CN113718200A - Method for preparing gradient-structure amorphous film based on high-temperature ion irradiation - Google Patents
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/00—Amorphous alloys
- C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5826—Treatment with charged particles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/02—Amorphous
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a method for preparing a gradient-structure amorphous film based on high-temperature ion irradiation, which is characterized in that high-temperature ion irradiation treatment is assisted on the basis of a high-quality amorphous film prepared by magnetron sputtering plating, so that the surface of a sample is crystallized and the inside of the sample keeps an amorphous structure, and thus, the high-strength and high-plasticity amorphous film with a gradient structure is prepared. The gradient amorphous film structure prepared by the invention is easy to realize by controlling the temperature and the injection dose of an ion irradiation experiment, thereby providing possibility for preparing a controllable amorphous film material with high mechanical property.
Description
Technical Field
The invention belongs to the technical field of nano metal film materials, and particularly relates to a method for preparing a high-strength and high-plasticity gradient structure amorphous film based on high-temperature ion irradiation.
Background
The amorphous alloy is different from a crystal material, has the characteristics of long-range disorder and short-range ordered atomic arrangement, and the strength and plastic deformation mode of the amorphous alloy are obviously different from those of the crystal material due to the characteristics. On one hand, the strength of the amorphous alloy is significantly higher than that of the crystalline material, so that the amorphous alloy becomes one of hot spots for engineering material development. On the other hand, due to the lack of plastic deformation carriers such as dislocations in the crystal, the plastic deformation of amorphous alloys is usually concentrated in highly localized shear bands, which limits the application of amorphous alloys in practical engineering to a large extent.
In order to improve the plastic deformation capacity of the amorphous alloy, a large amount of researches take the crystalline material as an additive phase to form a composite material with the amorphous alloy in a casting mode so as to integrate the strength of the amorphous alloy and the plastic deformation capacity of the crystalline material. Although this approach can greatly improve the plastic deformability of the amorphous alloy, the following two inevitable drawbacks still exist: firstly, the components, the grain size and the volume fraction of a crystal phase formed in the amorphous alloy are difficult to control; secondly, the prepared amorphous/crystalline composite material has better plastic deformation capability than that of single-phase amorphous alloy, but the strength of the amorphous/crystalline composite material tends to show a descending trend, namely the advantage of high strength of the amorphous alloy is weakened.
The other way to improve the plastic deformation capability of the amorphous alloy is to introduce a large amount of excess free volume into the amorphous alloy through room temperature ion irradiation treatment, so as to increase the volume of a plastic deformation carrier (shear transition zone) of the amorphous alloy, and further improve the capability of the amorphous alloy to resist localized deformation. This method has the same problems as the above method: the strength of the amorphous alloy is reduced while the plastic deformation capacity of the amorphous alloy is improved.
Disclosure of Invention
The invention aims to enable an amorphous alloy film to present a gradient material form with a surface crystallization and an internal amorphous structure through high-temperature (873 +/-10K) ion irradiation treatment, and simultaneously modify the internal amorphous alloy so as to achieve the purpose of simultaneously improving the strength and the plastic deformation capacity of the amorphous alloy. The method has the advantages that the thickness of the crystal layer is controllable, the strength of the amorphous alloy is further improved while the plastic deformation capacity of the amorphous alloy is improved, and therefore the possibility is provided for preparing the amorphous alloy thin film material with high strength and high plasticity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a gradient-structure amorphous film based on high-temperature ion irradiation. Firstly, a layer with the atomic percentage of W is deposited on a monocrystalline silicon (100) substrate by adopting a magnetron sputtering method65Ni35(at.%) of an amorphous film having a film thickness of 1 μm, and subjecting the amorphous film to He at 873 ± 10K+And (5) ion irradiation treatment.
The method specifically comprises the following steps:
1) ultrasonically cleaning a single-side polished monocrystalline silicon substrate to remove an oxide film on the surface, and then putting the single-side polished monocrystalline silicon substrate on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare film coating;
2) respectively arranging a pure W (99.99 at.%) target material and a pure Ni (99.99 at.%) target material to be sputtered on a target seat;
3) when the silicon chip is sputtered and deposited, a direct current power supply and a radio frequency power supply are respectively connected with corresponding target materials, the set atomic percentage is reached through the regulation and control of the power supply power in the sputtering process, the plating time is set through the deposition rate, and finally the required total thickness is reached.
4) He is carried out on the prepared amorphous film under 873 +/-10K+And (5) ion irradiation treatment.
Further, in step 1), the single-side polished single crystal silicon (100) substrate is cleaned by ultrasonic cleaning with acetone, alcohol and distilled water for 20min, and then the residual distilled water on the substrate is dried by a blower.
Further, in the step 3), the power of the power supply and the corresponding deposition rate are respectively 120 +/-6W of the direct-current power supply, and the deposition rate is 6.5-7.1 nm/min; the radio frequency power supply is 80 +/-4W, the deposition rate is 6.5-7.1nm/min, and the total thickness of the deposited film is 1 micron.
Further, in the step 3), the substrate table rotates at a constant speed at normal temperature, and the rotation speed is 175-185 °/min.
Further, in the step 4), He ions used are monovalent ions; the irradiation temperature is 873 +/-10K; upon irradiation with ionThe energy of the sub-beam is 120 +/-5 KeV; the ion implantation rate during irradiation was 4.0X 1013-4.4×1013ions/cm2s; the total ion irradiation dose was 7.7X 1016-7.9×1016ions/cm2(ii) a The pressure during injection is maintained at 1.0 × 10-4-9.1×10-5Pa。
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts magnetron sputtering technology, and prepares the W with atomic percentage by adjusting the sputtering power of the W target and the Ni target65Ni35(at.%) and passing He at 873 + -10K+Ion irradiation treatment makes the sample surface produce the crystalline layer, and inside is amorphous structure simultaneously to obtain the surface hardness and be higher than inside gradient structure, further improved amorphous alloy's intensity when promoting amorphous alloy plastic deformation ability. The modification treatment adopted by the invention is easy to control by controlling the temperature of ion irradiation and the dosage of ion implantation, thereby providing a new way for preparing controllable amorphous film materials with high strength and high plasticity.
The amorphous alloy prepared by magnetron sputtering before ion irradiation shows a phenomenon of local shear band instability expansion in a plastic deformation process, helium bubbles with certain volume fraction are injected into a sample after 873 +/-10K ion irradiation, a crystal layer is formed on the surface of the sample, and the gradient material with good internal toughness and high surface strength shows a characteristic of uniform deformation in the plastic deformation process.
Compared with other methods for improving the plastic deformation capacity of the amorphous alloy, the amorphous film with the gradient structure designed based on the high-temperature ion irradiation has good plastic deformation capacity, and simultaneously further improves the hardness of the amorphous alloy. Therefore, the method has unique advantages, is simple and easy to implement, and has obvious advantages.
Drawings
FIG. 1 shows the total thickness of 1 μm of the pre-ion irradiation W prepared according to the present invention65Ni35(at.%) transmission electron micrograph of amorphous thin film, resolution is 200nm, wherein the inset is the selected electron diffraction pattern of the surface region, the selected region is a circle of diameter 100 nm;
FIG. 2 is a view showing the preparation of W having a gradient structure by irradiation of 873 + -10K ions according to the present invention65Ni35(at.%) transmission electron micrograph of amorphous thin film. Wherein (a) is an overall graph with a resolution of 200nm, and the insets are selected electron diffraction patterns of the surface region and the inner region respectively, and the selected region is a circle with a diameter of 100 nm; (b) a partial enlargement of the surface region with a resolution of 20nm, (c) a partial enlargement of the inner region with a resolution of 5 nm;
FIG. 3 shows W before and after ion irradiation prepared by the present invention65Ni35(at.%) hardness of the amorphous film as a function of indentation depth;
FIG. 4 shows W before and after ion irradiation prepared by the present invention65Ni35(at.%) comparative plot of residual indentation morphology of amorphous films with resolution of 1 μm.
Detailed Description
The invention designs a W pair based on high-temperature ion irradiation treatment65Ni35(at.%) amorphous film is structurally modified to exhibit a "hard-on-surface-tough" gradient structure. On the basis of a high-quality amorphous film prepared by magnetron sputtering, a large amount of helium bubbles are injected into the interior of a sample through the combined action of high temperature and ion irradiation, but the amorphous structure is still maintained, and meanwhile, an obvious crystal phase appears on the surface. The samples of this gradient structure show a significantly better stiffness and plastic deformability than the samples before irradiation. The method specifically comprises the following steps:
1) ultrasonic cleaning a single-side polished monocrystalline silicon (100) substrate with acetone, alcohol and distilled water respectively, blow-drying the substrate by a hair drier, putting the substrate on a substrate table of ultrahigh vacuum magnetron sputtering equipment, and plating a film; in the preferred embodiment of the present invention, the single-side polished single crystal silicon substrate is ultrasonically cleaned with alcohol and acetone for 20min to ensure complete removal of the oxide film on the substrate surface.
2) Respectively arranging pure metal target materials (W target and Ni target) to be sputtered on target material seats corresponding to a direct current power supply and a radio frequency power supply, and controlling the sputtering rate of the targets by adjusting the power of the power supply; high-purity Ar is used as a main ionized gas, so that an effective glow discharge process is ensured. In the preferred embodiment of the invention, the power of the power supply and the corresponding deposition rate are respectively: the direct current power supply is 120 +/-6W, and the deposition rate is 6.5-7.1 nm/min; the radio frequency power supply is 80 +/-4W, and the deposition rate is 2.3-2.7 nm/min.
3) During sputtering deposition, the direct current power supply and the radio frequency power supply are respectively connected with the corresponding target materials, in order to avoid the influence of an oxide layer on the surface of the target material on the quality of a film, the pre-sputtering is firstly carried out before plating a sample, and the pre-sputtering power is as follows: 120 plus or minus 6W of direct current power supply, 80 plus or minus 4W of radio frequency power supply and 5min of pre-sputtering time. During deposition of the sample, the substrate was held in constant rotation at a rotation rate of about 175 ° -185 °/min to achieve the desired total thickness. In the preferred embodiment of the present invention, the substrate stage is performed at room temperature without heating or cooling, the total thickness of the thin film is 1 μm, and the plating is completed in one step without interruption.
4) Performing He ion irradiation treatment on the film after deposition, wherein the used He ions are monovalent ions; the irradiation temperature is 873 +/-10K; the energy of the ion beam is 120 +/-5 KeV during irradiation; the ion implantation rate during irradiation was 4.0X 1013-4.4×1013ions/cm2s; the total ion irradiation dose was 7.7X 1016-7.9×1016ions/cm2(ii) a The pressure during injection is maintained at 1.0 × 10-4-9.1×10-5Pa。
In summary, the present invention provides a method for designing an amorphous thin film with a gradient structure by high temperature ion irradiation. The invention adopts pure tungsten and pure nickel targets as sputtering target materials, the purity of the sputtering target materials is over 99.99 percent, and the prepared component is W65Ni35(at.%) and high-temp ion radiation treatment to obtain the high-strength high-plasticity amorphous film with gradient structure.
The following provides specific processes to illustrate the characteristics of the amorphous thin film material with the gradient structure and the preparation process thereof.
The specific process comprises the following steps:
1) selecting a monocrystalline silicon (100) substrate with the size consistent with that of an objective table, carrying out ultrasonic cleaning on the substrate by sequentially utilizing acetone, alcohol and distilled water, wherein the cleaning time is 20min, drying by using a hair drier, and placing on a substrate table of ultrahigh vacuum magnetron sputtering equipment for later use.
2) The pure tungsten target and the pure nickel target are arranged on the target seat, the direct current power supply is connected with the tungsten target, and the radio frequency power supply is connected with the nickel target. And (3) closing a sputtering cabin door, opening a cooling machine, pre-vacuumizing by using a mechanical pump, and opening the molecular pump when the vacuum degree reaches 100 Pa.
3) When the background vacuum degree reaches 1X 10-4And when Pa is needed, opening a valve of the argon bottle, adjusting the flow of the argon gas to 3.0ccm, opening a direct-current power supply, adjusting the direct-current power to 120 +/-6W and the radio-frequency power to 80 +/-4W, and preparing for sputtering.
4) Codeposition process parameters: power of the direct current power supply: 120 +/-6W, radio frequency power supply power: 80. + -.4W, additional substrate stage rotation, deposition temperature: and (4) room temperature. Under the parameters, the deposition rates of tungsten and nickel are respectively about 6.5-7.1 nanometers and 2.3-2.7 nanometers per minute, the deposition rates are required to be accurately obtained before film coating, and the thickness of a layer with the set thickness of 1 micrometer is obtained through one-time plating.
5) Performing He ion irradiation treatment on the film after deposition, wherein the used He ions are monovalent ions; the irradiation temperature is 873K; the energy of the ion beam is 120 +/-5 KeV during irradiation; the ion implantation rate during irradiation was 4.0X 1013-4.4×1013ions/cm2s; the total ion irradiation dose was 7.7X 1016-7.9×1016ions/cm2(ii) a The pressure during injection is maintained at 1.0 × 10-4-9.1×10-5Pa。
The microstructure and property differences of the samples before and after ion irradiation are explained below with reference to the accompanying drawings:
referring to FIGS. 1 and 2, FIGS. 1 and 2 are W before and after ion irradiation, respectively, prepared according to the present invention65Ni35(at.%) transmission electron micrograph of the film, it can be seen that the film before ion irradiation shows a single amorphous structure, and the film thickness is 1 micron. Separation deviceThe surface of the sample after the sub-irradiation is wrapped by a crystal layer, the thickness of the crystal layer is about 50 +/-3 nanometers, the inner part of the crystal layer still keeps an amorphous structure and is filled with a large number of helium bubbles, and a gradient material form with the inner part of the crystal structure and the surface of the crystal structure is formed.
Referring to fig. 3, fig. 3 is a graph showing the comparison of hardness of the amorphous thin film before and after ion irradiation according to the present invention, which is obtained by nano-indentation, with the variation of indentation depth. Wherein the hardness of the single-phase amorphous alloy before irradiation gradually reaches a plateau value (15 +/-0.45 GPa) along with the increase of the pressing depth. The samples having the gradient structure after the irradiation treatment showed a tendency that the hardness reached a maximum value first and then gradually decreased with increasing penetration depth, indicating that the surface region of the gradient structure had a higher hardness and the inner region had a relatively lower hardness value. It is noted that the hardness of the inner portion of the gradient structure, although lower relative to its surface area, is still significantly higher than that of the single-phase amorphous film prior to irradiation. Comparing the hardness before and after irradiation, the gradient structure caused by irradiation has the hardness which is obviously higher than that of single-phase amorphous alloy, and shows the performance characteristic of 'surface hard core toughness'.
Referring to FIG. 4, FIG. 4 is a comparison graph of residual indentation morphology of the amorphous thin film before and after ion irradiation, which is obtained by scanning electron microscope shooting, with an indentation depth of 1 micrometer and a strain rate of 0.05s-1. The sample before irradiation presents plastic deformation characteristics dominated by shear band deformation, no shear band is observed around the indentation of the sample after irradiation, and the gradient structure caused by irradiation has plastic deformation capability which is obviously superior to that of single-phase amorphous alloy by comparing the residual indentation morphology before and after irradiation.
In conclusion, the gradient structure with strength and plasticity obviously superior to those of single-phase amorphous alloy is prepared by means of high-temperature ion irradiation, the structure has the characteristics of surface layer crystallization and internal non-crystallization, and the gradient mechanical property of surface hard core toughness is shown, so that the strength of the gradient structure is further improved on the basis of improving the plastic deformation capacity of the amorphous alloy. Not only provides possibility for preparing controllable high-strength amorphous film material, but also provides a new idea for improving the plasticity of amorphous alloy. Moreover, the method is simple to operate and easy to implement.
Claims (5)
1. A method for preparing a gradient structure amorphous film based on high-temperature ion irradiation is characterized by comprising the following steps: firstly, a layer with the atomic percentage of W is deposited on a monocrystalline silicon (100) substrate by adopting a magnetron sputtering method65Ni35(at.%) of an amorphous film having a film thickness of 1 μm, and subjecting the amorphous film to He at 873 ± 10K+Ion irradiation treatment;
the method specifically comprises the following steps:
1) ultrasonically cleaning a single-side polished monocrystalline silicon substrate to remove an oxide film on the surface, and then putting the single-side polished monocrystalline silicon substrate on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare film coating;
2) respectively arranging a pure W (99.99 at.%) target material and a pure Ni (99.99 at.%) target material to be sputtered on a target seat;
3) when the silicon chip is sputtered and deposited, a direct current power supply and a radio frequency power supply are respectively connected with corresponding target materials, the set atomic percentage is reached through the regulation and control of the power supply power in the sputtering process, the plating time is set through the deposition rate, and finally the required total thickness is reached.
4) He is carried out on the prepared amorphous film under 873 +/-10K+And (5) ion irradiation treatment.
2. The method for preparing an amorphous thin film with a gradient structure based on high-temperature ion irradiation as claimed in claim 1, wherein in step 1), the single-side polished single-crystal silicon (100) substrate is cleaned by ultrasonic cleaning with acetone, alcohol and distilled water for 20min, and then the residual distilled water on the substrate is dried by a blower.
3. The method for preparing the amorphous film with the gradient structure based on the high-temperature ion irradiation as claimed in claim 1, wherein in the step 3), the power of the power supply and the corresponding deposition rate are respectively 120 ± 6W of the direct current power supply, and the deposition rate is 6.5-7.1 nm/min; the radio frequency power supply is 80 +/-4W, the deposition rate is 2.3-2.7nm/min, and the total thickness of the deposited film is 1 micron.
4. The method for preparing an amorphous thin film with a gradient structure based on high-temperature ion irradiation as claimed in claim 1, wherein in the step 3), the substrate stage is rotated at a constant speed at room temperature, and the rotation speed is about 175 ° -185 °/min.
5. The method for preparing the gradient-structure amorphous film based on the high-temperature ion irradiation as claimed in claim 1, wherein in the step 4), He ions are monovalent ions; the irradiation temperature is 873 +/-10K; the energy of the ion beam is 120 +/-5 KeV during irradiation; the ion implantation rate during irradiation was 4.0X 1013-4.4×1013ions/cm2s; the total ion irradiation dose was 7.7X 1016-7.9×1016ions/cm2(ii) a The pressure during injection is maintained at 1.0 × 10-4-9.1×10-5Pa。
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| CN109930122A (en) * | 2019-03-28 | 2019-06-25 | 西安交通大学 | A method of it is heterogeneous to prepare homogeneity amorphous multilayer membrane change non crystalline structure |
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| JPS61204372A (en) * | 1985-03-06 | 1986-09-10 | Univ Osaka | Method for making material amorphous by use of implantation of heterogeneous atom into solid by electron beam |
| US20090301610A1 (en) * | 2006-09-08 | 2009-12-10 | Universite D'orleans | Process for depositing a thin film of metal alloy on a substrate and metal alloy in thin-film form |
| CN1949459A (en) * | 2006-10-26 | 2007-04-18 | 昆明理工大学 | Method for directly preparing Cr-Si silicide resistance film on surface of monocrystalline silicon substrate |
| CN101660132A (en) * | 2009-09-28 | 2010-03-03 | 西安交通大学 | Method for preparing silicon-carbon hydride film by magnetron sputtering |
| CN102925869A (en) * | 2012-10-26 | 2013-02-13 | 西安交通大学 | Method for preparing amorphous/nanometer crystal multilayer-structure film |
| CN103215555A (en) * | 2013-04-11 | 2013-07-24 | 西安交通大学 | Method for preparing noncrystalline-nanocrystalline composite membrane by adopting co-sputtering method |
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| CN109930122A (en) * | 2019-03-28 | 2019-06-25 | 西安交通大学 | A method of it is heterogeneous to prepare homogeneity amorphous multilayer membrane change non crystalline structure |
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