CN110724941B - Method for preparing porous metal film by chemical plating process - Google Patents
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- CN110724941B CN110724941B CN201911175839.8A CN201911175839A CN110724941B CN 110724941 B CN110724941 B CN 110724941B CN 201911175839 A CN201911175839 A CN 201911175839A CN 110724941 B CN110724941 B CN 110724941B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1834—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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Abstract
本发明公开了一种化学镀工艺制备多孔金属膜的方法，包括以下步骤：(1)配置催化溶液：配置第一硅烷、第二硅烷、乙醇、水性聚合物溶液和水的混合溶液，在搅拌的过程中加入氨水调节pH值为9，常温搅拌1‑30min后，采用柠檬酸调节pH为7，在加入1‑200g/L的催化剂离子溶液，搅拌1‑30min后加入异丙醇，即得催化溶液；(2)活化基材：将上述催化溶液均匀涂覆到衬底表面，60‑150℃下烘1‑30min，即得活化的基材；(3)化学施镀：将活化的基材浸入镀液中施镀，施镀时间为15‑60min，温度为60‑90℃；(4)将施镀后的基材水洗并超声处理，即制得多孔金属膜。
The invention discloses a method for preparing a porous metal film by an chemical plating process. In the process of adding ammonia water to adjust the pH to 9, after stirring at room temperature for 1-30min, adopt citric acid to adjust the pH to 7, add 1-200g/L catalyst ion solution, stir for 1-30min and then add isopropanol to obtain Catalytic solution; (2) Activating base material: uniformly coat the above-mentioned catalytic solution on the surface of the substrate, and bake at 60-150° C. for 1-30 min to obtain an activated base material; (3) chemical plating: the activated base The material is immersed in the plating solution for plating, the plating time is 15-60 min, and the temperature is 60-90 °C; (4) the plated substrate is washed with water and ultrasonically treated to obtain a porous metal film.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a method for preparing a porous metal film by a chemical plating process.
Background
The porous metal membrane has the advantages of simple process flow, controllable aperture, low relative density, high specific strength, high specific surface area, light weight, sound insulation, heat insulation, good permeability, large adhesive force and the like, and has potential application value in a plurality of fields such as military affairs, buildings, ships, aviation industry and the like.
At present, most of porous metal membranes prepared from HDH titanium powder have the pore diameter reduced along with the increase of sintering temperature, and the porous metal membrane prepared by the method has the advantages of controllable pore diameter, easily controlled process, simple equipment and low cost and is widely concerned. For example: patent CN201410176004.5 discloses a porous metal membrane prepared by using stainless steel fiber sintered felt and a preparation method thereof, the method comprises the steps of oxidizing the surface of the stainless steel sintered felt, then placing the oxidized surface into a mixed solution of urea and nickel nitrate, and growing a nickel iron hydrotalcite film in situ on the surface of a stainless steel sintered felt substrate by controlling the reaction conditions such as the reaction temperature, the reaction time and the like. The porous metal membrane prepared by the method reduces the aperture ratio matrix of the porous metal membrane to a great extent, but has low separation precision and can only be used for solid-liquid separation, so the application field of the porous metal membrane is greatly reduced. Patent CN201410834347.6 discloses a method for preparing a high gradient porous metal film, which comprises plugging a porous metal substrate with pre-prepared inorganic powder, coating with metal powder, sintering at high temperature in hydrogen or inert atmosphere to obtain a gradient porous film containing impurities, and washing with chemical reagent (or vacuum infiltration) or removing residual impurities in the film substrate by ultrasonic process to obtain the high gradient porous metal film. Although the porous metal film prepared by the method has good integrity and high gradient, the process is complex and has obvious technical difference with the method.
Disclosure of Invention
The invention aims to provide a method for preparing a porous metal film by a chemical plating process, which can overcome the defects in the prior art, enrich the existing preparation method of the porous metal film and prepare the metal film with a complex shape.
The invention provides a method for preparing a porous metal film by a chemical plating process, which comprises the following steps:
(1) preparing a catalytic solution: preparing a mixed solution of first silane, second silane, ethanol, a water-based polymer solution and water, adding ammonia water to adjust the pH value to 9 in the stirring process, stirring at normal temperature for 1-30min, adjusting the pH value to 7 by using citric acid, adding a 1-200g/L catalyst ion solution, stirring for 1-30min, and adding isopropanol to obtain a catalytic solution;
(2) activating the substrate: uniformly coating the catalytic solution on the surface of a substrate, and drying at 60-150 ℃ for 1-30min to obtain an activated substrate;
(3) chemical plating: immersing the activated base material into a plating solution for plating, wherein the plating time is 15-60min, and the temperature is 60-90 ℃;
(4) and washing the plated base material with water and carrying out ultrasonic treatment to obtain the porous metal film.
Preferably, the first silane in step (1) is at least one of dimethyldimethoxysilane and methyldiethoxysilane.
Preferably, the second silane in step (1) is γ - (2, 3-glycidoxy) propyltrimethoxysilane.
Preferably, the mass fraction of the aqueous polymer solution in step (1) is 1 to 10%.
Preferably, the aqueous polymer solution in step (1) is at least one of sodium carboxymethyl cellulose, polyvinyl alcohol and polyvinylpyrrolidone aqueous solution.
Preferably, the catalyst ion in step (1) is at least one of palladium, gold, platinum and silver.
Preferably, the mass ratio of the first silane to the second silane to the ethanol to the aqueous polymer solution to the water to the isopropanol to the catalyst ion solution in step (1) is 1:0.1-5:2:10-150:0.1-100:10-1000: 0.5-50.
Preferably, the surface of the substrate in step (2) contains active groups, and the active groups include hydroxyl, carboxyl, epoxy, and mercapto.
Preferably, the electroless plating in the step (3) is at least one of electroless copper plating, electroless nickel plating and electroless cobalt plating, and the thickness of the metal plating layer prepared by the electroless plating is 2-5 μm.
Preferably, the ultrasonic treatment in the step (4) is to gradually increase the temperature from 30 ℃ to 120 ℃ at 20 ℃/min, and the ultrasonic medium is liquid paraffin.
Compared with the prior art, the invention has the beneficial effects that: the metal film is prepared by adopting the prepared catalytic solution to catalyze chemical plating reaction, and the separation of the base material and the metal film is realized by combining ultrasonic treatment. The method has the advantages of simple process, controllable aperture and thickness, and capability of preparing the porous metal film with a complex shape.
Drawings
FIG. 1 is an SEM photograph of a copper metal porous membrane according to example 1 of the present invention;
FIG. 2 is an XRD pattern of a porous metal copper film obtained in example 1 of the present invention.
Detailed Description
The embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.
A method for preparing a porous metal film by an electroless plating process comprises the following steps:
(1) preparing a catalytic solution: preparing a mixed solution of first silane, second silane, ethanol, a water-based polymer solution and water, adding ammonia water to adjust the pH value to 9 in the stirring process, stirring at normal temperature for 1-30min, adjusting the pH value to 7 by using citric acid, adding a 1-200g/L catalyst ion solution, stirring for 1-30min, and adding isopropanol to obtain a catalytic solution;
(2) activating the substrate: uniformly coating the catalytic solution on the surface of a substrate, and drying at 60-150 ℃ for 1-30min to obtain an activated substrate;
(3) chemical plating: immersing the activated base material into a plating solution for plating, wherein the plating time is 15-60min, and the temperature is 60-90 ℃;
(4) and washing the plated base material with water and carrying out ultrasonic treatment to obtain the porous metal film.
In the step (1), the first silane is at least one of dimethyldimethoxysilane and methyldiethoxysilane.
The second silane in the step (1) is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
The mass fraction of the aqueous polymer solution in the step (1) is 1-10%.
In the step (1), the aqueous polymer solution is at least one of sodium carboxymethylcellulose, polyvinyl alcohol and polyvinylpyrrolidone aqueous solution.
In the step (1), the catalyst ions are at least one of palladium, gold, platinum and silver.
In the step (1), the mass ratio of the first silane to the second silane to the ethanol to the aqueous polymer solution to the water to the isopropanol to the catalyst ion solution is 1:0.1-5:2:10-150:0.1-100:10-1000: 0.5-50.
The surface of the base material in the step (2) contains active groups, wherein the active groups comprise hydroxyl, carboxyl, epoxy and sulfydryl.
The chemical plating in the step (3) is at least one of chemical copper plating, chemical nickel plating and chemical cobalt plating, and the thickness of the metal plating layer prepared by the chemical plating is 2-5 mu m.
In the step (4), the ultrasonic treatment is to gradually increase the temperature from 30 ℃ to 120 ℃ at a speed of 20 ℃/min and 150 ℃, and the ultrasonic medium is liquid paraffin.
The metal film is prepared by adopting the prepared catalytic solution to catalyze chemical plating reaction, and the separation of the base material and the metal film is realized by combining ultrasonic treatment.
(1) The aperture is controllable: silane in the catalytic solution is hydrolyzed into a hydrophilic phase (Si-Si long chain) which is incompatible with the hydrophilic phase (hydrophilic resin) in the catalytic solution in the film forming process, phase separation is carried out in the film forming process to form a granular structure, in addition, the boiling points of solvents (water, ethanol and isopropanol) in the catalytic solution are different, the volatilization speeds are different in the film forming process, the surface of the catalytic film is also formed into granules, the relative contents of the two phases and different solvents are reasonably controlled, and the regulation and control of the granule size can be realized.
In the chemical plating process, metal ions are deposited on the surface of the catalytic film under the action of catalytic particles on the surface of the catalytic film, and the catalytic solution contains epoxy groups (introduced by second silane), so that the catalytic solution has strong adhesive force with the surface of a substrate (rich in active groups); in addition, only silanol groups, hydroxyl groups and epoxy groups in the catalytic film can adsorb catalyst particles, and the coordination bonds of the groups and the catalyst particles are weaker, so that the adhesion between the plating layer and the catalytic film is weaker, the metal plating layer falls off along the interface of the catalytic layer/the metal film, namely a pore structure is formed on the inner surface of the metal plating layer, and the size of the pores can be adjusted by the size of particles formed on the surface of the catalytic film.
(2) The thickness is controllable: the thickness of the plating layer increases along with the increase of the chemical plating time, and the invention can prepare the porous metal film with no thickness by controlling the chemical plating time and the chemical plating parameters.
(3) Porous metal films of complex shape can be prepared: chemical plating belongs to an in-situ deposition process, a plating layer is deposited on the surface of a substrate as long as a catalytic film is formed on the surface of the substrate, and porous metal films in different shapes can be prepared by controlling the shape of the substrate.
Example 1 of the invention:
a method for preparing a porous metal film by an electroless plating process comprises the following steps:
mixing 0.5 mass percent of hydrophilic polymer aqueous solution with gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and silver nitrate aqueous solution in a relative mass ratio of 75: 20: 5 stirring and mixing at the rotating speed of 500r/min to obtain the primer. Printing the base coating liquid on the surface of a base material, drying the base coating liquid at the temperature of 80 ℃ for 10min, chemically plating copper on the dried base material, wherein the plating time is 15min, the plating temperature is 60 ℃, then washing and ultrasonically treating the plated base material, gradually raising the ultrasonic temperature from 30 ℃ to 120 ℃ at the speed of 20 ℃/min, and obtaining the porous metal copper film by using paraffin as an ultrasonic medium.
As shown in figure 1, the back surface of the metal film is of a porous structure, and the internal structure of the pores is loose. Fig. 2 is a metal film XRD pattern. Diffraction peaks with the 2 theta of 43 degrees, 51 degrees and 74 degrees in an XRD spectrogram are characteristic peaks of face-centered cubic copper, and meanwhile, the half-height width of the characteristic peak of Cu is narrow, impurity phases do not exist, and the crystallinity is good. In conclusion, the process provided by the invention can be used for preparing the porous metal copper film.
Example 2 of the invention:
a method for preparing a porous metal film by an electroless plating process comprises the following steps:
mixing a hydrophilic polymer aqueous solution with a mass fraction of 10% with an aqueous solution of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and silver nitrate according to a relative mass ratio of 95: 20: 5 stirring and mixing at the rotating speed of 800r/min to obtain the primer. Printing the primer solution on the surface of the base material, drying the base material at the temperature of 97 ℃ for 15min, chemically plating copper on the dried base material, wherein the plating time is 26min, the plating temperature is 65 ℃, then washing and ultrasonically treating the plated base material, gradually heating the ultrasonic temperature from 30 ℃ to 127 ℃ at the speed of 20 ℃/min, and obtaining the porous metal copper film by using paraffin as an ultrasonic medium.
Example 3 of the invention:
a method for preparing a porous metal film by an electroless plating process comprises the following steps:
mixing a hydrophilic polymer aqueous solution with a mass fraction of 2% with an aqueous solution of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and silver nitrate according to a relative mass ratio of 115: 20: 5 stirring and mixing at the rotating speed of 1100r/min to obtain the primer. Printing the primer solution on the surface of the substrate, drying the substrate for 20min at 114 ℃, chemically plating nickel on the dried substrate, wherein the plating time is 37min, the plating temperature is 70 ℃, washing the plated substrate with water, carrying out ultrasonic treatment, gradually heating the ultrasonic temperature from 30 ℃ to 134 ℃ at 20 ℃/min, and using paraffin as an ultrasonic medium to obtain the porous metallic nickel film.
Example 4 of the invention:
a method for preparing a porous metal film by an electroless plating process comprises the following steps:
mixing a 4% hydrophilic polymer aqueous solution and an aqueous solution of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and silver nitrate in a relative mass ratio of 135: 20: 5 stirring and mixing at the rotating speed of 1400r/min to obtain the primer. Printing the primer solution on the surface of the substrate, drying the substrate at 131 ℃ for 25min, chemically plating nickel on the dried substrate, wherein the plating time is 48min, the plating temperature is 75 ℃, washing the plated substrate with water, carrying out ultrasonic treatment, gradually heating the ultrasonic temperature from 30 ℃ to 141 ℃ at 20 ℃/min, and taking paraffin as an ultrasonic medium to obtain the porous metallic nickel film.
Example 5 of the invention:
a method for preparing a porous metal film by an electroless plating process comprises the following steps:
mixing 6 mass percent of hydrophilic polymer aqueous solution with gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and silver nitrate aqueous solution according to a relative mass ratio of 155: 20: 5 stirring and mixing at the rotating speed of 1600r/min to obtain the primer. Printing the base coating liquid on the surface of a substrate, drying the base coating liquid at the temperature of 150 ℃ for 30min, chemically plating cobalt on the dried substrate, wherein the plating time is 60min, the plating temperature is 80 ℃, then washing and ultrasonically treating the plated substrate, gradually raising the ultrasonic temperature from 30 ℃ to 150 ℃ at the speed of 20 ℃/min, and obtaining the porous metal film cobalt by using paraffin as an ultrasonic medium.
The construction, features and functions of the present invention are described in detail in the embodiments illustrated in the drawings, which are only preferred embodiments of the present invention, but the present invention is not limited by the drawings, and all equivalent embodiments modified or changed according to the idea of the present invention should fall within the protection scope of the present invention without departing from the spirit of the present invention covered by the description and the drawings.
Claims (10)
1. A method for preparing a porous metal film by a chemical plating process is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a catalytic solution: preparing a mixed solution of first silane, second silane, ethanol, a water-based polymer solution and water, adding ammonia water to adjust the pH value to 9 in the stirring process, stirring at normal temperature for 1-30min, adjusting the pH value to 7 by using citric acid, adding a 1-200g/L catalyst ion solution, stirring for 1-30min, and adding isopropanol to obtain a catalytic solution;
(2) activating the substrate: uniformly coating the catalytic solution on the surface of a substrate, and drying at 60-150 ℃ for 1-30min to obtain an activated substrate;
(3) chemical plating: immersing the activated base material into a plating solution for plating, wherein the plating time is 15-60min, and the temperature is 60-90 ℃;
(4) and washing the plated base material with water and carrying out ultrasonic treatment to obtain the porous metal film.
2. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: in the step (1), the first silane is at least one of dimethyldimethoxysilane and methyldiethoxysilane.
3. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: the second silane in the step (1) is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
4. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: the mass fraction of the aqueous polymer solution in the step (1) is 1-10%.
5. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: in the step (1), the aqueous polymer solution is at least one of sodium carboxymethylcellulose, polyvinyl alcohol and polyvinylpyrrolidone aqueous solution.
6. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: in the step (1), the catalyst ions are at least one of palladium, gold, platinum and silver.
7. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: in the step (1), the mass ratio of the first silane to the second silane to the ethanol to the aqueous polymer solution to the water to the isopropanol to the catalyst ion solution is 1:0.1-5:2:10-150:0.1-100:10-1000: 0.5-50.
8. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: the surface of the base material in the step (2) contains active groups, wherein the active groups comprise hydroxyl, carboxyl, epoxy and sulfydryl.
9. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: the chemical plating in the step (3) is at least one of chemical copper plating, chemical nickel plating and chemical cobalt plating, and the thickness of the metal plating layer prepared by the chemical plating is 2-5 mu m.
10. The method for preparing a porous metal film according to the electroless plating process of claim 1, wherein: in the step (4), the ultrasonic treatment is to gradually increase the temperature from 30 ℃ to 120 ℃ at a speed of 20 ℃/min and 150 ℃, and the ultrasonic medium is liquid paraffin.
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| US6776826B1 (en) * | 2001-07-27 | 2004-08-17 | Gbn Technologies, Inc. | Composition and method for electroless plating of non-conductive substrates |
| CN108754461A (en) * | 2018-05-24 | 2018-11-06 | 合肥学院 | A kind of method of surface of polymer substrates selective chemical plating |
| CN109750284A (en) * | 2019-03-27 | 2019-05-14 | 合肥学院 | A method for electroless plating on the surface of a large substrate |
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| CN101135052B (en) * | 2006-08-30 | 2010-08-18 | 中国科学院大连化学物理研究所 | Method for preparing metallic complex film |
| US20160312365A1 (en) * | 2015-04-24 | 2016-10-27 | Kanto Gakuin School Corporation | Electroless plating method and electroless plating film |
| CN109016778B (en) * | 2017-06-09 | 2020-09-08 | 清华大学 | Method for preparing porous metal composite structure |
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| US6776826B1 (en) * | 2001-07-27 | 2004-08-17 | Gbn Technologies, Inc. | Composition and method for electroless plating of non-conductive substrates |
| CN108754461A (en) * | 2018-05-24 | 2018-11-06 | 合肥学院 | A kind of method of surface of polymer substrates selective chemical plating |
| CN109750284A (en) * | 2019-03-27 | 2019-05-14 | 合肥学院 | A method for electroless plating on the surface of a large substrate |
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| porous MoO2 nanosheets as non-noble bifunctional electrocatalysts for overall water splitting;jin,YS et al;《advanced materials》;20160518;第28卷(第19期);第3785-3790页 * |
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