CN212357369U - Preparation device of silver-plated antibacterial fabric - Google Patents

Preparation device of silver-plated antibacterial fabric Download PDF

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CN212357369U
CN212357369U CN202020997495.0U CN202020997495U CN212357369U CN 212357369 U CN212357369 U CN 212357369U CN 202020997495 U CN202020997495 U CN 202020997495U CN 212357369 U CN212357369 U CN 212357369U
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silver
reaction cavity
reaction chamber
target
substrate
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张仁熙
金成刚
常鹏
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Suzhou Weipeng Electrical Technology Co ltd
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Suzhou Weipeng Electrical Technology Co ltd
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Abstract

The utility model discloses a preparation facilities of silver-plated antibacterial fabric, including reaction cavity, plasma power and vacuum suction pump, vacuum suction pump and the inside intercommunication of reaction cavity, positive electrode and negative electrode of being connected with plasma power two poles of the earth are installed respectively to the inside both sides of reaction cavity, bottom installation target platform in the reaction cavity, reaction cavity middle part movable mounting shield cover, sputtering gas entry is seted up to the reaction cavity lateral wall between target platform and the shield cover, reaction cavity top installation substrate platform, and modified gas entry is seted up to reaction cavity top and another lateral wall that the sputtering gas entry is relative. Compared with the prior art, the utility model adopts an integrated modification-sputtering reaction cavity form, and has compact and reasonable structure; the distance between the substrate table and the target table can be adjusted, and the thickness of the coating can be conveniently controlled.

Description

Preparation device of silver-plated antibacterial fabric
Technical Field
The utility model relates to a functional fabric processing technology field, concretely relates to silver-plated antibacterial fabric's preparation facilities.
Background
The metallization of the fabric surface is one of the important ways for realizing the composite functionalization of materials, silver has very effective broad-spectrum antibacterial property in all metals, and no report that a human body is allergic to pure silver is found so far, so that a layer of silver is deposited on the surface of fabric materials such as fibers to obtain silver fibers, and the silver fibers have the functions of resisting bacteria, deodorizing and the like, so that the fiber materials can be widely applied to the fields of medical treatment, air purification, antibacterial textiles, food preservation and the like. Silver-based antibacterial agents have been recognized as functional textiles using silver as an antibacterial agent by virtue of their high efficacy, broad spectrum and non-drug resistance, and have been rapidly developed in recent years. However, silver as an inorganic metal has poor bonding property with fibers, and the silver-containing antibacterial fabric has the disadvantages of easy shedding of silver, poor stability and non-persistent antibacterial property, and a preparation method of a silver-based antibacterial fabric with better antibacterial property, high stability and low cost still needs to be further developed.
The prior fiber surface silver plating technology mainly comprises electroplating, chemical plating and vacuum plating. The first and the last Electroplating (Electroplating) technique was used, in which silver ions in an Electroplating solution are reduced on a cathode by an external current and plated on the surface of a fiber substrate. However, the method has the problems of poor bonding force between the plating layer and the substrate, easy stripping of the plating layer, large internal stress of the plating layer, easy cracking and foaming and the like, and the substrate needs pretreatment and post-treatment in the electroplating process, so the process is complicated, and therefore, the method is rarely applied to silver plating on fiber fabrics.
The Electroless plating (Electroless plating) technique is a highly selective method, which uses a suitable reducing agent in solution to reduce silver ions and deposit the silver ions on the surface of the fiber under the action of catalysis of certain metals or other methods. The chemical silver plating method has simple process and easy realization, because of being taken attention. However, the fiber obtained by silver plating has lower plating fastness and poor binding force, so the application range is narrower, and the problems of low production efficiency, high cost, environmental pollution and the like exist. The Lnlin's Utility model patent 200710013290.3, a stable and multiple replenishment method for chemical silver plating of fibers, discloses a method for chemical silver plating of fibers, which relates to pretreatment of multiple processes of deoiling, coarsening and sensitization and chemical plating solution consisting of multiple chemical components. The patent application No. 00110169.2 of Chinese utility model discloses a method for preparing low resistivity conductive fiber, and relates to a chemical plating solution composed of multiple components. In the patent application 'a method and a device for vertical winding continuous chemical silver plating for flexible fabric' of Chinese utility model with application number 201410190506.3, a silver plating method for vertical winding operation coating of fabric and continuous replenishment of chemical plating solution is disclosed. In the patent application "chemical silver plating equipment for fabric and its special method" with application number 201210156524.0, a method for preventing the generation of a large amount of irritant gas when cleaning the chemical silver plating equipment with concentrated nitric acid after metal deposition is proposed.
The vacuum plating technology is also called Physical Vapor Deposition (PVD) method, which comprises vacuum evaporation, vacuum sputtering, vacuum ion plating and the like, the plating surface of the vacuum fiber silver plating method is uniform and compact, the shape retention is very good, the defect density is low, the original performance of the non-metal base material is kept, and the vacuum fiber silver plating method also has various functional characteristics of natural silver, and is the optimal scheme of the current high-quality silver-plated antibacterial fabric.
However, the conventional vacuum silver plating process is complex and troublesome because the substrate is required to be strictly cleaned. In the chinese utility model patent application No. 200410024079.8, "method for preparing silver-plated fabric", a vacuum ion plating method for preparing soft electromagnetic shielding fabric is disclosed. The patent application No. 201110351496.3 of the Chinese utility model entitled "preparation method of silver-plated fiber fabric" also discloses a vacuum sputtering method for preparing silver-plated fiber fabric with antibacterial and bacteriostatic effects. The fiber base material has poor surface polarity, the surface energy of the surface of the fiber material is low, the fiber material is chemically inert, the surface is polluted, a weak boundary layer exists and the like, so that the bonding strength of the silver coating and the base material is not enough, and the silver coating is easy to peel off when being subjected to external forces such as bending, friction, scouring and the like, so that the antibacterial and bacteriostatic effects are lost. Therefore, the development of a vacuum plating process with compact and uniform plating layer, stable antibacterial effect, high speed and good adhesive force has strong practical requirements.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a preparation facilities of preparation silvering antibacterial fiber that efficient, strong adaptability, silver-plated layer are fine and close stable.
The utility model discloses a reach above-mentioned purpose, specifically can realize through following technical scheme:
the utility model provides a preparation facilities of silver-plated antibiotic fabric, including reaction chamber, plasma power and vacuum suction pump, the vacuum suction pump communicates with the reaction chamber is inside, the inside both sides of reaction chamber are installed respectively with the positive electrode and the negative electrode of plasma power two poles of the earth connection, the bottom installation target platform in the reaction chamber, reaction chamber middle part movable mounting shield cover, sputtering gas entry is seted up to the reaction chamber lateral wall between target platform and the shield cover, reaction chamber top installation substrate platform, the modified gas entry is seted up to the reaction chamber top and another lateral wall relative with the sputtering gas entry.
Furthermore, the fabric substrate is fixed on a substrate table, the target is placed on the target table, and the distance between the target table and the substrate table is 50-400 mm.
Furthermore, a vertical adjusting mechanism is arranged between the target material table and the base material table, and the distance between the target material table and the base material table is adjusted through the vertical adjusting mechanism.
Further, the power of the plasma power supply is 6000-.
Compared with the prior art, the utility model adopts an integrated modification-sputtering reaction cavity form, and has compact and reasonable structure; the thickness of the coating can be conveniently controlled by adjusting the distance between the substrate table and the target table; is suitable for multi-process step operation under high voltage condition on the textile fiber.
Drawings
FIG. 1 is a schematic structural view of a manufacturing apparatus of the present invention;
fig. 2 is a schematic flow chart of the preparation method of the present invention.
In the figure, 1, a reaction chamber; 11. a positive electrode; 12. a negative electrode; 13. a target table; 14. a shield case; 15. a sputtering gas inlet; 16. a substrate table; 17. a modified gas inlet; 2. a plasma power supply; 3. a vacuum suction pump.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1 and 2, the utility model provides a preparation facilities of silver-plated antibacterial fabric, the device includes reaction chamber 1, plasma power 2 and vacuum suction pump 3, vacuum suction pump 3 and the inside intercommunication of reaction chamber 1, positive electrode 11 and negative electrode 12 with 2 two pole connections of plasma power are installed respectively to the inside both sides of reaction chamber 1, bottom horizontal installation target platform 13 in reaction chamber 1, reaction chamber 1 middle part movable mounting shield cover 14, sputter gas entry 15 is seted up to reaction chamber 1 lateral wall between target platform 13 and the shield cover 14, reaction chamber 1 top horizontal installation substrate platform 16, modified gas entry 17 is seted up to reaction chamber 1 top and another lateral wall relative with sputter gas entry 15.
In the specific embodiment, the fabric substrate is fixed on a substrate table 16, the target is placed on a target table 13, the distance between the target table 13 and the substrate table 16 is 50-400mm, a vertical adjusting mechanism is arranged between the target table 13 and the substrate table 16, and the distance between the target table 13 and the substrate table 16 is adjusted through the vertical adjusting mechanism.
Preferably, the power of the plasma power supply 2 is 6000-.
The reaction cavity 1 is a surface modification-sputtering integrated chamber and is used for cavity body of fiber substrate surface modification pretreatment and vacuum sputtering, and the two links are completed in the same cavity body; the positive electrode 11 and the negative electrode 12 are electrodes for gas ionization, and are respectively externally connected with a plasma power supply 2; the plasma power supply 2 is a plasma high-voltage power supply for exciting the reaction gas to perform gas ionization. The substrate table 16 is used for fixing the fiber substrate, and generally adopts a clamping mode; the target table 13 is used for placing a silver alloy target, and the silver alloy is a silver-rare earth metal element alloy, preferably a silver-cerium alloy. The shielding cover 14 is used for shielding the silver alloy target table 13 in the surface modification pretreatment link of the fabric substrate, so that the silver alloy target is prevented from being polluted by reaction gas; the sputtering gas inlet 15 is an inlet for introducing sputtering gas; the modified gas inlet 17 is an inlet for a reactive gas for the surface modification pretreatment of the textile substrate. The top of the reaction cavity 1 is provided with a vacuum suction hole 18, the vacuum suction pump 3 is communicated with the inside of the reaction cavity 1 through the vacuum suction hole, and the integrated reaction cavity 1 reaches the required vacuum degree through air suction.
Utilize the utility model discloses a method for preparing silver-plated antibacterial fabric with preparation facilities, including following step:
s1, fabric surface modification pretreatment: placing a fabric substrate on a substrate table 16 of a reaction cavity 1, vacuumizing the reaction cavity 1 to be not more than 10Pa, closing a shielding cover 14, filling modified reaction gas, selecting the type of the modified reaction gas according to different fabric substrate types, starting a plasma power supply 2 for modification treatment, wherein the voltage is 1000-1300V, the current is 6-10A, the reaction pressure is 10-200Pa, and the reaction time is 3-25 s;
s2, sputtering coating treatment: after the modification pretreatment process is finished, the shielding cover 14 is opened, the vacuum suction pump 3 is started for suction at the same time, and the reaction cavity 1 is vacuumized to be not more than 10-3Pa, filling sputtering reaction gas which is one or two or more of argon, nitrogen, helium and krypton, preferably argon or mixed gas of argon and nitrogen; and (2) starting a plasma power supply to perform sputtering coating treatment by taking silver alloy as a target, wherein the voltage is 1000-2500V, the current is 8-12A, the sputtering reaction pressure is not more than 10Pa, the distance between the fiber substrate table 16 and the target table 13 is adjusted, the deposition rate is controlled to be not more than 40nm/min, and the coating thickness is not more than 200 nm.
The method for preparing the silver-plated antibacterial fiber comprises two processes, wherein one process is a fabric surface pretreatment modification process, and the other process is a vacuum sputtering coating process.
In the pretreatment modification link, the fiber base material is subjected to surface modification treatment by using a low-pressure gas discharge reaction, because the energy of high-activity particles generated by gas discharge is higher than the energy of most chemical bonds, the particles in a high-energy state bombard the surface of the fiber material, molecular chains are broken, reactions such as crosslinking, chemical modification, etching and the like are generated, interface chemical reactions between gas and solid phases are initiated, and simultaneously, gaseous products generated by surface etching are mixed with ionized gas due to the interface chemical reactions.
After the surface of the fiber substrate is modified, the fiber substrate enters a vacuum sputtering link to be subjected to silver plating treatment. The smaller the seed crystal size of the silver coating and the better the particle dispersibility, the better the sterilization and bacteriostasis effects, in the application, the silver alloy target is adopted, and the difference of atomic numbers of elements in the silver alloy is utilized, so that the sputtering target atomic momentum is different, the deposition rates of different elements on the fiber base material are different, and finally the film with good dispersibility is formed.
In a specific embodiment, when the fabric substrate is a natural plant fiber fabric, the modifying reaction gas in step S1 is a mixture of one or more of oxygen, carbon monoxide and argon, preferably oxygen or a mixture of oxygen and argon.
When the fabric base material is a natural animal fiber fabric, the modified reaction gas is one or a mixture of two or more of ammonia gas, nitrogen gas, argon gas and helium gas, and preferably argon gas or a mixture of argon gas and ammonia gas.
When the fabric base material is a polyester fiber fabric, the modified reaction gas is one or a mixture of two or more of ammonia gas, monomethylamine, hydrogen gas and nitrogen gas, preferably ammonia gas or a mixture of ammonia gas and nitrogen gas.
When the fabric substrate is a polypropylene fiber fabric, the modifying reaction gas is oxygen, carbon monoxide, methanol or methyl ether, preferably oxygen.
When the fabric base material is a nylon fiber fabric, the modified reaction gas is one or a mixture of two or more of ammonia gas, monomethylamine, hydrogen gas, nitrogen gas, argon gas and helium gas, and preferably ammonia gas or a mixture of ammonia gas and argon gas.
When the fabric base material is acrylic fiber fabric, the modifying reaction gas is oxygen, carbon monoxide, methanol or methyl ether, preferably oxygen.
When the fabric substrate is a spandex-based fabric, the modifying reaction gas is oxygen, acetone, nitrogen dioxide, carbon monoxide, methanol or methyl ether, preferably oxygen.
When the fabric substrate is vinylon fiber fabric, the modified reaction gas is one or a mixture of two or more of monomethylamine, dimethylamine, trimethylamine, ammonia, hydrogen, nitrogen, argon and helium, preferably monomethylamine or a mixture of monomethylamine and argon.
When the fabric base material is a polyvinyl chloride fiber fabric, the modified reaction gas is one or a mixture of two or more of nitrogen, helium, argon, carbon monoxide, methanol and methyl ether, and preferably oxygen or a mixture of oxygen and argon.
The preparation method of the utility model is different according to the components and the structure of the fiber material, the surface energy, the chemical inertia degree, the weak boundary layer on the surface and other properties are different, and the corresponding reactivity on the surface is also different. Therefore, when the material is subjected to surface treatment, modification treatment is performed using reaction gases in different atmospheres. In the present application, an oxygen-containing element or an inert gas atmosphere is often used for a material containing an unsaturated chemical bond, and an atmosphere containing hydrogen, nitrogen, or an inert gas is often used for a material containing a saturated chemical bond.
Preferably, functional groups are introduced into the material surface of the fabric substrate by crosslinking or grafting after the fabric surface modification pretreatment of step S1. Thereby changing the polarity, wettability, adhesiveness and other capabilities of the surface of the fiber material and improving the binding force between the subsequent silver plating layer and the surface of the material.
In an embodiment, preferably, a shielding cover is disposed between the target and the substrate table, and the shielding cover is closed when the fabric surface modification pretreatment of step S1 is performed; when the sputter coating process of step S2 is performed, the shield case is opened.
In one embodiment, in step S2, the silver alloy is a silver-rare earth metal alloy; more preferably a silver cerium alloy.
In one embodiment, preferably, in step S2, the target is spaced from the fabric substrate by 50-400mm, and the deposition rate is controlled by adjusting the distance between the target and the fabric substrate. This application is still through the distance of adjusting substrate and target platform, and the thickness of control coating film.
In one embodiment, in step S2, the sputtering reaction gas is one or a mixture of two or more of argon, nitrogen, helium and krypton.
Example one
The surface silver plating treatment is carried out by adopting a polyester fiber substrate with the width of 50cm and the width of 180g per square meter and adopting a surface modification-sputtering integrated reaction chamber, and the distance between a substrate table 16 and a target table 13 is 30 cm.
S1, firstly, starting the vacuum suction pump 3 to enable the vacuum degree of the reaction cavity 1 to be 5Pa, then filling modified reaction gas, adopting ammonia gas as surface modified reaction gas, enabling the reaction pressure to be 30Pa, enabling the reaction time to be 15S, enabling the plasma power supply 2 to output 1200V voltage and enabling the working current to be 10A.
S2, closing the plasma power supply 2, starting the vacuum suction pump 3 to ensure that the vacuum degree of the reaction cavity 1 is 0.002Pa, then filling sputtering gas argon, starting the plasma power supply to perform sputtering coating treatment, wherein the voltage is 1000V, the current is 12A, the sputtering pressure is 8Pa, the deposition rate is 35nm/min, and the coating thickness is 120 nm.
The silver-plated polyester fiber fabric prepared by the method of the embodiment has an antibacterial rate of 98% through antibacterial detection.
Example two
The surface silver plating treatment is carried out by adopting polypropylene fiber base materials with the breadth of 60cm and the width of 160 g/square meter and adopting a surface modification-sputtering integrated reaction chamber, and the distance between a base material table and a target table is 25 cm.
S1, firstly, starting the vacuum suction pump 3 to enable the vacuum degree of the reaction cavity 1 to be 10Pa, then filling modified reaction gas, adopting oxygen as surface modified reaction gas, enabling the reaction pressure to be 35Pa, enabling the reaction time to be 12S, enabling the output voltage of a plasma power supply to be 1100V, and enabling the working current to be 9A;
s2, closing the plasma power supply 2, starting the vacuum suction pump 3 to ensure that the vacuum degree of the reaction cavity 1 is 0.0015Pa, then filling the sputtering gas of argon and nitrogen mixed gas with the volume ratio of 8:1, starting the plasma power supply to perform sputtering coating treatment with the voltage of 2500V, the current of 8A, the sputtering gas pressure of 5Pa, the deposition rate of 40nm/min and the coating thickness of 150 nm.
The silver-plated polypropylene fiber fabric prepared by the method of the embodiment has 99% of bacteriostasis rate through bacteriostasis detection.
EXAMPLE III
The method adopts natural plant fiber base material with the breadth of 50cm and the width of 160 g/square meter, adopts a surface modification-sputtering integrated reaction chamber to carry out surface silver plating treatment, and the distance between a base material platform and a target platform is 40 cm.
S1, firstly, starting the vacuum suction pump 3 to enable the vacuum degree of the reaction cavity 1 to be 8Pa, then filling modified reaction gas, adopting oxygen and argon mixed gas as surface modified reaction gas, wherein the reaction pressure is 200Pa, the reaction time is 25S, the output voltage of the plasma power supply is 1200V, and the working current is 10A;
s2, closing the plasma power supply 2, starting the vacuum suction pump 3 to enable the vacuum degree of the reaction cavity 1 to be 0.0005Pa, then filling a mixed gas of argon and nitrogen which are sputtering gases, wherein the volume ratio of the argon to the nitrogen is 2:1, starting the plasma power supply to perform sputtering coating treatment, the voltage is 1300V, the current is 10A, the sputtering pressure is 5Pa, the deposition rate is 30nm/min, and the coating thickness is 200 nm.
The silver-plated natural plant fiber fabric prepared by the method of the embodiment has an antibacterial rate of 97% by antibacterial detection.
Example four
The surface silver plating treatment is carried out by adopting a vinylon fiber substrate with the width of 50cm and the width of 160 g/square meter and adopting a surface modification-sputtering integrated reaction chamber, and the distance between a substrate table and a target table is 40 cm.
S1, firstly, starting the vacuum suction pump 3 to enable the vacuum degree of the reaction cavity 1 to be 4Pa, then filling modified reaction gas, adopting a mixed gas of monomethylamine and argon as the surface modified reaction gas, wherein the reaction gas pressure is 5Pa, the reaction time is 3S, the output voltage of the plasma power supply is 1000V, and the working current is 8A;
s2, turning off the plasma power supply 2, starting the vacuum suction pump 3 to ensure that the vacuum degree of the reaction cavity 1 is 0.0009Pa, then filling the sputtering gas of helium and krypton with the volume ratio of 1:4, starting the plasma power supply to perform sputtering coating treatment, wherein the voltage is 2000V, the current is 10A, the sputtering pressure is 9Pa, the deposition rate is 20nm/min, and the coating thickness is 100 nm.
The silver-plated vinylon fiber fabric prepared by the method of the embodiment has 99% of bacteriostasis rate through bacteriostasis detection.
The specific embodiments of the present invention are only for explaining the present invention, and are not intended to limit the present invention, and those skilled in the art can make modifications to the present embodiment as required without inventive contribution after reading the present specification, but all the embodiments are protected by patent laws within the scope of the claims of the present invention.

Claims (4)

1. The utility model provides a preparation facilities of silver-plated antibiotic fabric, a serial communication port, including reaction chamber (1), plasma power (2) and vacuum suction pump (3), the vacuum suction pump communicates with the reaction chamber is inside, positive electrode (11) and negative electrode (12) of being connected with plasma power two poles of the earth are installed respectively to the inside both sides of reaction chamber, bottom installation's target platform (13) in the reaction chamber, reaction chamber middle part movable mounting shield cover (14), sputter gas entry (15) are seted up to the reaction chamber lateral wall between target platform and the shield cover, reaction chamber top installation substrate platform (16), modified gas entry (17) are seted up to the reaction chamber top and the relative another lateral wall of sputter gas entry.
2. The apparatus according to claim 1, wherein the fabric substrate is fixed on a substrate table, the target is placed on the target table, and the target table is spaced from the substrate table by a distance of 50 to 400 mm.
3. The apparatus for preparing silver-plated antibacterial fabric according to claim 1, wherein a vertical adjustment mechanism is installed between the target table and the substrate table, and the distance between the target table and the substrate table is adjusted by the vertical adjustment mechanism.
4. The apparatus for preparing silver-plated antibacterial fabric according to claim 1, wherein the power of the plasma power source is 6000-.
CN202020997495.0U 2020-06-03 2020-06-03 Preparation device of silver-plated antibacterial fabric Active CN212357369U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111500991A (en) * 2020-06-03 2020-08-07 苏州卫鹏机电科技有限公司 Preparation method and device of silver-plated antibacterial fabric

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111500991A (en) * 2020-06-03 2020-08-07 苏州卫鹏机电科技有限公司 Preparation method and device of silver-plated antibacterial fabric

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