CN109135196A - A method of electromagnetic shielding material is prepared with aqueous hybrid sizing agent surface modified glass fiber - Google Patents
A method of electromagnetic shielding material is prepared with aqueous hybrid sizing agent surface modified glass fiber Download PDFInfo
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- CN109135196A CN109135196A CN201811017161.6A CN201811017161A CN109135196A CN 109135196 A CN109135196 A CN 109135196A CN 201811017161 A CN201811017161 A CN 201811017161A CN 109135196 A CN109135196 A CN 109135196A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/1095—Coating to obtain coated fabrics
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/12—General methods of coating; Devices therefor
- C03C25/16—Dipping
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/42—Coatings containing inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/465—Coatings containing composite materials
- C03C25/47—Coatings containing composite materials containing particles, fibres or flakes, e.g. in a continuous phase
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a kind of methods with aqueous hybrid sizing agent surface modified glass fiber preparation electromagnetic shielding material, and glass fibre is heat-treated in tube furnace, after being cleaned by ultrasonic in acetone solvent, wash, drying;It is lifted, is placed in thermostatic constant wet chamber after impregnating the glass fibre of drying in aqueous hybrid sizing agent using Best-Effort request device, obtain the modified glass fibre in surface;Glass fabric is made in the modified glass fibre in surface, impregnates in acetone soln, after washing, is soaked in roughening solution, after cleaning, be put into sensitizing solution, after cleaning, be put into activating solution, finally wash;The glass fabric pre-processed is put into main salt solution, ammonium hydroxide tune pH is added, water-bath oscillation adds reducing agent to react, cleans, dries to obtain nickel coated glass fibres fabric;Using hand molding will nickel coated glass fibres fabric infiltrate epoxy resin after be superimposed, be placed on moulded board, first precuring elevated cure again demoulds to obtain electromagnetic shielding material after cooling.
Description
Technical field
The invention belongs to cotton glass fiber applications fields, and in particular to a kind of to use aqueous hybrid sizing agent surface modified glass
The method of fiber preparation electromagnetic shielding material.
Background technique
It is being continuously increased with the development of science and technology with progress, the use of electronic product and equipment, these electronic products all can
Different degrees of electromagnetic radiation is generated, electromagnetic radiation can not only cause mutual interference to electronic product, but also be good for people
Health also has certain harm.Therefore, protection growing interest of the people for electromagnetic radiation.The material of Protection Product is common at present
Metal coating method obtains.There are conductive coating, vacuum coating, sputter coating, spraying using wider metal coating method at present
With plated film etc..In these metal coating techniques, electroless plating technology is a kind of advantageous metal coating method, this be by
It is a kind of easy to operate, low-cost technology in electroless plating method, and gained coating is uniform, and electric conductivity is good, is suitable for multiple
The metal or non-metallic matrix material of miscellaneous shape.The method that chemical plating all can be used in current most fiber metallizes.
The fabric of metallization not only has the flexibility and some excellent properties of itself of fabric, but also possesses metal-plated
The electric conductivity of layer, thus metalized fibers fabric has become a kind of functional new material, in conductive filler, electromagnetic shielding, doctor
There is potential application prospect in the fields such as treatment, memorizing material.Epoxy resin due to good mechanical property, insulation performance and
Building-up property etc. is to be used to prepare the matrix with excellent properties material using more at present, can be with glass fibre, carbon
Fiber and assorted fibre and its fabric etc. are compound to prepare functional composite material, widens it in electronics, national defence and other industry etc.
The application in field.
Application No. is 201710253895.3 Chinese patents, disclose nickel coated glass fibres fabric/epoxy resin electromagnetism
The preparation method of shielding composite, but nickel coated glass fibres fabric/epoxy resin composite material bending strength and impact
Intensity has dropped 53.6%, 14.83% relative to glass fabric/epoxy resin respectively.
For the present invention in a manner of in-situ polymerization, design synthesis aqueous epoxy resins hydridization sizing agent utilizes the aqueous miscellaneous of synthesis
Change sizing agent and glass fabric is made by handling fiberglass surfacing, then by the modified glass fibre in surface, changes
It has been apt to glass fabric to the wettability of matrix epoxy resin, bending strength and the excellent glass fibre-of impact strength is made
Epoxy resin electromagnetic shielding composite material.
Summary of the invention
The purpose of the present invention is being directed to existing problem, provide a kind of fine with aqueous hybrid sizing agent surface modified glass
The method of dimension preparation electromagnetic shielding material, the composite material according to this method production have excellent electromagnetic shielding performance, mechanics
Performance, interface performance and heat resistance.
The present invention is achieved by the following technical solutions:
A method of electromagnetic shielding material is prepared with aqueous hybrid sizing agent surface modified glass fiber, which is characterized in that packet
Include following steps:
(1) aqueous hybrid sizing agent is modified to the surface of glass fibre:
Glass fibre is heat-treated 25-35min in 390-410 DEG C of tube furnace, after being cleaned by ultrasonic 2-4h in acetone solvent, water
It washes 3-5 times, is dried in 75-85 DEG C of baking oven;Using Best-Effort request device, by the glass fibre of drying in aqueous hybrid sizing agent
It after middle dipping 5-15min, is lifted, is placed in 70-75h in thermostatic constant wet chamber, obtain the modified glass fibre in surface;
(2) glass fabric surface pre-treating process:
Glass fabric is made in the modified glass fibre in gained surface in (1), is put into 25-35 DEG C of acetone soln and impregnates
Oil removing 15-25min, wash with distilled water after, be soaked in 55-65 DEG C of roughening solution after 25-35min, clean, place into
15-25min in 30-40 DEG C of sensitizing solution after cleaning, is put into 15-25min in 25-35 DEG C of activating solution, finally clear with distilled water
It washes;
(3) preparation of nickel coated glass fibres fabric:
The glass fabric that gained has pre-processed in (2) is put into 25-35 parts of main salt solution, 1.25-1.75 parts of ammonium hydroxide are added
PH is adjusted, is placed in 75-85 DEG C of water-bath and vibrates, after 8.3-11.7 parts of reducing agent reaction 35-45min are added, clean, dry to obtain plating
Nickel glass fabric;
(4) preparation of electromagnetic shielding material:
90-110 parts of epoxy resin are uniformly mixed with 22.5-27.5 parts of curing agent, using hand molding by gained nickel plating glass in (3)
It is superimposed after glass fabric infiltration epoxy resin, is placed on moulded board, is warming up to 105- after precuring 1-3h at 55-65 DEG C
Solidify 3-5h at 115 DEG C, demoulded after cooling, electromagnetic shielding material is made.
Further, in step (1) aqueous hybrid sizing agent preparation: be added into 8-12 parts of aqueous epoxy curing agents
2.4-3.6 parts of ethyl orthosilicates stir 25-35min, add 0.48-0.72 parts of coupling agent KH550 stirring 5-15min, are added dropwise
After 8-12 parts of aqueous epoxy resins stirring 25-35min, deionized water dilution is added, the water that dioxide-containing silica is 8-12% is made
Property hydridization sizing agent.
Further, acetone soln concentration is 40% in step (2), and roughening solution is the NaOH solution of 40g/L, sensitizing solution
For the SnCl of 30g/L2Solution, activating solution are the PdCl of 0.1g/L2Solution.
Further, in step (3) main salt solution by 30g/L main salt NiSO4·6H2The complexing agent of O and 30g/L
Na3C6H5O7·2H2O composition;Reducing agent is the NaH of 35g/L2PO2·H2O。
The present invention has the advantage that compared with prior art
(1) in a manner of in-situ polymerization, design synthesis aqueous epoxy resins hydridization sizing agent, the mechanical property and heat of hydridization sizing agent
Stability is more excellent, and inorganic particulate size is more uniform in hydridization sizing agent system, and the degree that is uniformly dispersed is good, inorganic particulate with it is organic
There is good interfacial adhesion performance between matrix;Using the aqueous hybrid sizing agent of synthesis by fiberglass surfacing
Reason improves the mechanical property and wettability of fiber, improves glass fabric pair after the processing of aqueous hybrid sizing agent
The wettability of matrix epoxy resin, makes glass fiber reinforced epoxy resin composite material at high temperature, still there is good interface
Binding performance;Galss fiber reinforced resin based composites can be effectively improved using the aqueous hybrid sizing agent of design synthesis
Interface performance and heat resistance.
(2) using glass fabric made of the modified glass fibre in surface as basis material, using the method for chemical plating
It is prepared for nickel-glass fabric, later using nickel-glass fabric as filler, epoxy resin is prepared for as matrix
Nickel coated glass fibres fabric-epoxy resin composite material;Roughening treatment is carried out to glass fabric surface using NaOH solution,
Roughening can be such that the specific surface area of glass fabric and surface-active increases, to improve fabric matrix and the coat of metal
Between caking property.
Specific embodiment
Embodiment 1
A method of electromagnetic shielding material is prepared with aqueous hybrid sizing agent surface modified glass fiber, which is characterized in that packet
Include following steps:
(1) aqueous hybrid sizing agent is modified to the surface of glass fibre:
Glass fibre is heat-treated 25min in 390-410 DEG C of tube furnace, after being cleaned by ultrasonic 2h in acetone solvent, washing 3
It is secondary, it is dried in 75-85 DEG C of baking oven;Using Best-Effort request device, the glass fibre of drying is soaked in aqueous hybrid sizing agent
It after stain 5min, is lifted, is placed in 70h in thermostatic constant wet chamber, obtain the modified glass fibre in surface;
(2) glass fabric surface pre-treating process:
Glass fabric is made in the modified glass fibre in gained surface in (1), is put into 25-35 DEG C of acetone soln and impregnates
Oil removing 15min, wash with distilled water after, be soaked in 55-65 DEG C of roughening solution after 25min, clean, place into 30-40 DEG C
Sensitizing solution in 15min, after cleaning, be put into 15min in 25-35 DEG C of activating solution, finally wash with distilled water;
(3) preparation of nickel coated glass fibres fabric:
The glass fabric that gained has pre-processed in (2) is put into 25 parts of main salt solution, adds 1.25 parts of ammonium hydroxide to adjust pH, sets
It is vibrated in 75-85 DEG C of water-bath, after 8.3 parts of reducing agent reaction 35min are added, clean, dries to obtain nickel coated glass fibres fabric;
(4) preparation of electromagnetic shielding material:
90 parts of epoxy resin are uniformly mixed with 22.5 parts of curing agent, are knitted gained nickel coated glass fibres in (3) using hand molding
It is superimposed after object infiltration epoxy resin, is placed on moulded board, is warming up at 105-115 DEG C and solidifies after precuring 1h at 55-65 DEG C
3h is demoulded after cooling, and electromagnetic shielding material is made.
Further, in step (1) aqueous hybrid sizing agent preparation: into 8 parts of aqueous epoxy curing agents be added 2.4 parts
Ethyl orthosilicate stirs 25min, adds 0.48 part of coupling agent KH550 stirring 5min, 8 parts of aqueous epoxy resins stirrings are added dropwise
After 25min, deionized water dilution is added, the aqueous hybrid sizing agent that dioxide-containing silica is 8% is made.
Further, acetone soln concentration is 40% in step (2), and roughening solution is the NaOH solution of 40g/L, sensitizing solution
For the SnCl of 30g/L2Solution, activating solution are the PdCl of 0.1g/L2Solution.
Further, in step (3) main salt solution by 30g/L main salt NiSO4·6H2The complexing agent of O and 30g/L
Na3C6H5O7·2H2O composition;Reducing agent is the NaH of 35g/L2PO2·H2O。
Embodiment 2
A method of electromagnetic shielding material is prepared with aqueous hybrid sizing agent surface modified glass fiber, which is characterized in that packet
Include following steps:
(1) aqueous hybrid sizing agent is modified to the surface of glass fibre:
Glass fibre is heat-treated 35min in 390-410 DEG C of tube furnace, after being cleaned by ultrasonic 4h in acetone solvent, washing 5
It is secondary, it is dried in 75-85 DEG C of baking oven;Using Best-Effort request device, the glass fibre of drying is soaked in aqueous hybrid sizing agent
It after stain 15min, is lifted, is placed in 75h in thermostatic constant wet chamber, obtain the modified glass fibre in surface;
(2) glass fabric surface pre-treating process:
Glass fabric is made in the modified glass fibre in gained surface in (1), is put into 25-35 DEG C of acetone soln and impregnates
Oil removing 25min, wash with distilled water after, be soaked in 55-65 DEG C of roughening solution after 35min, clean, place into 30-40 DEG C
Sensitizing solution in 25min, after cleaning, be put into 25min in 25-35 DEG C of activating solution, finally wash with distilled water;
(3) preparation of nickel coated glass fibres fabric:
The glass fabric that gained has pre-processed in (2) is put into 35 parts of main salt solution, adds 1.75 parts of ammonium hydroxide to adjust pH, sets
It is vibrated in 75-85 DEG C of water-bath, after 11.7 parts of reducing agent reaction 45min are added, clean, dries to obtain nickel coated glass fibres fabric;
(4) preparation of electromagnetic shielding material:
110 parts of epoxy resin are uniformly mixed with 27.5 parts of curing agent, are knitted gained nickel coated glass fibres in (3) using hand molding
It is superimposed after object infiltration epoxy resin, is placed on moulded board, is warming up at 105-115 DEG C and solidifies after precuring 3h at 55-65 DEG C
5h is demoulded after cooling, and electromagnetic shielding material is made.
Further, in step (1) aqueous hybrid sizing agent preparation: be added 3.6 into 12 parts of aqueous epoxy curing agents
Part ethyl orthosilicate stirs 35min, adds 0.72 part of coupling agent KH550 stirring 15min, 12 parts of aqueous epoxy resins are added dropwise and stir
After mixing 35min, deionized water dilution is added, the aqueous hybrid sizing agent that dioxide-containing silica is 12% is made.
Further, acetone soln concentration is 40% in step (2), and roughening solution is the NaOH solution of 40g/L, sensitizing solution
For the SnCl of 30g/L2Solution, activating solution are the PdCl of 0.1g/L2Solution.
Further, in step (3) main salt solution by 30g/L main salt NiSO4·6H2The complexing agent of O and 30g/L
Na3C6H5O7·2H2O composition;Reducing agent is the NaH of 35g/L2PO2·H2O。
There is excellent electromagnetic shielding performance, mechanical property, interface performance and heat resistance according to the method for the present invention production
Energy;Not do glass fabric-epoxy resin composite material of any modification as blank control, according to the present embodiment system
53% and 69% is respectively increased in interface shear strength of the electromagnetic shielding material of work at room temperature and 150 DEG C, and shielding properties is in 2-
It can achieve 64-76dB within the scope of 18GHz.
Claims (4)
1. a kind of method with aqueous hybrid sizing agent surface modified glass fiber preparation electromagnetic shielding material, which is characterized in that
Include the following steps:
(1) aqueous hybrid sizing agent is modified to the surface of glass fibre:
Glass fibre is heat-treated 25-35min in 390-410 DEG C of tube furnace, after being cleaned by ultrasonic 2-4h in acetone solvent, water
It washes 3-5 times, is dried in 75-85 DEG C of baking oven;Using Best-Effort request device, by the glass fibre of drying in aqueous hybrid sizing agent
It after middle dipping 5-15min, is lifted, is placed in 70-75h in thermostatic constant wet chamber, obtain the modified glass fibre in surface;
(2) glass fabric surface pre-treating process:
Glass fabric is made in the modified glass fibre in gained surface in (1), is put into 25-35 DEG C of acetone soln and impregnates
Oil removing 15-25min, wash with distilled water after, be soaked in 55-65 DEG C of roughening solution after 25-35min, clean, place into
15-25min in 30-40 DEG C of sensitizing solution after cleaning, is put into 15-25min in 25-35 DEG C of activating solution, finally clear with distilled water
It washes;
(3) preparation of nickel coated glass fibres fabric:
The glass fabric that gained has pre-processed in (2) is put into 25-35 parts of main salt solution, 1.25-1.75 parts of ammonium hydroxide are added
PH is adjusted, is placed in 75-85 DEG C of water-bath and vibrates, after 8.3-11.7 parts of reducing agent reaction 35-45min are added, clean, dry to obtain plating
Nickel glass fabric;
(4) preparation of electromagnetic shielding material:
90-110 parts of epoxy resin are uniformly mixed with 22.5-27.5 parts of curing agent, using hand molding by gained nickel plating glass in (3)
It is superimposed after glass fabric infiltration epoxy resin, is placed on moulded board, is warming up to 105- after precuring 1-3h at 55-65 DEG C
Solidify 3-5h at 115 DEG C, demoulded after cooling, electromagnetic shielding material is made.
2. a kind of aqueous hybrid sizing agent surface modified glass fiber preparation electromagnetic shielding material according to claim 1
Method, which is characterized in that the preparation of aqueous hybrid sizing agent in step (1):
2.4-3.6 parts of ethyl orthosilicates are added into 8-12 parts of aqueous epoxy curing agents and stir 25-35min, add 0.48-
0.72 part of coupling agent KH550 stirs 5-15min, and after 8-12 parts of aqueous epoxy resins stirring 25-35min are added dropwise, deionization is added
The aqueous hybrid sizing agent that dioxide-containing silica is 8-12% is made in water dilution.
3. a kind of aqueous hybrid sizing agent surface modified glass fiber preparation electromagnetic shielding material according to claim 1
Method, which is characterized in that in step (2) acetone soln concentration be 40%, roughening solution be 40g/L NaOH solution, sensitizing solution
For the SnCl of 30g/L2Solution, activating solution are the PdCl of 0.1g/L2Solution.
4. a kind of aqueous hybrid sizing agent surface modified glass fiber preparation electromagnetic shielding material according to claim 1
Method, which is characterized in that in step (3) main salt solution by 30g/L main salt NiSO4·6H2The complexing agent of O and 30g/L
Na3C6H5O7·2H2O composition;Reducing agent is the NaH of 35g/L2PO2·H2O。
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Cited By (6)
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CN109705533A (en) * | 2019-01-22 | 2019-05-03 | 重庆纤维研究设计院股份有限公司 | A kind of preparation method of resin/copper facing glass fiber compound material and products thereof and application |
CN111056768A (en) * | 2019-12-02 | 2020-04-24 | 罗登峰 | Low-temperature-resistant asphalt concrete and preparation method thereof |
CN112521029A (en) * | 2020-11-30 | 2021-03-19 | 北京宇航系统工程研究所 | Method for improving thermal conductivity of glass fiber |
CN114105494A (en) * | 2021-10-22 | 2022-03-01 | 北京科技大学 | Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber |
CN114751659A (en) * | 2022-04-19 | 2022-07-15 | 安徽中纤新材料有限公司 | Conductive glass fiber and preparation method thereof |
CN115626781A (en) * | 2022-11-11 | 2023-01-20 | 杭州师范大学 | Metal-plated glass fiber with metal oxide as medium and preparation method thereof |
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---|---|---|---|---|
CN109705533A (en) * | 2019-01-22 | 2019-05-03 | 重庆纤维研究设计院股份有限公司 | A kind of preparation method of resin/copper facing glass fiber compound material and products thereof and application |
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CN112521029A (en) * | 2020-11-30 | 2021-03-19 | 北京宇航系统工程研究所 | Method for improving thermal conductivity of glass fiber |
CN114105494A (en) * | 2021-10-22 | 2022-03-01 | 北京科技大学 | Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber |
CN114105494B (en) * | 2021-10-22 | 2022-10-04 | 北京科技大学 | Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber |
CN114751659A (en) * | 2022-04-19 | 2022-07-15 | 安徽中纤新材料有限公司 | Conductive glass fiber and preparation method thereof |
CN115626781A (en) * | 2022-11-11 | 2023-01-20 | 杭州师范大学 | Metal-plated glass fiber with metal oxide as medium and preparation method thereof |
CN115626781B (en) * | 2022-11-11 | 2023-12-29 | 杭州师范大学 | Metal-plated glass fiber with metal oxide as medium and preparation method thereof |
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Application publication date: 20190104 |