CN111501010A - In-situ preparation method of metal fiber reinforced composite film - Google Patents

In-situ preparation method of metal fiber reinforced composite film Download PDF

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Publication number
CN111501010A
CN111501010A CN202010363528.0A CN202010363528A CN111501010A CN 111501010 A CN111501010 A CN 111501010A CN 202010363528 A CN202010363528 A CN 202010363528A CN 111501010 A CN111501010 A CN 111501010A
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composite film
substrate
reinforced composite
metal fiber
active screen
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吉小超
马天
康越
黄献聪
王刚
刘凯峰
龙知洲
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Institute of Quartermaster Engineering Technology Institute of Systems Engineering Academy of Military Sciences
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Institute of Quartermaster Engineering Technology Institute of Systems Engineering Academy of Military Sciences
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges

Abstract

The invention provides an in-situ preparation method of a metal fiber reinforced composite film. The plasma-assisted chemical vapor deposition method and the catalytic action of carbon plasma are utilized to generate metal fibers (silver, copper, aluminum, tin, platinum and the like) by reaction while sputtering the film, thereby realizing the in-situ preparation of the metal fiber reinforced composite film. The method realizes the sputtering synthesis of the one-dimensional metal fiber and the in-situ preparation of the fiber reinforced composite film, and the composite structure can adjust the stress state and the toughness of the film and endow the film with excellent performances of conductivity, friction reduction and the like.

Description

In-situ preparation method of metal fiber reinforced composite film
Technical Field
The invention belongs to the technical field of composite coating preparation, and particularly relates to an in-situ preparation method of a metal fiber reinforced composite film.
Background
The film material science is an important branch of material science, and a layer of film different from the material of a base body is deposited and attached on the surface of the base body, so that the base material is endowed with excellent wear resistance, corrosion resistance and surface mechanical properties, and even parts can obtain special properties of heat, electricity, light, sound, magnetism and the like. Composite films are an important direction of film research, which aims to improve the properties of a single film or to obtain properties that are not achieved by a single film by means of composite techniques. The composite film can be classified into a nanocrystal-embedded composite film, a nano multilayer composite film, a nano columnar crystal composite film, a mixed nanocrystal composite film, and the like according to the structure. By preparing various nano composite films, the hardness, thermal stability, corrosion resistance, oxidation resistance and low friction and wear performance of the film can be effectively improved.
The fiber reinforced composite structure is an important form of composite material, and has the advantages of toughening the matrix material by using dispersed fibers, improving the stress state of the whole material and prolonging the service life of the material. Accordingly, fiber-reinforced composite structures have found wide application in the field of composite materials. At present, with the rapid development of flexible electronic devices, a novel functional film has received much attention, however, reports on fiber-reinforced composite films are still few, mainly because the preparation process of the fiber-reinforced composite film is complex, and the difficulty lies in how to achieve uniform dispersion of fibers in a film system.
The preparation method of the fiber reinforced composite film can be divided into a premixing composite method and an in-situ composite method according to the mixing mode of the fiber and the base material. The premixing compounding method is to premix the fiber and the substrate material, and then to prepare the corresponding composite coating by means of sol-gel, electroplating and the like. The premixing method has the advantage that the preparation process is relatively simple, but because the mixing process is usually liquid phase mixing, the problem of agglomeration of fibers in the mixing process is difficult to avoid, and pores in the coating are often generated to cause cracking of the coating.
Compared with the premixing method, the in-situ composite method can well realize the uniform dispersion of the fibers in the base material, but the preparation process is more complicated and often does not leave the advanced surface engineering technology (physical vapor deposition or chemical vapor deposition). The fiber reinforced nano composite film is prepared in situ, and the preparation process can be divided into a two-step method and a one-step method. The two-step method means that the growth and preparation of the fiber are completed in the preparation process, and on the basis, the matrix material is further deposited and prepared to realize the final composition. The difficulty of the two-step method lies in controlling the structure of fiber growth, so that the matrix material can well penetrate into the gaps of the fibers to form the composite coating, and at present, researchers have realized the two-step preparation of the SiC nanotube and carbon nanotube reinforced composite film. The one-step method is to simultaneously realize the growth of the fiber and the preparation of the film substrate by utilizing an advanced preparation process, and has the difficulty of simultaneously controlling the preparation of the film and the growth of the fiber.
Disclosure of Invention
The invention aims to overcome the technical problem of preparing the metal fiber reinforced composite film in the prior art, and provides an in-situ preparation method of the metal fiber reinforced composite film and a device used by the method.
The invention provides a device for preparing a metal fiber reinforced composite film in situ, which comprises: a reaction cavity of plasma-assisted chemical vapor deposition (PECVD) equipment, an upper polar plate and a lower polar plate of the PECVD equipment which are arranged in the reaction cavity, a substrate (a metal fiber reinforced composite film to be sputtered is formed on the surface of the substrate) which is arranged on the lower polar plate, and an active screen which covers the substrate,
the substrate is spaced from the lower plate by a certain distance,
the upper surface and the lower surface of the active screen are respectively provided with target plates which are parallel to each other and are spaced at a certain distance, wherein the target plate on the lower surface is a hollow structure and is spaced from the surface of the substrate,
the material of the hollow target material plate on the lower surface can be stainless steel or iron-nickel alloy, and the material of the target material plate on the upper surface is the material of a metal fiber reinforcement to be sputtered, and specifically can be silver, copper, aluminum, platinum and the like;
the in-situ preparation method of the metal fiber reinforced composite film provided by the invention comprises the following steps: by adopting the device, the metal fiber is generated by the reaction of the plasma-assisted chemical vapor deposition method and the catalytic action of the carbon source plasma while the film is generated by sputtering, so that the in-situ preparation of the metal fiber reinforced composite film is realized.
The metal fiber can be micro-nano fiber of silver, copper, aluminum, platinum and other metals;
the composite film is a carbon-based composite film.
Specifically, the in-situ preparation method of the metal fiber reinforced composite film provided by the invention comprises the following steps:
1) placing a substrate on a lower polar plate of Plasma Enhanced Chemical Vapor Deposition (PECVD) equipment, separating the substrate from the lower polar plate by using an insulating cushion block, covering an active screen above the substrate, adjusting the distance between the surface of the substrate and the lower surface of the active screen,
the upper surface and the lower surface of the active screen are respectively target plates which are parallel to each other and are spaced at a certain distance, wherein the target plate on the lower surface is a hollow structure;
the material of the target material plate on the upper surface of the active screen is the material of a metal fiber reinforcement body to be sputtered;
2) pumping the reaction cavity to vacuum, introducing high-purity hydrogen into the reaction cavity, switching on a power supply after the pressure of the hydrogen reaches 0.5-4mbar, adjusting the voltage to ionize the hydrogen in the cavity to generate plasma, heating the whole cavity, introducing mixed gas of carbon source gas and a carrier when the temperature is close to 400 ℃, adjusting the voltage of the power supply to 200-300V, adjusting the pressure of the gas in the cavity to 0.8-2mbar, performing reactive deposition, and simultaneously depositing generated metal fibers to obtain a composite film, namely forming the metal fiber reinforced composite film on the surface of the substrate.
In the step 1) of the method, the substrate has a smooth surface and is made of silicon wafers, metals, ceramics, glass and the like;
the insulating cushion block can be made of ceramics or glass;
the substrate is separated from the lower polar plate by the insulating cushion block, so that the substrate is in a floating potential in the sputtering reaction preparation process, namely, the conductive substrate material is not directly connected with the electrode;
adjusting the distance between the surface of the substrate and the lower surface of the active screen through the insulating cushion block;
the distance of the substrate surface from the lower surface of the active screen may be: 5-40mm, specifically 15-25mm, more specifically 20 mm;
the distance between the upper surface and the lower surface of the active screen, namely, the distance between the upper target plate and the lower target plate, can be as follows: 5-20mm, specifically 5-10mm, more specifically 6 mm;
a certain distance is arranged between the upper surface target material plate and the lower surface target material plate of the active screen, and the purpose of the certain distance is to generate a hollow cathode effect between the two plates in the preparation process and promote the sputtering strength; the lower surface target material plate of the active screen is of a hollow structure, so that metal ions sputtered from the upper surface target material plate can be deposited on the surface of the substrate;
in the step 2), the power supply voltage is adjusted to 400V to ionize the hydrogen in the cavity to generate plasma,
the carbon source gas can be one or a mixture of any more of methane, acetylene, ethanol, acetone, n-hexane and n-butane; specifically, methane or acetylene;
the carrier can be hydrogen and/or argon;
the volume ratio of the carbon source gas to the carrier can be 2% -98% -8%: 92%, in particular 5%: 95% or 8%: 92 percent;
in the preparation process, the power supply voltage is adjusted to fluctuate within the range of 200-300V, so that a hollow cathode effect is generated between sputtering targets, metal sputtered from the upper surface target plate and nano particles sputtered from the lower surface hollow target plate generate metal nano wires in a preferred orientation mode in the catalytic environment of carbon source plasma, and meanwhile, the composite film is generated through deposition.
When the upper surface target material plate of the active screen is made of silver and the hollow target material plate of the lower surface of the active screen is made of stainless steel, the silver nanowire reinforced composite film is prepared, and the film substrate is composed of silver, stainless steel and amorphous carbon;
when the upper surface target plate of the active screen is made of copper and the hollow target plate of the lower surface is made of stainless steel, the copper nanowire reinforced composite film is prepared, and the film substrate is composed of copper, stainless steel and amorphous carbon.
Compared with the prior art for preparing the fiber reinforced composite film, the invention provides the in-situ preparation method of the metal fiber reinforced composite film, which successfully realizes the preparation of the metal micro-nano fiber by sputtering and synchronously realizes the preparation of the composite film on the basis. The method greatly improves the efficiency of preparing the fiber reinforced composite film and reduces the preparation difficulty. Meanwhile, the problem of randomness of fiber distribution in the fiber reinforced composite film is well solved, and the problem of fiber agglomeration in the traditional preparation process is avoided. The obtained fiber reinforced composite structure can effectively improve the stress state of a coating system, and has good application prospect in the fields of novel flexible electronic devices, wear resistance, biological antibiosis, electromagnetic shielding and the like.
The invention provides an in-situ preparation method of a metal fiber reinforced composite film. The method utilizes an active screen technology to realize the one-step method for preparing the metal fiber reinforced composite film on the surfaces of different substrates. Through process control, the method can realize the generation of metal fibers (Ag and Cu) in the sputtering process and simultaneously realize the preparation of the composite film. Provides a new idea and a new method for preparing the fiber reinforced composite film.
Drawings
FIG. 1 is a schematic cross-sectional view of an apparatus for manufacturing a metal fiber-reinforced composite film according to the present invention and a sample placement;
FIG. 2(a) is a surface SEM topography of a silver wire reinforced composite film prepared in example 1 of the present invention; FIG. 2(b) is a graph showing the result of energy spectrum analysis data of 316 stainless steel coated with a silver wire reinforced composite film prepared in example 1; FIG. 2(c) is a comparison of the results of the antifriction test of example 1 in which the 316 stainless steel was coated with a silver wire reinforced composite film and the results of the antifriction test of the uncoated 316 stainless steel.
FIG. 3(a) is a SEM image of the surface of the copper wire reinforced composite film prepared in example 2 of the present invention; FIG. 3(b) is a graph of the energy spectrum analysis data of the copper wire reinforced composite film on the surface of the silicon wafer.
Detailed Description
The present invention will be described below with reference to specific examples, but the present invention is not limited thereto.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
The apparatus used in the following examples is schematically shown in FIG. 1.
Example 1 preparation of silver wire reinforced composite film
The embodiment provides a preparation method of an in-situ grown silver wire reinforced carbon-based composite film, which mainly comprises the following steps:
providing a cylindrical 316 stainless steel material substrate (25mm × 3mm), polishing the upper surface, ultrasonically cleaning by using alcohol, then placing on a lower plate sample table in a reaction cavity, separating the substrate from the lower plate sample table by using a non-conductive alumina ceramic cushion block (so that a sample is positioned at a floating potential), placing a stainless steel active screen cover above the sample, wherein the active screen cover consists of two parallel target materials, the lower hollow target material is 316 stainless steel, the upper target material is a 99.99% silver plate, the distance between the substrate and the lower target material is 20mm, and the distance between the two target materials is 6 mm.
After the setting is finished, the reaction cavity is closed, the vacuumizing is carried out to 0.07mbar, then high-purity hydrogen is introduced into the cavity, when the air pressure in the cavity reaches 1mbar, the sample table is powered on, the power supply voltage is adjusted to 400V, and the hydrogen in the cavity is ionized to generate plasma to heat the whole cavity. Measuring the temperature of a 316 stainless steel test block close to the position of the sample by using a thermocouple, adjusting the precursor introduced into the cavity when the temperature is close to 400 ℃, and introducing mixed gas of high-purity methane and high-purity hydrogen, wherein the volume mixing ratio is 5%: 95 percent. When the air pressure is stable (1mbar), the power voltage is adjusted to 240V, and the deposition preparation of the silver fiber reinforced composite film is started. In the preparation process, strong plasmas generated by the hollow cathode effect among sputtering target materials are utilized to sputter silver and stainless steel nano particles from the surfaces of the target materials, wherein the silver nano particles grow according to a certain preferred orientation under the catalysis of carbon plasmas to further form silver wires, and the film base material is formed by compounding stainless steel, silver and carbon.
FIG. 2(a) is a SEM topography of the surface of the prepared silver wire reinforced composite film; as can be seen from fig. 2(a), some silver wires are embedded in the composite coating, and part of the silver wires are exposed on the surface of the coating; the diameter of the silver wire is 0.5-3 μm; the friction test results show that (fig. 2(c)), the friction coefficient of 316 stainless steel coated with the silver wire reinforced composite film is lower and more stable, about 0.27; and the friction coefficient obtained by the surface friction test with the stainless steel material under the same condition fluctuates sharply within the range of 0.4-0.5. The counter-friction piece of the friction test is an aluminum ball, and the friction load is 5 kg.
Fig. 2(b) is a graph showing the result of the energy spectrum analysis data of the 316 stainless steel coated with the silver wire reinforced composite film prepared.
Example 2 preparation of in-situ grown copper wire-reinforced carbon-based composite film
The embodiment provides a preparation process of an in-situ grown copper wire reinforced carbon-based composite film, which mainly comprises the following steps:
providing a silicon wafer substrate, ultrasonically cleaning the surface of the silicon wafer substrate by using alcohol, then placing the silicon wafer substrate on a lower polar plate in a plasma reaction cavity, and adjusting the height of the substrate by using an alumina ceramic cushion block. The arrangement of the stainless steel active screen cover is similar to that in example 1, the lower hollow target is 316 stainless steel, and the upper target is 99.99% copper plate. The distance between the sample and the lower target material is 20mm, and the distance between the two target materials is 6 mm.
After the sample is placed, vacuumizing the reaction cavity to 0.07mbar, introducing high-purity hydrogen into the cavity, adjusting the air pressure in the cavity to 1mbar, switching on the power supply, adjusting the power supply voltage to 400V, ionizing the hydrogen introduced into the cavity, and heating the cavity by using the generated plasma. A thermocouple was placed at an equivalent location near the sample and the real-time temperature during the preparation was measured. When the temperature reaches 400 ℃, adjusting the gas components introduced into the cavity, and introducing mixed gas of high-purity acetylene and high-purity hydrogen, wherein the volume mixing ratio is 8%: 92 percent. In the preparation process, the power supply voltage is adjusted to fluctuate within the range of 200-300V, so that a hollow cathode effect is generated between sputtering target materials, sputtered copper and stainless steel nano particles generate copper nano wires in a preferred orientation mode under the catalytic environment of carbon source plasma, and a composite film is generated by deposition, wherein the film base material is composed of copper, stainless steel and amorphous carbon.
FIG. 3(a) is a SEM topography of the surface of the prepared copper wire reinforced composite film; from fig. 3(a), it can be seen that the copper fiber reinforced composite film is formed by the reaction, and part of the copper fiber is exposed on the surface of the coating; the diameter of the copper wire is 150-350 nm; FIG. 3(b) is a graph of the energy spectrum analysis data of the copper wire reinforced composite film on the surface of the silicon wafer.

Claims (9)

1. An apparatus for in-situ preparation of a metal fiber reinforced composite film, comprising: a reaction cavity of plasma-assisted chemical vapor deposition equipment, an upper polar plate and a lower polar plate of PECVD equipment arranged in the reaction cavity, a substrate arranged on the lower polar plate and an active screen covered above the substrate,
the substrate is spaced from the lower plate by a certain distance,
the upper surface and the lower surface of the active screen are respectively target plates which are parallel to each other and are spaced by a certain distance, wherein the target plates on the lower surface are of hollow structures, and are spaced from the surface of the substrate.
2. The apparatus of claim 1, wherein: the material of the hollow target plate on the lower surface is stainless steel or iron-nickel alloy, and the material of the target plate on the upper surface is the material of a metal fiber reinforcement body to be sputtered.
3. An in-situ preparation method of a metal fiber reinforced composite film is disclosed, wherein the metal fiber is micro-nano fiber of silver, copper, aluminum or platinum; the composite film is a carbon-based composite film;
the in-situ preparation method comprises the following steps: the device of claim 1 or 2 is adopted, and the metal fiber is generated by the reaction of the plasma-assisted chemical vapor deposition method and the carbon plasma in the process of generating the film by sputtering, so that the in-situ preparation of the metal fiber reinforced composite film is realized.
4. The method of claim 3, wherein: the in-situ preparation method of the metal fiber reinforced composite film comprises the following steps:
1) placing the substrate on a lower polar plate of a plasma-assisted chemical vapor deposition device, separating the substrate from the lower polar plate by using an insulating cushion block, covering an active screen above the substrate, adjusting the distance between the surface of the substrate and the lower surface of the active screen,
the upper surface and the lower surface of the active screen are respectively target plates which are parallel to each other and are spaced at a certain distance, wherein the target plate on the lower surface is a hollow structure;
the material of the target material plate on the upper surface of the active screen is the material of a metal fiber reinforcement body to be sputtered;
2) pumping the reaction cavity to vacuum, introducing high-purity hydrogen into the reaction cavity, switching on a power supply after the pressure of the reaction cavity reaches 0.5-4mbar, adjusting the voltage to ionize the hydrogen in the cavity to generate plasma, heating the whole cavity, introducing mixed gas of carbon source gas and a carrier when the temperature is close to 400 ℃, adjusting the voltage of the power supply to 200-300V, reacting to generate metal fibers, and simultaneously depositing to obtain a composite film, namely forming the metal fiber reinforced composite film on the surface of the substrate.
5. The method of claim 4, wherein: in the step 1), the substrate has a smooth surface and is made of silicon wafers, metal, ceramic or glass;
the distance from the surface of the substrate to the lower surface of the active screen is as follows: 5-40 mm;
the distance between the upper surface and the lower surface of the active screen, namely, the distance between the upper target plate and the lower target plate, is as follows: 5-20 mm.
6. The method of claim 5, wherein: the distance between the surface of the substrate and the lower surface of the active screen is 20 mm;
the distance between the upper and lower surfaces of the active screen, i.e., the distance between the upper and lower target plates, was 6 mm.
7. The method according to any one of claims 4-6, wherein: in the step 2), the power supply voltage is adjusted to 400V to ensure that the hydrogen in the cavity is ionized to generate plasma,
the carbon source gas is one or a mixture of any more of methane, acetylene, ethanol, acetone, n-hexane and n-butane;
the carrier is hydrogen and/or argon;
the volume ratio of the carbon source gas to the carrier is 2%: 98% -8%: 92 percent.
8. The method according to any one of claims 3-7, wherein: the upper surface target material plate of the active screen is made of silver, the lower surface hollow target material plate of the active screen is made of stainless steel, the silver nanowire reinforced composite film is prepared, and the film substrate is composed of silver, stainless steel and amorphous carbon;
the upper surface target material plate of the active screen is made of copper, when the hollow target material plate of the lower surface is made of stainless steel, the copper nanowire reinforced composite film is prepared, and the film base material is composed of copper, stainless steel and amorphous carbon.
9. The metal fiber reinforced composite film prepared by the method of any one of claims 3 to 8, wherein the metal fiber is micro-nanofiber of silver, copper, aluminum or platinum; the composite film is a carbon-based composite film.
CN202010363528.0A 2020-04-30 2020-04-30 In-situ preparation method of metal fiber reinforced composite film Pending CN111501010A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112647051A (en) * 2020-12-14 2021-04-13 军事科学院***工程研究院军需工程技术研究所 Ag-containing metal composite film and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101469407A (en) * 2007-12-28 2009-07-01 北京有色金属研究总院 Sputtering equipment with close packing tip anode
CN104583446A (en) * 2012-07-05 2015-04-29 伯明翰大学 Long-lasting antibacterial metallic surfaces and methods for their production
CN110468376A (en) * 2019-08-27 2019-11-19 吉林大学 A kind of carbon-coated Silver nanorod array and its preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101469407A (en) * 2007-12-28 2009-07-01 北京有色金属研究总院 Sputtering equipment with close packing tip anode
CN104583446A (en) * 2012-07-05 2015-04-29 伯明翰大学 Long-lasting antibacterial metallic surfaces and methods for their production
CN110468376A (en) * 2019-08-27 2019-11-19 吉林大学 A kind of carbon-coated Silver nanorod array and its preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIAOCHAO JI, ET AL.: ""In situ synthesis of the one-dimensional Ag wires reinforced composites film by a novel active screen plasma process: Nanostructure and excellent adhesion resistance"", 《MATERIALS LETTERS》 *
XIAOCHAO JI, ET AL.: ""Synthesis and in-vitro antibacterial properties of a functionally graded Ag impregnated composite surface"", 《MATERIALS SCIENCE AND ENGINEERING: C》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112647051A (en) * 2020-12-14 2021-04-13 军事科学院***工程研究院军需工程技术研究所 Ag-containing metal composite film and preparation method thereof

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Application publication date: 20200807