CN111172511A - Method for preparing metal film layer on surface of organic material - Google Patents
Method for preparing metal film layer on surface of organic material Download PDFInfo
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- CN111172511A CN111172511A CN202010054944.2A CN202010054944A CN111172511A CN 111172511 A CN111172511 A CN 111172511A CN 202010054944 A CN202010054944 A CN 202010054944A CN 111172511 A CN111172511 A CN 111172511A
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical 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 metallic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/406—Oxides of iron group metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/408—Oxides of copper or solid solutions thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical 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
- C23C16/455—Chemical 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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
Abstract
The invention relates to the technical field of artware manufacturing, in particular to a method for preparing a metal film layer on the surface of an organic material. According to the invention, the first metal film layer is plated on the organic material in an atomic layer deposition mode, so that a film layer with uniform thickness can be formed on each part of the surface of a complex shape, and the thickness of the formed film layer can be accurately controlled. The method adopts the atomic layer deposition mode to plate the first metal film layer on the organic material, can form film layers with uniform thickness on all parts of the surface with a complex shape, and can accurately control the thickness of the formed film layers. The method for preparing the metal film layer on the surface of the organic material provided by the invention obviously improves the quality of the handicraft plated with metal on the surface of the organic material.
Description
Technical Field
The invention relates to the technical field of handicraft manufacturing, in particular to a method for preparing a metal film layer on the surface of an organic material.
Background
The preparation of metal film on the surface of organic material (such as fresh flower, small plant, small animal, insect, etc.) is an important technology for making handicraft. Meanwhile, in order to obtain the micro structure on the surface of the body of small animals such as insects, metal film layers with special micro structures can be manufactured on the surfaces of the small animals, and the metal film layers are used for further scientific research. In the fabrication of these metal film layers, the most critical is the first step: how to prepare the surface of the non-conductive organic material into a conductive surface. For this purpose, a metal film layer is usually prepared, and then various other metal film layers are prepared. The preparation of the first metal film layer is crucial and directly determines the quality of the subsequent metal film layer.
The existing method for preparing the first metal film layer is a conductive spraying method, and the yield of the finally obtained product is about 60-70%.
Disclosure of Invention
The method for preparing the first metal film layer on the surface of the organic material may be a) a conductive spraying method; b) chemical vapor deposition; c) physical vapor deposition. The greatest disadvantage of these methods is that they do not allow the surface of a sample of complex shape to be uniformly coated with a metal film, and the desired metal film is not usually obtained in the direction away from the gas source or the heat source or plasma source. The metal films produced by these methods often have voids, non-uniform film thickness, and stress in the film.
In order to form various metal film layers on the surface of a non-conductive organic material, the surface must be made conductive. The nature of the first metal film layer formed by rendering the surface of the non-conductive organic material conductive directly determines the nature and quality of the subsequent preparation of other metal films. The aforementioned conductive spraying method, chemical vapor deposition method and physical vapor deposition method inevitably cause non-uniformity problem, so that any subsequent method for forming other metal film layer inevitably causes non-uniformity problem of the film layer, which is especially prominent in the sample with complex shape.
The invention adopts a preparation method of a metal film layer, namely an Atomic Layer Deposition (ALD) method to prepare a first metal film layer on the surface of an organic material, so as to overcome the defects of the existing method.
The invention provides a method for preparing a metal film layer on the surface of an organic material.
In some possible embodiments, the pre-treatment comprises trimming the organic material, followed by washing and drying.
In some possible embodiments, the cleaning uses deionized water to clean the surface of the organic material until the surface is free of foreign matter.
In some possible embodiments, the drying is oven dried to constant weight.
In some possible embodiments, the atomic layer deposition step is as follows:
(a) cleaning with inert gas, introducing a first gas phase precursor, and waiting for 1-5 seconds;
(b) cleaning with inert gas, introducing a second gas-phase precursor, and waiting for 1-5 seconds;
(c) cleaning with inert gas;
the temperature in the atomic layer deposition process is 60-300 ℃.
In some possible embodiments, in step (a), the inert gas purge is for 0.1 to 5.0 seconds;
and/or
In the step (b), inert gas is used for cleaning for 0.1-5.0 seconds;
and/or
In the step (c), inert gas purging is performed for 0.1 to 5.0 seconds.
In some possible embodiments, in step (a), the first gas phase precursor is introduced for 0.01 to 5.0 seconds;
and/or
And (b) introducing a second gas-phase precursor for 0.01-5.0 seconds.
In some possible embodiments, the inert gas comprises any one of nitrogen, helium, and argon.
In some possible embodiments, the organic material comprises a plant sample, an animal sample.
In some possible embodiments, the first metal film layer includes any one of a copper layer, a nickel layer, a gold layer, a zinc layer, an aluminum layer, or an oxide film layer thereof.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method adopts the atomic layer deposition mode to plate the first metal film layer on the organic material, can form film layers with uniform thickness on all parts of the surface with a complex shape, and can accurately control the thickness of the formed film layers.
(2) The invention accurately controls the formation and growth of the surface film on the atomic level, and prepares the nano film with ultra-uniform thickness, high precision and high shape retention.
(3) The method for preparing the metal film layer on the surface of the organic material provided by the invention obviously improves the quality of the handicraft plated with metal on the surface of the organic material, thereby achieving the purposes of increasing sales and reducing cost.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be described in further detail with reference to specific embodiments. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and therefore the scope of the present invention is not limited to the specific embodiments disclosed below.
The main methods for preparing the first metal film layer on the surface of the organic material can be a) a conductive spraying method, b) a chemical vapor deposition method and c) a physical vapor deposition method.
CVD (chemical vapor deposition) is a process in which two different gases are introduced into a reaction chamber at the same time, and a new material is formed by chemical reaction between the two gases, usually through the inner wall of a high temperature reaction chamber or plasma, and deposited on the surface of a sample.
PVD (physical vapor deposition) is a technique for depositing a thin film having a specific function on the surface of a substrate by vaporizing a material source, a solid or liquid surface, into gas atoms and molecules by a physical method such as heating or ion sputtering under vacuum conditions and by a low pressure gas process.
The high temperature heating, plasma technique or ion sputtering technique used in the above two methods may cause problems of non-uniformity, pinholes and stress of the formed thin film.
The embodiment of the invention provides a method for preparing a metal film layer on the surface of an organic material.
ALD (atomic layer deposition) is a method of plating a substrate surface with gaseous species in a monoatomic film. In an atomic layer deposition process, the chemical reaction of a new layer of atomic film is directly related to the previous layer, with only one layer of atoms being deposited per reaction. Since a gas phase material is used, the gas can reach any surface of a complex structure, and simultaneously the use of high temperature, plasma technology or ion sputtering technology is avoided, so that the formed film can be very uniform.
The three coating methods are shown in Table 1.
TABLE 1 comparison of ALD, CVD and PVD
The invention adopts a preparation method of a metal film layer, namely an Atomic Layer Deposition (ALD) method to prepare a first metal film layer on the surface of an organic material, so as to overcome the defects of the existing method, thereby achieving the purpose of improving the quality and the process of manufacturing artware with metal plated on the surface of the organic material, and providing a good basis for scientifically researching and obtaining the complete microstructure of the body surfaces of organic materials such as animal samples (insects and the like) and plant samples.
In some possible embodiments, the organic material in the present invention includes a plant sample and an animal sample.
Plant samples mainly refer to small plants such as flowers, and of course, some parts of large plants can also be used as organic materials in the invention; the animal sample mainly refers to small animals, such as insects, and some parts of large animals can be used as the organic material in the invention; the limitation on the size of a plant or animal sample is mainly due to the sample space limitations of the atomic layer deposition instrument.
In some possible embodiments, the pre-treatment comprises trimming the organic material, followed by washing and drying.
The trimming is generally performed with scissors, but may be performed in other ways, and the trimming is performed to make the sample have a good overall shape and maintain the original appearance of the sample as much as possible.
In some possible embodiments, the cleaning uses deionized water to clean the surface of the organic material until the surface is free of foreign matter.
And repeatedly cleaning the surface of the trimmed sample by using deionized water for many times until no foreign matters exist on the surface.
In some possible embodiments, the drying is oven dried to constant weight.
The original shape of the sample is kept as much as possible in the drying process, for example, the sample can be placed in an oven at 110 ℃ to be dried to constant weight. Of course, the temperature of the oven may be higher or lower as long as the original shape of the sample is not greatly affected and the drying effect is achieved. Of course, the drying method in the present invention is not limited to this, and other drying methods may be employed.
In some possible embodiments, the atomic layer deposition step is as follows:
(a) cleaning with inert gas, introducing a first gas phase precursor, and waiting for 1-5 seconds;
(b) cleaning with inert gas, introducing a second gas-phase precursor, and waiting for 1-5 seconds;
(c) cleaning with inert gas;
the temperature in the atomic layer deposition process is 60-300 ℃.
The atomic layer deposition method adopted by the invention can avoid the defects brought by the traditional method because only the first precursor and the second precursor in gas phase are used and the proper temperature treatment is adopted, because the gas-phase precursor can contact any surface with a complex structure. The low temperature atomic layer deposition method can further enable the organic material which forms deformation at high temperature to keep the original shape. The atomic layer deposition method has highly controllable parameters and can be realized on complex three-dimensional structure substrates with various sizes. The formation and growth of the surface layer film are accurately controlled at the atomic level, and the nano-grade film with ultra-uniform thickness, high precision and high shape retention is prepared, so that the quality of the handicraft article plated with metal on the surface of the organic material is obviously improved.
In some possible embodiments, in step (a), the inert gas purge is for 0.1 to 5.0 seconds;
and/or
In the step (b), inert gas is used for cleaning for 0.1-5.0 seconds;
and/or
In the step (c), inert gas purging is performed for 0.1 to 5.0 seconds.
The purpose of the inert gas purge is to remove unreacted vapor phase precursors or vapor phase precursors to which deposition is not robust or byproducts of the reaction. Therefore, the cleaning time of the inert gas can be selected according to actual requirements.
In the present invention, tests have found that the above-mentioned good effects can be achieved by purging with inert gas for a suitable period of time. Therefore, the time for purging with the inert gas in the steps (a), (b) and (c) may be 0.1 to 5.0 seconds, or 0.1 to 5.0 seconds may be selected for one or both of the steps, and other purging times may be selected for the other steps.
In various embodiments of the present invention, the time value between 0.1 and 5.0 seconds can be selected to be any time value between 0.1 and 5.0 seconds, such as 0.1 seconds, 0.2 seconds, 0.5 seconds, 1.0 second, 1.5 seconds, 2.0 seconds, 3.0 seconds, 4.0 seconds, 5.0 seconds, and the like.
In some possible embodiments, in step (a), the first gas phase precursor is introduced for 0.01 to 5.0 seconds;
and/or
And (b) introducing a second gas-phase precursor for 0.01-5.0 seconds.
In the invention, tests show that the good effect can be achieved by introducing the first gas phase precursor for a proper time. Therefore, the time for introducing the first gas phase precursor and the time for introducing the second gas phase precursor in the steps (a) and (b) can be both 0.01 to 5.0 seconds, or 0.01 to 5.0 seconds can be selected in any step, and other phase precursor introduction times can be selected in other steps.
In various embodiments of the present invention, the time value between 0.01 and 5.0 seconds can be selected to be any time value between 0.01 and 5.0 seconds, such as 0.01 seconds, 0.02 seconds, 0.05 seconds, 0.1 seconds, 0.2 seconds, 0.5 seconds, 1.0 seconds, 1.5 seconds, 2.0 seconds, 3.0 seconds, 4.0 seconds, 5.0 seconds, and the like.
In some possible embodiments, the inert gas comprises any one of nitrogen, helium, and argon.
In the invention, the nitrogen, helium and argon in the inert gas can be pure nitrogen, helium and argon; the high-purity nitrogen, helium and argon can be used, wherein the high purity is more than 99.9999 percent; etc. as long as the object of the present invention is satisfied.
In some possible embodiments, the first metal film layer includes any one of a copper layer, a nickel layer, a gold layer, a zinc layer, an aluminum layer, or an oxide film layer thereof.
The oxide film layer refers to the oxide film layer of any one of the foregoing metals. For example, the first metal film layer may be any one of a copper oxide layer, a nickel oxide layer, a gold oxide layer, a zinc oxide layer, and an aluminum oxide layer.
Different gas phase precursors are needed for preparing different metal films, and the needed metal film layer is generated by matching with different temperatures. A single atomic layer deposition process results in a single atomic layer thickness.
Such as Al2O3The temperature of the atomic layer deposition reaction chamber in the atomic layer deposition process can be set to be 150 ℃; atomic layer deposition of PtThe temperature of the atomic layer deposition reaction chamber in the process of deposition can be set to 300 ℃; the temperature of the atomic layer deposition reaction chamber in the copper atomic layer deposition process can be set to be 60 ℃; and so on.
In addition, the thickness of the metal film layer prepared by the method can be selected according to the requirement, and the atomic layer deposition process can be repeatedly cycled.
The following examples are given.
Example 1
The flowers were trimmed with scissors to maintain their original appearance as much as possible.
And repeatedly cleaning the surface of the treated fresh flower by using deionized water for many times until no foreign matters exist on the surface.
The cleaned fresh flowers are dried in an oven at 110 ℃ to constant weight, and the original shape of the sample is maintained as much as possible.
Preparation of Atomic Layer Deposition (ALD): the atomic layer deposition technology is a method for forming a film by alternately and impulsively introducing gas-phase precursors into a reaction chamber and carrying out gas-solid phase chemical adsorption reaction on the surface of a deposition substrate. Al (Al)2O3The main technical parameters of atomic layer deposition are set as follows:
cleaning with high-purity inert gas: nitrogen for 1 second.
Gas-phase precursor A: moisture, time 0.05 seconds.
Waiting time: 1.5 seconds.
Re-cleaning with high-purity inert gas: nitrogen for 1 second.
Gas-phase precursor B: TMA, time 0.05 second.
Waiting time: 1.5 seconds.
Re-cleaning with high-purity inert gas: nitrogen for 1 second.
Temperature of atomic layer deposition reaction chamber: at 150 ℃.
The main technical parameters in the Pt atomic layer deposition method are as follows:
cleaning with high-purity inert gas: nitrogen for 3 seconds.
Gas-phase precursor A: o is2The time was 2 seconds.
Waiting time: for 3 seconds.
Re-cleaning with high-purity inert gas: nitrogen for 4 seconds.
Gas phase precursor B MeCpPtMe3And the time was 0.08 seconds.
Waiting time: for 4 seconds.
Re-cleaning with high-purity inert gas: nitrogen for 3 seconds.
Temperature of atomic layer deposition reaction chamber: at 300 ℃.
Example 2
Different from the embodiment 1, the main technical parameters of the Pt atomic layer deposition are set as follows:
cleaning with high-purity inert gas: nitrogen for 3 seconds.
Gas-phase precursor A: o is2The time was 2 seconds.
Waiting time: for 3 seconds.
Re-cleaning with high-purity inert gas: nitrogen for 4 seconds.
Gas-phase precursor B: MeCpPtMe3And the time was 0.08 seconds.
Waiting time: for 4 seconds.
Re-cleaning with high-purity inert gas: nitrogen for 3 seconds.
Temperature of atomic layer deposition reaction chamber: at 300 ℃.
The thickness and uniformity of the film layers prepared by atomic layer deposition of examples 1 and 2 were measured by TEM. The TEM measurement method is to cut a sample with a Dual beam focused ion beam (Dual beam FIB), thin the sample to less than 100nm, and observe the sample at high magnification (10000 to 1000000 times) using a Transmission Electron Microscope (TEM) to measure the thickness and uniformity of the deposited film.
The film thicknesses of the film layers obtained in example 1 and example 2 were 80nm (100 cycles) and 60nm (100 cycles), respectively, and a highly precise and conformal nano-scale thin film with an ultra-uniform thickness was formed (multi-point sampling measurement, error was not more than + -3%). And the detection shows that the film layer has no pinhole and no stress.
The yield of the handicraft with metal plated on the surface of the organic material is more than 90%, and the quality is obviously improved.
Of course, the flowers in the present example can be replaced with other plants or other animal samples, and the effects consistent with those of examples 1 and 2 above can be obtained.
The invention adopts a novel preparation method of a metal film layer, namely Atomic Layer Deposition (ALD), to prepare a first metal film layer on the surface of an organic material, so as to overcome the defects of the existing method. Thereby achieving the purpose of improving the quality and the process of manufacturing the handicraft with metal plated on the surface of the organic material and providing a good technical basis for researching the complete microstructure of the body surface of the organic material such as small animal insects and the like in science.
In the description of the present specification, the description of the terms "some embodiments," "specific embodiments," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiments or examples is included in at least one embodiment or example of the invention. In this specification, an express statement of the above term does not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The method for preparing the metal film layer on the surface of the organic material is characterized in that the pretreated organic material is subjected to atomic layer deposition to prepare the first metal film layer on the surface of the organic material.
2. The method for preparing the metal film layer on the surface of the organic material as claimed in claim 1, wherein the pretreatment comprises trimming the organic material, and then washing and drying.
3. The method of claim 2, wherein the cleaning step is performed with deionized water until the surface of the organic material is free of foreign matters.
4. The method for preparing the metal film layer on the surface of the organic material according to claim 2, wherein the drying is carried out by using an oven to reach a constant weight.
5. The method for preparing the metal film layer on the surface of the organic material according to claim 1, wherein the atomic layer deposition comprises the following steps:
(a) cleaning with inert gas, introducing a first gas phase precursor, and waiting for 1-5 seconds;
(b) cleaning with inert gas, introducing a second gas-phase precursor, and waiting for 1-5 seconds;
(c) cleaning with inert gas;
the temperature in the atomic layer deposition process is 60-300 ℃.
6. The method for preparing a metal film layer on the surface of an organic material according to claim 5, wherein in the step (a), the inert gas is purged for 0.1 to 5.0 seconds;
and/or
In the step (b), inert gas is used for cleaning for 0.1-5.0 seconds;
and/or
In the step (c), inert gas purging is performed for 0.1 to 5.0 seconds.
7. The method for preparing a metal film on the surface of an organic material according to claim 5, wherein in the step (a), the first gas phase precursor is introduced for 0.01 to 5.0 seconds;
and/or
And (b) introducing a second gas-phase precursor for 0.01-5.0 seconds.
8. The method for preparing the metal film layer on the surface of the organic material as claimed in claim 5, wherein the inert gas comprises any one of nitrogen, helium and argon.
9. The method for preparing the metal film layer on the surface of the organic material as claimed in any one of claims 1 to 8, wherein the organic material comprises a plant sample and an animal sample.
10. The method for preparing the metal film layer on the surface of the organic material as claimed in any one of claims 1 to 8, wherein the first metal film layer comprises any one of a copper layer, a nickel layer, a gold layer, a zinc layer, an aluminum layer or an oxide film thereof.
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