CN115322014B - Ceramic substrate with metal coating and preparation method thereof - Google Patents
Ceramic substrate with metal coating and preparation method thereof Download PDFInfo
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- CN115322014B CN115322014B CN202211114450.4A CN202211114450A CN115322014B CN 115322014 B CN115322014 B CN 115322014B CN 202211114450 A CN202211114450 A CN 202211114450A CN 115322014 B CN115322014 B CN 115322014B
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- ceramic substrate
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- metal
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5144—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the metals of the iron group
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
Abstract
The invention discloses a ceramic substrate containing a metal coating, which comprises a ceramic substrate, a polyphenol/polyethyleneimine polymerization bonding layer formed on the ceramic substrate through in-situ copolymerization reaction, catalytic sites formed on the polymer bonding layer through ion chelation and reduction reaction, and a metal coating chemically plated on the catalytic sites. The ceramic substrate containing the metal coating with the structure is sintered at high temperature after a chemical plating process, has stable and uniform high conductivity and excellent high-temperature resistance, and can keep good conductivity and mechanical properties after being bent, folded and washed for many times.
Description
Technical Field
The invention relates to a fiber production technology, in particular to a ceramic substrate containing a metal coating and a preparation method thereof.
Background
With the rapid development of flexible electronic technology, various intelligent wearable textile products with the functions of health detection, disease prevention, electromagnetic shielding, energy conversion, storage, man-machine interaction and the like are correspondingly produced. For the wearable fabrics of intelligence, on the one hand need realize to size miniaturization, device lightweight and device system flexibility, extensibility etc. requirement itself, on the other hand must satisfy when it receives under various mechanical deformation and the exogenic action, the stability that electronic device still can maintain normal operating condition. Therefore, the conductive fiber with high conductivity, good mechanical flexibility and long service life is designed and prepared, can meet the deformation requirements of bending, stretching, even folding and the like, and is the research and development core of the intelligent wearable textile field.
On one hand, compared with metal fibers, the textile product has the advantages that the metal nanoparticles deposited on the surface of the textile fibers can meet the requirement of electronic devices on mechanical flexibility, and the interconnected conductive network can realize the rapid transmission of electrons. On the other hand, among many metal deposition systems, electroless plating is receiving attention because of its simple process equipment, low cost and high production efficiency. In particular, electroless plating can perform all-around metal plating of a fiber aggregate having a rough surface and porous inside in a solution against the influence of gravity.
Currently, less research has been done on the production of textile fibers containing metal coatings by electroless plating. On one hand, the surface of the textile fiber needs to be roughened, sensitized and activated to obtain a platable surface with catalytic activity, but the adhesion between the catalyst and the substrate in sensitization and activation is weak, so that the bonding force between the metal plating layer and the substrate is poor; on the other hand, in the chemical plating process, it is a challenge to realize the structural design and quality optimization of the plating layer by controlling factors such as the formula of the plating solution, the selection of a reducing agent, the reaction temperature and time, and the like. In addition, due to the difference in physical properties between metal and textile fibers, when the textile fibers with metal coatings are subjected to alternating cyclic stresses, a build-up of defects can form inside the material, which in turn can degrade the structural properties and ultimately lead to cracking of the metal coating.
The prior art reports that polymer assisted electroless plating is used to prepare polymeric fibers containing metal coatings. For example, zheng et al used polymethacryloxyethyltrimethyl ammonium chloride (PMETAC) to assist electroless plating to produce a film having a resistance of less than 0.2 Ω. Sq -1 According to the copper-plated cotton fabric, one end of a double-end functional group of the PMETAC is firmly combined with a substrate, and the other end of the PMETAC captures a large amount of catalyst ions, so that the resistance of the electrode is only increased by 350% after the electrode is bent for 1000 times with the radius of 5 mm. However, the conductive properties, mechanical properties, and durability of the conductive fiber need to be further improved, and the use of the polymer compound as a substrate has limitations in expanding the application of the conductive fiber in a high temperature (e.g., greater than 500 ℃) environment.
Disclosure of Invention
The invention aims to provide a ceramic substrate containing a metal coating, which is sintered at high temperature after an electroless plating process, has stable and uniform high conductivity and excellent high-temperature resistance, and can keep good conductivity and mechanical properties after being bent, folded and washed for many times.
To achieve the above objects, the present invention provides a ceramic substrate having a metal coating layer, including a ceramic substrate, a polyphenol/polyethyleneimine polymeric tie layer formed on the ceramic substrate through an in-situ copolymerization reaction, catalytic sites formed on the polymeric tie layer through an ion chelation and reduction reaction, and a metal coating layer electroless-plated on the catalytic sites.
Preferably, the ceramic substrate is made of one or any combination of ceramic fibers, ceramic yarns, non-woven ceramic membranes or ceramic felts.
Preferably, the polyphenol is levodopa, tannic acid or curcumin;
the solvent of levodopa is tris (hydroxymethyl) aminomethane hydrochloride;
the solvent of the tannic acid is deionized water;
the solvent of curcumin is absolute ethyl alcohol.
Preferably, the catalytic sites adopt palladium ions, copper ions or nickel ions as catalyst ions for ion chelation and reduction reaction.
Preferably, the metal coating is a copper coating, a nickel coating, a silver coating or a gold coating.
A method for preparing a ceramic substrate based on a metal coating, comprising the steps of:
s1, grafting polyphenol/polyethyleneimine polymer on the surface of a ceramic matrix;
s2, carrying out ion chelation and reduction treatment on the ceramic matrix grafted with the polyphenol/polyethyleneimine polymer obtained in the step S1;
s3, performing chemical plating to deposit metal on the ceramic matrix subjected to ion chelation and reduction in the step S2;
and S4, carrying out high-temperature sintering treatment on the ceramic substrate subjected to chemical plating and metal deposition.
Preferably, step S1 specifically includes the following steps:
s11, soaking the ceramic substrate in a buffer mixed solution containing polyphenol and polyethyleneimine for chemical grafting;
s12, washing the ceramic substrate with the polyphenol/polyethyleneimine polymer;
s13, drying in an oven.
Preferably, step S2 specifically includes the following steps:
s21, immersing the ceramic substrate with the polyphenol/polyethyleneimine polymer bonding layer into an aqueous solution of ammonium tetrachloropalladate, copper sulfate pentahydrate or nickel sulfate hexahydrate for ion chelation and reduction treatment;
s22, cleaning the ceramic substrate with the catalytic active sites by using clear water.
Preferably, step S3 specifically includes the following steps:
s31, immersing the textile substrate with the catalytic active sites into nickel chemical plating solution, copper chemical plating solution, silver chemical plating solution or gold chemical plating solution for chemical plating;
s32, washing with deionized water;
and S33, drying to obtain the ceramic substrate with the metal deposited on the surface.
Preferably, step S4 specifically includes the following steps:
s41, placing the ceramic substrate with the metal deposited on the surface into a muffle furnace in a vacuum environment for high-temperature sintering;
and S42, cooling at room temperature to obtain the ceramic substrate containing the metal coating.
Therefore, the ceramic substrate containing the metal coating with the structure is sintered at high temperature after the chemical plating process, has stable and uniform high conductivity and excellent high-temperature resistance, and can keep good conductivity and mechanical properties after being bent, folded and washed for many times.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 depicts a profile view representing an exemplary nickel-coated ceramic yarn produced by the method depicted in FIG. 1;
FIG. 3 depicts a profile view representing an exemplary nickel-coated ceramic block produced by the method depicted in FIG. 1;
fig. 4 is a scanning electron microscope image of a nickel coated ceramic yarn of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the present embodiment is based on the technical solution, and the detailed implementation and the specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
FIG. 1 is a schematic flow diagram of the present invention; as shown in fig. 1, the structure of the present invention comprises a ceramic substrate, a polyphenol/polyethyleneimine polymeric tie layer formed on the ceramic substrate by in-situ copolymerization, catalytic sites formed on the polymeric tie layer by ion chelation and reduction reactions, and a metal coating layer electroless-plated on the catalytic sites. Wherein, the ceramic substrate is made of one or any combination of ceramic fiber, ceramic yarn, non-woven ceramic membrane or ceramic felt. Preferably, the polyphenol is levodopa, tannic acid or curcumin; the solvent of levodopa is tris (hydroxymethyl) aminomethane hydrochloride; the solvent of the tannin is deionized water; the solvent of curcumin is absolute ethyl alcohol. Preferably, the catalytic sites adopt palladium ions, copper ions or nickel ions as catalyst ions for ion chelation and reduction reaction. Preferably, the metal coating is a copper coating, a nickel coating, a silver coating or a gold coating.
A method for preparing a ceramic substrate based on a metal coating, comprising the steps of:
s1, grafting polyphenol/polyethyleneimine polymer on the surface of a ceramic matrix;
preferably, step S1 specifically includes the following steps:
s11, soaking the ceramic substrate in a buffer mixed solution containing polyphenol and polyethyleneimine for chemical grafting;
in particular, the ceramic matrix is soaked in mixed buffer solution containing 0.2-5 mg/ml polyphenol and 0.1-2 mg/ml polyethyleneimine for 60-240 minutes, the temperature is 25 ℃, and the stirring speed is 200-600 rpm so as to carry out polymerization.
In this example, type 310 ceramic yarn and a titanium oxide ceramic membrane prepared by 3M company were immersed in a tris (hydroxymethyl) aminomethane hydrochloride buffer solution containing 0.2mg/ml of levodopa and 0.2mg/ml of polyethyleneimine for 240 minutes at 25 ℃ and at a stirring speed of 200rpm to carry out polymerization. The levodopa/polyethyleneimine polymer may be chemically active at the surface of each fiber in the ceramic matrix.
S12, washing the ceramic substrate with the polyphenol/polyethyleneimine polymer;
and S13, drying in an oven.
S2, carrying out ion chelation and reduction treatment on the ceramic matrix grafted with the polyphenol/polyethyleneimine polymer obtained in the step S1;
preferably, step S2 specifically includes the following steps:
s21, immersing the ceramic substrate with the polyphenol/polyethyleneimine polymer bonding layer into an aqueous solution of ammonium tetrachloropalladate, copper sulfate pentahydrate or nickel sulfate hexahydrate for ion chelation and reduction treatment;
in particular, the ceramic substrate with the polyphenol/polyethyleneimine polymer bonding layer is immersed in 5-10 mM of tetrachloropalladate, copper sulfate pentahydrate or nickel sulfate hexahydrate aqueous solution for 1-3 hours for ion chelation and reduction.
In this example, a ceramic substrate with a polyphenol/polyethyleneimine polymeric tie layer was immersed in a 5mM aqueous solution of tetrachloropalladate for 1 hour for ion chelation and reduction. The chloropalladate can be changed into palladium atoms in a reducing environment, and the chloropalladate has the capability of catalyzing and reducing various metal ions, such as Ni 2+ Is catalyzed to be rapidly reduced into metallic Ni particles.
S22, cleaning the ceramic substrate with the catalytic active sites by using clear water.
S3, performing chemical plating to deposit metal on the ceramic matrix subjected to ion chelation and reduction in the step S2;
preferably, step S3 specifically includes the following steps:
s31, immersing the textile substrate with the catalytic active sites into nickel chemical plating solution, copper chemical plating solution, silver chemical plating solution or gold chemical plating solution for chemical plating;
in particular, the ceramic matrix after ion chelation and reduction is immersed in nickel chemical plating solution consisting of 40g/L of nickel sulfate hexahydrate, 20g/L of sodium citrate, 10g/L of lactic acid and 1g/L of dimethylamino borane for 30 to 180 minutes for chemical plating;
in this example, the ceramic substrate after ion chelation and reduction was immersed in a nickel electroless plating solution composed of 40g/L of nickel sulfate hexahydrate, 20g/L of sodium citrate, 10g/L of lactic acid, and 1g/L of dimethylaminoborane. As the chemical time goes on, the nickel layer thickness of the ceramic yarn is increased, so that the conductivity is generated, the resistance is reduced to 3 omega cm < -1 > in the 60-minute chemical plating, and then the ceramic matrix with the metal deposited on the surface is obtained after the washing and the drying by deionized water.
S32, washing with deionized water;
and S33, drying to obtain the ceramic substrate with the metal deposited on the surface.
And S4, carrying out high-temperature sintering treatment on the ceramic substrate subjected to chemical plating and metal deposition.
Preferably, step S4 specifically includes the following steps:
s41, placing the ceramic substrate with the metal deposited on the surface into a muffle furnace in a vacuum environment for high-temperature sintering;
and S42, cooling at room temperature to obtain the ceramic substrate containing the metal coating. The working process comprises the following steps:
the ceramic matrix after metal deposition is put into a vacuum muffle furnace and sintered for 60-120 minutes at the temperature of 200-800 ℃ to regrow metal nano particles, and then the ceramic matrix containing the metal coating with good conductivity and mechanical property is obtained after cooling at room temperature.
In this example, the ceramic substrate after metal deposition was placed in a vacuum muffle furnace, and during high-temperature calcination, the substrate was pre-calcined at 200 ℃ for 1 hour, and then calcined at 800 ℃ for 1 hour. The metal crystal grains can generate metal regrowth under high-temperature reduction, because the metal nano-particles have strong surface activity, the metal nano-particles are mutually attracted and bonded in the high-temperature process, and the high-temperature environment enables the metal nano-particles to obtain enough energy transfer, namely, the small crystal grains are mutually fused to form large crystal grains, and the large crystal grains swallow the small crystal grains. By controlling the pre-calcining time and the calcining time, the metal morphology structure can be effectively controlled, and the flexibility and the conductivity of the ceramic matrix of the compact metal coating can be balanced.
FIG. 2 depicts a profile view representing an exemplary nickel-coated ceramic yarn produced by the method depicted in FIG. 1; FIG. 3 depicts a profile view representing an exemplary nickel-coated ceramic block produced by the method depicted in FIG. 1; fig. 4 is a scanning electron microscope image of the nickel-coated ceramic yarn of the present invention, and as can be seen from fig. 2 to 4, the metal-coated ceramic substrate obtained by the present invention can achieve structural stability at high temperatures. And the ceramic matrix containing the metal coating prepared in the embodiment of the invention can keep the structure unchanged for 48 hours at 600 ℃, and when the temperature reaches 1100 ℃, the conductive ceramic matrix with the compact metal coating can realize the structural stability for 2 hours. In addition, the high-temperature-resistant flexible conductor prepared from the ceramic substrate containing the metal coating can realize bending, folding, knotting and even washing.
Therefore, the ceramic substrate containing the metal coating with the structure is sintered at high temperature after the chemical plating process, has stable and uniform high conductivity and excellent high-temperature resistance, and can keep good conductivity and mechanical properties after being bent, folded and washed for many times.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (7)
1. A ceramic substrate comprising a metal coating, characterized in that: the catalyst comprises a ceramic substrate, a polyphenol/polyethyleneimine polymeric bonding layer formed on the ceramic substrate through in-situ copolymerization reaction, a catalytic site formed on the polymeric bonding layer through ion chelation and reduction reaction, and a metal coating chemically plated on the catalytic site;
the ceramic substrate is made of one or any combination of ceramic fibers, ceramic yarns, non-woven ceramic membranes or ceramic felts;
the polyphenol is levodopa, tannic acid or curcumin;
the solvent of levodopa is tris (hydroxymethyl) aminomethane hydrochloride;
the solvent of the tannic acid is deionized water;
the curcumin solvent is absolute ethyl alcohol;
the preparation method of the ceramic substrate containing the metal coating comprises the following steps:
s1, grafting polyphenol/polyethyleneimine polymer on the surface of a ceramic matrix;
s2, carrying out ion chelation and reduction treatment on the ceramic matrix grafted with the polyphenol/polyethyleneimine polymer obtained in the step S1;
s3, performing chemical plating to deposit metal on the ceramic matrix subjected to ion chelation and reduction in the step S2;
and S4, carrying out high-temperature sintering treatment on the ceramic substrate subjected to chemical plating and metal deposition.
2. The ceramic substrate with the metal coating according to claim 1, wherein: the catalytic sites adopt palladium ions, copper ions or nickel ions as catalyst ions to carry out ion chelation and reduction reactions.
3. The ceramic substrate with the metal coating according to claim 1, wherein: the metal coating is a copper coating, a nickel coating, a silver coating or a gold coating.
4. The ceramic substrate with the metal coating according to claim 1, wherein: the step S1 specifically includes the following steps:
s11, soaking the ceramic substrate in a buffer mixed solution containing polyphenol and polyethyleneimine for chemical grafting;
s12, washing the ceramic substrate with the polyphenol/polyethyleneimine polymer;
and S13, drying in an oven.
5. The ceramic substrate with the metal coating according to claim 1, wherein: the step S2 specifically includes the following steps:
s21, immersing the ceramic substrate with the polyphenol/polyethyleneimine polymer bonding layer into an aqueous solution of ammonium tetrachloropalladate, copper sulfate pentahydrate or nickel sulfate hexahydrate for ion chelation and reduction treatment;
s22, cleaning the ceramic substrate with the catalytic active sites by using clear water.
6. The ceramic substrate with a metal coating according to claim 1, wherein: the step S3 specifically includes the following steps:
s31, immersing the textile substrate with the catalytic active sites into nickel chemical plating solution, copper chemical plating solution, silver chemical plating solution or gold chemical plating solution for chemical plating;
s32, washing with deionized water;
and S33, drying to obtain the ceramic substrate with the metal deposited on the surface.
7. The ceramic substrate with the metal coating according to claim 1, wherein: step S4 specifically includes the following steps:
s41, placing the ceramic substrate with the metal deposited on the surface into a muffle furnace in a vacuum environment for high-temperature sintering;
and S42, cooling at room temperature to obtain the ceramic substrate containing the metal coating.
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| CN115322014B true CN115322014B (en) | 2023-04-11 |
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| JP4544913B2 (en) * | 2004-03-24 | 2010-09-15 | 富士フイルム株式会社 | Surface graft formation method, conductive film formation method, metal pattern formation method, multilayer wiring board formation method, surface graft material, and conductive material |
| CN101003439A (en) * | 2006-11-09 | 2007-07-25 | 中国矿业大学 | Ion implantation of cupper, nickel as pretreatment technique for electroless copper on surface of ceramics |
| FR2944982B1 (en) * | 2009-04-30 | 2011-10-14 | Commissariat Energie Atomique | PROCESS FOR PREPARING A METALLIZED SUBSTRATE, ANDTHE SUBSTRATE AND USES THEREOF |
| CN102995395B (en) * | 2011-09-15 | 2014-12-17 | 香港理工大学 | Conductive textile and its making method |
| BR112019024670A2 (en) * | 2017-05-25 | 2020-06-16 | Basf Se | ARTICLE, PROCESS TO PRODUCE THE ARTICLE AND USES OF AN ARTICLE AND A POLYMERIC BODY |
| CN110265190A (en) * | 2018-03-12 | 2019-09-20 | 深圳先进技术研究院 | A kind of preparation method of three-dimension flexible conductor |
| JP6843455B1 (en) * | 2020-04-27 | 2021-03-17 | 石原ケミカル株式会社 | Nickel colloid catalyst solution for electroless nickel or nickel alloy plating and electroless nickel or nickel alloy plating method |
| CN111635261A (en) * | 2020-06-30 | 2020-09-08 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material and preparation method thereof |
| CN112695305A (en) * | 2020-12-13 | 2021-04-23 | 娄底市精细陶瓷工业技术检测中心(国家电子陶瓷产品质量监督检验中心(湖南)) | Preparation method of high-binding-force electroplated film ceramic resistor |
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