plating liquid.The use temperature of chemical bronze plating liquid is 40～50 ℃, and using the pH value is 12～13, and the time of electroless copper is 2～10 minutes.Consisting of of used chemical bronze plating liquid: Salzburg vitriol 16g/L; Seignette salt 14g/L; Disodium ethylene diamine tetraacetate 19.5g/L; Sodium hydroxide 14g/L; Formaldehyde 15mL/L.
Beneficial effect of the present invention: the present invention proposes with methods such as grafting, absorption, cause the electroless copper process.Its technical process is: with dehydrated alcohol or acetone PET is carried out oil removal treatment earlier, then load light trigger benzophenone (BP), initiation grafting Acrylic Acid Monomer under UV-irradiation afterwards.Can carry out chemisorption to silver ions behind the Acrylic Acid Monomer in the grafting of pet sheet face, thereby reach the activatory purpose.
The present invention need not to use plasma processing, and technology is simple, and uses AgNO
3Replace PdCl
2As the catalyzer of electroless copper, help reducing cost.
Description of drawings
Fig. 1 is the reaction unit synoptic diagram that UV-light causes the gas phase graft acrylic acid.
Wherein 1 is acrylic acid solution, and 2 is ultraviolet lamp, and 3 is reaction vessel, and 4 is polyester film (PET film).
Embodiment
Embodiment 1
(1) PET film oil removing: put in the dehydrated alcohol PET film into ultrasonic cleaning 5 minutes, ultrasonic cleaning 2 minutes in distilled water then, taking-up is dried.
(2) PET film load light trigger: (BP) is dissolved in the acetone with benzophenone, and making concentration is the BP solution of 0.9g/L, under the normal temperature PET film put in the BP solution and soaks 10 minutes, takes out then and dries.
(3) UV-light causes the gas phase graft acrylic acid: have the PET film of BP to put in the reaction unit that is full of the vinylformic acid steam load, the reaction unit synoptic diagram as shown in Figure 1.Used ultraviolet lamp power is 9 watts, and predominant wavelength is 254nm; It is 1cm that load has the PET film of BP and the distance of ultraviolet lamp; The time of UV-irradiation is 30 minutes; The massfraction of used acrylic acid solution is 50%.
(4) activation: UV-light is caused PET film behind the gas phase graft acrylic acid put in the distilled water ultrasonic cleaning into 2 minutes, put pH value then into and be in 11.75 the ammonia soln normal temperature immersion 15 seconds down, put the AgNO that concentration is 0.5g/L again into
3Normal temperature soaked 15 seconds down in the solution, put in the distilled water under the normal temperature soaking and washing at last into 5 seconds.
(5) electroless copper: the PET film after will activating is put into and is carried out electroless copper in the chemical bronze plating liquid.The temperature of chemical bronze plating liquid is 40 ℃, and the pH value is 12.58, and the time of electroless copper is 2.5 minutes.Consisting of of used chemical bronze plating liquid: Salzburg vitriol 16g/L; Seignette salt 14g/L; Disodium ethylene diamine tetraacetate 19.5g/L; Sodium hydroxide 14g/L; Formaldehyde 15mL/L.
Embodiment 2
(1) PET film oil removing: put in the dehydrated alcohol PET film into ultrasonic cleaning 3 minutes, ultrasonic cleaning 3 minutes in distilled water then, taking-up is dried.
(2) PET film load light trigger: (BP) is dissolved in the acetone with benzophenone, and making concentration is the BP solution of 1.0g/L, under the normal temperature PET film put in the BP solution and soaks 3 minutes, takes out then and dries.
(3) UV-light causes the gas phase graft acrylic acid: have the PET film of BP to put in the reaction unit that is full of the vinylformic acid steam load, the reaction unit synoptic diagram as shown in Figure 1.Used ultraviolet lamp power is 15 watts, and predominant wavelength is 254nm; It is 1cm that load has the PET film of BP and the distance of ultraviolet lamp; The time of UV-irradiation is 5 minutes; The massfraction of used acrylic acid solution is 10%.
(4) activation: UV-light is caused PET film behind the gas phase graft acrylic acid put in the distilled water ultrasonic cleaning into 3 minutes, put pH value then into and be in 11.56 the ammonia soln normal temperature immersion 10 seconds down, put the AgNO that concentration is 0.5g/L again into
3Normal temperature soaked 15 seconds down in the solution, put in the distilled water under the normal temperature soaking and washing at last into 4 seconds.
(5) electroless copper: the PET film after will activating is put into and is carried out electroless copper in the chemical bronze plating liquid.The temperature of chemical bronze plating liquid is 40 ℃, and the pH value is 12.61, and the time of electroless copper is 2.5 minutes.Consisting of of used chemical bronze plating liquid: Salzburg vitriol 16g/L; Seignette salt 14g/L; Disodium ethylene diamine tetraacetate 19.5g/L; Sodium hydroxide 14g/L; Formaldehyde 15mL/L.
Embodiment 3
(1) PET film oil removing: put in the acetone PET film into ultrasonic cleaning 5 minutes, ultrasonic cleaning 3 minutes in distilled water then, taking-up is dried.
(2) PET film load light trigger: (BP) is dissolved in the acetone with benzophenone, and making concentration is the BP solution of 0.3g/L, under the normal temperature PET film put in the BP solution and soaks 15 minutes, takes out then and dries.
(3) UV-light causes the gas phase graft acrylic acid: have the PET film of BP to put in the reaction unit that is full of the vinylformic acid steam load, the reaction unit synoptic diagram as shown in Figure 1.Used ultraviolet lamp power is 9 watts, and predominant wavelength is 254nm; It is 2cm that load has the PET film of BP and the distance of ultraviolet lamp; The time of UV-irradiation is 5 minutes; The massfraction of used acrylic acid solution is 30%.
(4) activation: UV-light is caused PET film behind the gas phase graft acrylic acid put in the distilled water ultrasonic cleaning into 2 minutes, put pH value then into and be in 11.50 the ammonia soln normal temperature immersion 20 seconds down, put the AgNO that concentration is 0.5g/L again into
3Normal temperature soaked 10 seconds down in the solution, put in the distilled water under the normal temperature soaking and washing at last into 2 seconds.
(5) electroless copper: the PET film after will activating is put into and is carried out electroless copper in the chemical bronze plating liquid.The temperature of chemical bronze plating liquid is 42 ℃, and the pH value is 12.59, and the time of electroless copper is 10 minutes.Consisting of of used chemical bronze plating liquid: Salzburg vitriol 16g/L; Seignette salt 14g/L; Disodium ethylene diamine tetraacetate 19.5g/L; Sodium hydroxide 14g/L; Formaldehyde 15mL/L.
(1) PET film oil removing: put in the acetone PET film into ultrasonic cleaning 5 minutes, ultrasonic cleaning 3 minutes in distilled water then, taking-up is dried.
(2) PET film load light trigger: (BP) is dissolved in the acetone with benzophenone, and making concentration is the BP solution of 0.3g/L, under the normal temperature PET film put in the BP solution and soaks 3 minutes, takes out then and dries.
(3) UV-light causes the gas phase graft acrylic acid: have the PET film of BP to put in the reaction unit that is full of the vinylformic acid steam load, the reaction unit synoptic diagram as shown in Figure 1.Used ultraviolet lamp power is 15 watts, and predominant wavelength is 254nm; It is 5cm that load has the PET film of BP and the distance of ultraviolet lamp; The time of UV-irradiation is 5 minutes; The massfraction of used acrylic acid solution is 10%.
(4) activation: UV-light is caused PET film behind the gas phase graft acrylic acid put in the distilled water ultrasonic cleaning into 2 minutes, put pH value then into and be in 12.00 the ammonia soln normal temperature immersion 10 seconds down, put the AgNO that concentration is 1.0g/L again into
3Normal temperature soaked 30 seconds down in the solution, put in the distilled water under the normal temperature soaking and washing at last into 3 seconds.
(5) electroless copper: the PET film after will activating is put into and is carried out electroless copper in the chemical bronze plating liquid.The temperature of chemical bronze plating liquid is 42 ℃, and the pH value is 12.59, and the time of electroless copper is 8 minutes.Consisting of of used chemical bronze plating liquid: Salzburg vitriol 16g/L; Seignette salt 14g/L; Disodium ethylene diamine tetraacetate 19.5g/L; Sodium hydroxide 14g/L; Formaldehyde 15mL/L.
Claims (9)
1. method of not having the palladium electroless copper on polyester film is characterized in that may further comprise the steps:
(1) polyester film carries out ultrasonic cleaning oil removing 3～5 minutes in organic solvent, ultrasonic cleaning 2～3 minutes in distilled water again;
(2) polyester film area load light trigger;
(3) polyester film behind the load light trigger carries out vapor phase process photo-grafting vinylformic acid under UV-irradiation, ultrasonic cleaning 2～3 minutes in distilled water subsequently;
(4) the polyester film normal temperature behind the graft acrylic acid soaked ammonia soln 10～20 seconds earlier down, soaked AgNO again
3Solution carried out activation treatment in 10～30 seconds;
(5) polyester film after the activation is put into and is carried out electroless copper in the chemical bronze plating liquid.
2. method according to claim 1 is characterized in that: the used organic solvent of oil removing is dehydrated alcohol or acetone in the above-mentioned steps (1).
3. method according to claim 1 is characterized in that: used light trigger is a benzophenone in the above-mentioned steps (2), and benzophenone is dissolved in the acetone, and making concentration is the benzophenone solution of 0.3～1.0g/L.
4. method according to claim 1 is characterized in that: use in the above-mentioned steps (3) vapor phase process to carry out ultraviolet radiation graft vinylformic acid, being about to load has the polyester film of light trigger to put into to carry out ultraviolet radiation graft vinylformic acid in the container that is filled with the vinylformic acid steam.
5. method according to claim 4 is characterized in that: the aforesaid propylene acid vapour is by the mode of high pure nitrogen to the acrylic acid solution bubbling produced.
6. according to claim 1 or 4 described methods, it is characterized in that: the power of above-mentioned used ultraviolet lamp is 9 watts or 15 watts, and predominant wavelength is 254nm.
7. according to claim 1 or 4 described methods, it is characterized in that: the concentration of aforesaid propylene acid solution is massfraction 10%～50%.
8. according to claim 1 or 4 described methods, it is characterized in that: the power of above-mentioned ultraviolet lamp is 9 watt-hours, and it is 1.0～2.0cm that ultraviolet lamp and load have the distance of the polyester film of light trigger, and the time of UV-irradiation is 5～30 minutes; The power of ultraviolet lamp is 15 watt-hours, and it is 1.0～5.0cm that ultraviolet lamp and load have the distance of the polyester film of light trigger, and the time of UV-irradiation is 5～15 minutes.
9. method according to claim 1 is characterized in that: used AgNO when carrying out activation treatment in the above-mentioned steps (4)
3The concentration of solution is 0.5～1.0g/L, and the pH value of ammonia soln is 11.5～12.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100433659A CN102121101B (en) | 2011-02-23 | 2011-02-23 | Method for chemically plating copper without palladium on polyester film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100433659A CN102121101B (en) | 2011-02-23 | 2011-02-23 | Method for chemically plating copper without palladium on polyester film |
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| CN102121101A true CN102121101A (en) | 2011-07-13 |
| CN102121101B CN102121101B (en) | 2012-06-27 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517568A (en) * | 2012-01-05 | 2012-06-27 | 惠州市金百泽电路科技有限公司 | Chemical copper plating method for liquid-phase PEG (Polyethylene Glycol) optically-grafted modified PET (Polyethylene Glycol Terephthalate) film |
| WO2013123731A1 (en) * | 2012-02-21 | 2013-08-29 | 北京化工大学 | Cu film on substrate surface, manufacturing method therefor and application thereof |
| CN103774191A (en) * | 2014-02-24 | 2014-05-07 | 襄垣县韩山度假有限责任公司 | Copper plating method of leaf carving artware |
| CN108440780A (en) * | 2018-02-10 | 2018-08-24 | 朱东洋 | A kind of preparation method of the special PET film of polyester copper plating film |
| CN108588006A (en) * | 2018-05-10 | 2018-09-28 | 华东理工大学 | A kind of biological support and its preparation method and application for liver cell dimensional culture |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517568A (en) * | 2012-01-05 | 2012-06-27 | 惠州市金百泽电路科技有限公司 | Chemical copper plating method for liquid-phase PEG (Polyethylene Glycol) optically-grafted modified PET (Polyethylene Glycol Terephthalate) film |
| CN102517568B (en) * | 2012-01-05 | 2013-09-25 | 惠州市金百泽电路科技有限公司 | Chemical copper plating method for liquid-phase PEG (Polyethylene Glycol) optically-grafted modified PET (Polyethylene Glycol Terephthalate) film |
| WO2013123731A1 (en) * | 2012-02-21 | 2013-08-29 | 北京化工大学 | Cu film on substrate surface, manufacturing method therefor and application thereof |
| CN103774191A (en) * | 2014-02-24 | 2014-05-07 | 襄垣县韩山度假有限责任公司 | Copper plating method of leaf carving artware |
| CN108440780A (en) * | 2018-02-10 | 2018-08-24 | 朱东洋 | A kind of preparation method of the special PET film of polyester copper plating film |
| CN108588006A (en) * | 2018-05-10 | 2018-09-28 | 华东理工大学 | A kind of biological support and its preparation method and application for liver cell dimensional culture |
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| Publication number | Publication date |
|---|---|
| CN102121101B (en) | 2012-06-27 |
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Effective date of registration: 20130807 Address after: 518029, Guangdong Province, Shenzhen Futian District Bagua three road deep medicine building, room 5, building 501 Patentee after: Shenzhou Tianze Technology Industrial Co. Ltd. Address before: 510006 Panyu District, Guangzhou, Guangzhou University,, West Ring Road, No. 100 Patentee before: Guangdong University of Technology |
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Correction item: Patentee Correct: Shenzhen Tianze Science Industry Co., Ltd.|518029, Guangdong Province, Shenzhen Futian District Bagua three road deep medicine building, room 5, building 501 False: Shenzhou Tianze Technology Industrial Co. Ltd.|518029, Guangdong Province, Shenzhen Futian District Bagua three road deep medicine building, room 5, building 501 Number: 35 Volume: 29 |
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Free format text: CORRECT: PATENTEE; FROM: SHENZHEN TIANZE TECHNOLOGY INDUSTRY CO., LTD.:518029 SHENZHEN, GUANGDONG PROVINCE TO: SHENZHEN TIANZE SCIENCE INDUSTRY CO., LTD.:518029 SHENZHEN, GUANGDONG PROVINCE |