TW202138297A - Method of manufacturing ordered arrangement of graphene-carbon nano tube of metal substrate and composite coatings for carbon deposit - Google Patents

Abstract

The invention discloses a method of manufacturing ordered arrangement of graphene-carbon nano tube of metal substrate and composite coatings for carbon deposit, which deposits sputtering target and penetrating fluid into evacuated penetrating oven in order to make the penetrating fluid penetrates the sputtering target in the evacuated penetrating oven, and places the penetrated sputtering target into evacuated magnetic control sputtering machine and controls cooling water of the evacuated magnetic control sputtering target machine, namely, operates evacuated magnetic control sputtering process on the metal substrate, utilizes the characteristic of metal organic salt of the penetrating fluid that can remain non-magnetic under 150℃before decomposition, decomposes nano metal organic salt particles in high temperature zone after being sputtering and depositing on the metal substrate as catalyst of carbon so the carbon that came from the sputtering target can form carbon structural layer on concave / convex rough portion of the metal substrate. Accordingly, the invention reflects the beneficial effects of being easy and time saving on manufacture.

Description

Manufacturing method of orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on metal substrate

The present invention relates to a manufacturing method of orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on a metal substrate, and in particular refers to a method that is simpler and more convenient in manufacturing, and can save manufacturing man-hours. In its overall implementation and use, it is more practical and functional.

According to the vigorous development of high technology, the volume of electronic components tends to be miniaturized, and the density per unit area is getting higher and higher, and their performance is continuously enhanced. Under these factors, the product quality of electronic components Demand is increasing almost every year.

Among them, as for the metal substrate of common electronic components, the metal substrate is mainly used in the corrosion tank to clean the surface with chemical agents (such as strong acid, strong alkali) to remove oil and rust during the manufacturing process. And after the agent is removed by the neutralization tank and the cleaning tank, and through a plurality of chemical tanks, the surface of the aluminum foil is chemically eroded and corroded to form a plurality of concave-shaped surfaces, and then subjected to neutralization cleaning, strong acid and electrochemical action After forming the oxidation tank of the voltage-resistant oxide layer, the process of making the metal substrate is completed by cleaning the neutralization tank and the drying tank.

However, although the above-mentioned metal substrate manufacturing method can achieve the expected effect of manufacturing the metal substrate, it is also discovered in the actual implementation process that the metal substrate needs to pass through a plurality of different grooves in the production process. The number of different steps not only makes the steps extremely complicated and inconvenient, but also consumes a lot of production man-hours, so that there is still room for improvement in the overall implementation.

The reason is that, in view of this, the inventor upholds many years of rich experience in design, development and actual production in the related industry, and then researches and improves it to provide a metal substrate with an ordered arrangement of graphene carbon nanotubes and a composite coating of carbon deposition. Manufacturing methods in order to achieve the purpose of better practical value.

The main purpose of the present invention is to provide a method for manufacturing graphene carbon nanotubes with metal substrates in an orderly arrangement and carbon deposition composite coating, which is mainly easier and more convenient in manufacturing, and can save manufacturing man-hours. And in its overall implementation and use, it is more practical and functional.

The main purpose and effect of the manufacturing method of the orderly arrangement and carbon deposition composite coating of the graphene carbon nanotubes on the metal substrate of the present invention are achieved by the following specific technical means:

The main system includes the following steps:

A. Graphite sputtering target: Graphite is made into various geometric shapes of magnetron sputtering target;

B. Permeate: Dissolve the organic metal salt in an organic solvent to make it reach saturated solubility to produce a permeate;

C. Infiltration: Put the sputtering target and the permeate into a vacuum infiltration furnace together, and allow the permeate to penetrate into the sputtering target under the vacuum environment in the vacuum infiltration furnace;

D. Metal base material: the metal base material is formed with irregularities on both sides of the surface;

E. Sputtering: Put the sputtering target after the penetration of the penetrating liquid into the vacuum magnetron sputtering machine, control the cooling water in the vacuum magnetron sputtering target machine, and then you can The metal substrate is subjected to vacuum magnetron sputtering operation, and the organic metal salt of the permeate remains non-magnetic before being decomposed at 150°C. After being sputtered, the metal of the nano-organic metal salt is decomposed to the high temperature zone. The particles are deposited on the metal substrate as a catalyst for carbon, so that the carbon from the sputtering target is rapidly bonded to each other to form an ordered carbon structure, which can be formed on the unevenness of the metal substrate Ordered two-dimensional or three-dimensional carbon structure layer.

A preferred embodiment of the method for manufacturing a composite coating of graphene carbon nanotubes with orderly arrangement and carbon deposition on a metal substrate of the present invention, wherein the sputtering target has a graphite content of ≧99.95% and a porosity of 15% ~30%.

A preferred embodiment of the method for manufacturing a composite coating of graphene carbon nanotubes with orderly arrangement and carbon deposition on a metal substrate of the present invention, wherein the vacuum infiltration furnace is provided with a furnace body, and the sputtering target is provided in the furnace body And make the permeate to submerge the sputtering target material in the furnace body, and the furnace body is provided with a vacuum valve connected to the air pressure control device, and the high vacuum pump of the air pressure control device can be used to vacuum the interior of the furnace body Work, and set up a vacuum gauge on the furnace body, and observe the pressure value inside the furnace body through the vacuum gauge.

A preferred embodiment of the method for manufacturing a composite coating of graphene carbon nanotubes with an orderly arrangement and carbon deposition on a metal substrate of the present invention, wherein the furnace body of the vacuum infiltration furnace is connected with a permeate recovery tank through which the infiltration The liquid recovery tank recovers the used permeate for repeated recycling.

The preferred embodiment of the manufacturing method of the ordered arrangement of graphene carbon nanotubes and carbon deposition composite coating of the metal substrate of the present invention, wherein the metal substrate is a high-purity aluminum foil with an aluminum content ≧99.7%, and a copper content 99.7% of any kind of high-purity copper foil.

A preferred embodiment of the method for manufacturing a composite coating of graphene carbon nanotubes with orderly arrangement and carbon deposition on a metal substrate of the present invention, wherein the metal substrate is subjected to rough chemical plating, electrochemical corrosion, and spraying on both sides , Either method of vapor sputtering has uneven roughness formed on the surface.

The preferred embodiment of the manufacturing method of the orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on the metal substrate of the present invention, wherein the vacuum magnetron sputtering target machine is a plane vacuum magnetron sputtering target machine, Any of circular plane vacuum magnetron sputtering target machine, cylindrical magnetic vacuum magnetron sputtering target machine.

The preferred embodiment of the manufacturing method of orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on a metal substrate of the present invention, wherein the target surface of the sputtering target is maintained at most 150°C or less, and at the same time The working temperature in the cavity of the vacuum magnetron sputtering machine is at least 300° C. and the vacuum degree is below 0.1 Pa.

The preferred embodiment of the method for manufacturing a composite coating of graphene carbon nanotubes with orderly arrangement and carbon deposition on a metal substrate of the present invention, wherein the organic metal salt is any one of iron, cobalt, and nickel.

A preferred embodiment of the method for manufacturing a composite coating of graphene carbon nanotubes with orderly arrangement and carbon deposition on a metal substrate of the present invention, wherein the carbon structure layer formed on the concave-convex rough portion of the metal substrate is Any one or a combination of carbon nanotubes and graphene.

In order to make the technical content, the purpose of the invention and the effects achieved by the present invention more complete and clear, the following detailed descriptions are given, and please refer to the disclosed drawings and figure numbers together:

First of all, please refer to the first figure shown in the schematic diagram of the production process of the present invention. The present invention mainly includes the following steps:

A. Graphite sputtering target: High-purity graphite with graphite content ≧99.95% is made into various geometric magnetron sputtering targets, and the porosity of the sputtering target is controlled to be 15%~30%;

B. Penetrant: Dissolve organic metal salts [such as iron, cobalt, nickel, etc.] in an organic solvent to achieve saturated solubility to produce a permeate;

C. Infiltration: Please refer to the second figure as shown in the schematic diagram of the vacuum infiltration furnace of the present invention, and put the sputtering target (1) and the penetrant (2) into the vacuum infiltration furnace (3) together. The vacuum infiltration furnace (3) is provided with a furnace body (31) in which the sputtering target material (1) is provided, and the infiltration liquid (2) is allowed to flood the furnace body (31) Sputtering target material (1), the furnace body (31) is provided with a vacuum valve (311) connected to the air pressure control device (32), and the high vacuum pump of the air pressure control device (32) can be used for the furnace body (31) ) Is vacuumed inside, and the furnace body (31) is provided with a vacuum gauge (312) so that the pressure value inside the furnace body (31) can be observed through the vacuum gauge (312), so that the permeate ( 2) Infiltrate into the sputtering target (1) under the vacuum environment in the furnace body (31), and the furnace body (31) is connected with a permeate recovery tank (33) so that the permeate can pass through The recovery tank (33) recovers the used permeate for repeated recycling;

D. Metal substrate: Metal substrates such as high-purity aluminum foil with aluminum content ≧99.7% or high-purity copper foil with copper content 99.7% are subjected to rough chemical plating or electrochemical corrosion, spraying or evaporation on both sides to Concave and convex rough parts are formed on the surface of the metal substrate;

E. Sputtering: Put the sputtering target (1) after the penetration of the penetrant (2) into the vacuum magnetron sputtering machine (4), the vacuum magnetron sputtering target machine (4) can be Planar vacuum magnetron sputtering target machine [please refer to the third figure together. This invention is applied to the use state of plane vacuum magnetron sputtering target machine as shown in the schematic diagram], circular plane vacuum magnetron sputtering target machine [please again Also refer to the fourth figure. The application of the present invention in the circular plane vacuum magnetron sputtering target machine is shown in the schematic diagram], the cylindrical magnetic vacuum magnetron sputtering target machine [please also refer to the fifth figure. The application of the present invention As shown in the schematic diagram of the use state of the cylindrical magnetic vacuum magnetron sputtering target machine], control the cooling water in the vacuum magnetron sputtering target machine (4) to make the target material of the sputtering target material (1) The surface work is maintained at most below 150°C, and the working temperature in the cavity of the vacuum magnetron sputtering machine (4) is at least 300°C or more, and the vacuum degree is below 0.1Pa. (5) Carrying out vacuum magnetron sputtering operation [please refer to the sixth figure together with the schematic diagram of the vacuum magnetron sputtering operation in the enhanced unbalanced closed magnetic field of the present invention, and the seventh figure of the present invention in the large-scale multi-target unbalanced closing A schematic diagram of a vacuum magnetron sputtering operation state under a magnetic field, Fig. 8 is another schematic diagram of a vacuum magnetron sputtering operation of the present invention, and Fig. 9 is another schematic diagram of a vacuum magnetron sputtering operation of the present invention], The organometallic salt [such as iron, cobalt, nickel, etc.] using the permeate (2) remains non-magnetic before being decomposed at 150°C, and decomposes iron, cobalt, nickel, etc. into the high temperature zone after being sputtered The metal particles of nanoorganometallic salt are deposited on the metal substrate (5), which act as a carbon catalyst, so that the endless carbon atoms or carbon clusters from the sputtering target (1) quickly interact with each other. Bonded to form an ordered carbon structure, and then an ordered two of carbon nanotubes or graphene can be formed on the entire or partial surface of the metal substrate (5). One-dimensional or three-dimensional carbon structure layer (51) [shown in Figure 10, a schematic view of the forming state of the present invention, Figure 11, a schematic view of another forming state of the present invention, and Figure 12, a schematic view of another forming state of the present invention], and The working conditions of the vacuum magnetron sputtering target machine (4) are maintained to control the length or sheet diameter of the carbon structure layer (51) formed on the metal substrate (5).

In this way, the metal substrate (5) can be applied to capacitor electrode foil, super capacitor electrode foil, lithium battery electrode, heat dissipation film, EMI heat dissipation film, and the like.

Based on the above, the description of the use and implementation of the present invention shows that, compared with the prior art, the present invention is mainly simpler and more convenient in manufacturing, and can save manufacturing man-hours, and is implemented in its entirety. Those who use more practical functional characteristics.

However, the foregoing embodiments or drawings do not limit the product structure or usage mode of the present invention, and any appropriate changes or modifications by persons with ordinary knowledge in the relevant technical field should be regarded as not departing from the patent scope of the present invention.

In summary, the embodiments of the present invention can indeed achieve the expected use effect, and the specific structure disclosed by it has not been seen in similar products, nor has it been disclosed before the application, since it has fully complied with the provisions of the patent law. In accordance with the requirements, Yan filed an application for a patent for invention in accordance with the law, and asked for favors for examination and granted a patent.

1: Sputtering target

2: penetrant

3: Vacuum infiltration furnace

31: Furnace

311: Vacuum valve

312: Vacuum gauge

32: Air pressure control device

33: Permeate recovery tank

4: Vacuum magnetron sputtering target machine

5: Metal substrate

51: Carbon structure layer

Figure 1: Schematic diagram of the production process of the present invention

Figure 2: Schematic diagram of the vacuum infiltration furnace structure of the present invention

Figure 3: Schematic diagram of the use state of the present invention applied to the plane vacuum magnetron sputtering target machine

Figure 4: Schematic diagram of the use state of the present invention applied to the circular plane vacuum magnetron sputtering target machine

Figure 5: Schematic diagram of the use of the present invention applied to cylindrical magnetic vacuum magnetron sputtering target machine

Figure 6: Schematic diagram of the vacuum magnetron sputtering operation of the present invention in an enhanced unbalanced closed magnetic field

Figure 7: Schematic diagram of the vacuum magnetron sputtering operation of the present invention in a large multi-target unbalanced closed magnetic field

Figure 8: Another schematic diagram of the present invention for vacuum magnetron sputtering operation

Figure 9: Another schematic diagram of the present invention for vacuum magnetron sputtering operation

Figure 10: Schematic diagram of the forming state of the present invention

Figure 11: A schematic diagram of another forming state of the present invention

Figure 12: A schematic diagram of another forming state of the present invention

Claims (10)

A manufacturing method of orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on a metal substrate mainly includes the following steps: A. Graphite sputtering target: Graphite is made into various geometric shapes of magnetron sputtering target; B. Permeate: Dissolve the organic metal salt in an organic solvent to make it reach saturated solubility to produce a permeate; C. Infiltration: Put the sputtering target and the permeate into a vacuum infiltration furnace together, and allow the permeate to penetrate into the sputtering target under the vacuum environment in the vacuum infiltration furnace; D. Metal base material: the metal base material is formed with irregularities on both sides of the surface; E. Sputtering: Put the sputtering target after the penetration of the penetrating liquid into the vacuum magnetron sputtering machine, control the cooling water in the vacuum magnetron sputtering target machine, and then you can The metal substrate is subjected to vacuum magnetron sputtering operation, and the organic metal salt of the permeate remains non-magnetic before being decomposed at 150°C. After being sputtered, the metal of the nano-organic metal salt is decomposed to the high temperature zone. The particles are deposited on the metal substrate as a catalyst for carbon, so that the carbon from the sputtering target is rapidly bonded to each other to form an ordered carbon structure, which can be formed on the unevenness of the metal substrate Ordered two-dimensional or three-dimensional carbon structure layer. The orderly arrangement of graphene carbon nanotubes and carbon deposition composite coating manufacturing method for metal substrates according to claim 1, wherein the sputtering target has a graphite content of ≧99.95% and a porosity of 15%~ 30%. The method for manufacturing an orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on a metal substrate according to claim 1, wherein the vacuum infiltration furnace is provided with a furnace body, and the sputtering target material is provided in the furnace body , And make the permeate to submerge the sputtering target in the furnace body, a vacuum valve is provided in the furnace body to connect with the air pressure control device, and the high vacuum pump of the air pressure control device can vacuumize the inside of the furnace body , And the furnace body is provided with a vacuum gauge, and the pressure value inside the furnace body is observed through the vacuum gauge. According to claim 3, the orderly arrangement of graphene carbon nanotubes on a metal substrate and a carbon deposition composite coating manufacturing method, wherein the furnace body of the vacuum infiltration furnace is connected with a permeate recovery tank through which the permeate The recovery tank recovers the used permeate for repeated recycling. The method for manufacturing an orderly arrangement and carbon deposition composite coating of graphene carbon nanotubes on a metal substrate according to claim 1, wherein the metal substrate is a high-purity aluminum foil with an aluminum content of ≧99.7%, and a copper content of 99.7 % Of any kind of high-purity copper foil. According to claim 1 or 5, the orderly arrangement of graphene carbon nanotubes on a metal substrate and the carbon deposition composite coating manufacturing method, wherein the metal substrate is subjected to rough chemical plating, electrochemical corrosion, Either spraying or sputtering has uneven roughness formed on the surface. According to claim 1, the orderly arrangement and carbon deposition composite coating manufacturing method of graphene carbon nanotubes on a metal substrate, wherein the vacuum magnetron sputtering target machine is a plane vacuum magnetron sputtering target machine, a circular Either a flat plane vacuum magnetron sputtering target machine or a cylindrical magnetic vacuum magnetron sputtering target machine. According to claim 1, the orderly arrangement of graphene carbon nanotubes on metal substrates and the carbon deposition composite coating manufacturing method, wherein the target surface of the sputtering target is maintained at most 150°C or less, while the The working temperature in the cavity of the vacuum magnetron sputtering machine is at least 300℃ and the vacuum degree is below 0.1Pa. The method for manufacturing a composite coating of ordered arrangement and carbon deposition of graphene carbon nanotubes on a metal substrate according to claim 1, wherein the organometallic salt is any one of iron, cobalt, and nickel. The method for manufacturing a composite coating of ordered arrangement and carbon deposition of graphene carbon nanotubes on a metal substrate according to claim 1, wherein the carbon structure layer formed on the uneven portion of the metal substrate is carbon Any one or a combination of nanotubes and graphene.

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