CN109930122B - Method for preparing homogeneous amorphous multilayer film to change heterogeneity of amorphous structure - Google Patents
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- 238000007747 plating Methods 0.000 claims description 23
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
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Abstract
The invention discloses a method for preparing a homogeneous amorphous multilayer film to change the heterogeneity of an amorphous structure. The film is completely composed of the same single amorphous and has a multilayer structure. The method adopts magnetron sputtering technology, adopts an intermittent deposition process in the sputtering coating process, changes the free volume content by controlling the thickness of a single layer, introduces an amorphous/amorphous interface, enables a homogeneous film to present the structural characteristics of multilayer, and increases the structural heterogeneity of the amorphous film. The film prepared by the invention has compact structure and clear interface layer, and can easily control the film structure by controlling the thickness of different layers, thereby providing possibility for increasing the structural heterogeneity of the amorphous film, improving the mechanical property of the amorphous film material and preparing the nano material with controllable mechanical property. Meanwhile, the method is simple to operate, low in cost and easy to realize and popularize industrially.
Description
Technical Field
The invention belongs to the technical field of nano metal films, relates to a nano-scale multilayer structure film, and particularly relates to a method for preparing a homogeneous amorphous multilayer structure film by a magnetron sputtering technology.
Background
Different from crystal materials, the amorphous alloy shows the structural characteristics of long-range disorder and short-range order, and does not have crystal structure defects such as dislocation, crystal boundary, twin crystal and the like. The special structural characteristics endow the amorphous alloy with a plurality of excellent performances, such as higher compressive strength (which can be close to a theoretical value), better elastic performance (the elastic limit strain is about 2 percent), good corrosion resistance, good wear resistance and the like. However, under the room temperature condition, the deformation of the amorphous alloy material is easily concentrated in a local shear zone area of 10-20nm, and the shear zone is rapidly increased in value and expanded to generate localized deformation, so that the material is finally fractured, the poor plastic deformation capability is shown, and the engineering application of the amorphous alloy is severely restricted.
Researches find that the structural heterogeneity of the amorphous alloy is improved, the deformation localization can be effectively inhibited, and the mechanical property of the amorphous alloy is improved. The reason may be that the heterostructure can effectively promote the generation of multiple shear bands and hinder the main shear band from expanding, suppressing the degree of localization of the deformation. In the current experiments and researches, methods for improving the heterogeneity of amorphous alloys generally comprise: nano alloying, rolling, shot blasting, etc. However, the above methods have certain limitations: introducing nanocrystalline to destroy the integral amorphous structure of the material; the rolling and spraying method is not easy to realize and control, and belongs to the later-stage modification technology. Therefore, a method for simply and effectively improving the structural heterogeneity of the amorphous alloy on the premise of keeping the integral amorphous structure is found, and the method has important significance for improving the plastic deformation behavior of the amorphous alloy.
Disclosure of Invention
The invention aims to provide a preparation method of a homogeneous nano amorphous multilayer structure film. The film is completely composed of the same amorphous alloy components and presents a multilayer structure. The film prepared by the process has compact structure and fine interface layer, and the thickness of the amorphous layer can be easily controlled by controlling the plating time, so that amorphous multilayer films with different modulation wavelengths and modulation ratios can be prepared, and the possibility of preparing single-phase nano amorphous alloy materials with controllable mechanical properties is provided. Meanwhile, the method is simple to operate, low in cost and easy to realize and popularize industrially.
The invention relates to a method for preparing a homogeneous amorphous multilayer film to change the heterogeneity of an amorphous structure, which comprises the following steps:
1) ultrasonically cleaning a monocrystalline silicon substrate with acetone and alcohol for 10-15min respectively, blow-drying with a hair dryer, and placing on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare for coating;
2) arranging an alloy target to be sputtered on a target seat, and controlling the sputtering rate of the target to be 4-10nm/min by adjusting the power of a power supply to be 30-150W; high-purity argon is used as a main ionized gas, so that an effective glow discharge process is ensured;
3) the amorphous multilayer structure film is prepared by adopting an intermittent deposition mode, and the sputtering is suspended for 2-30min every time the deposition is carried out for 2-60min, so that the film and the target material are cooled; and simultaneously, rotating the substrate table, repeating the plating stop process, and controlling the total plating time to finally reach the required film thickness and layer number and the corresponding modulation ratio.
In the step 2), the alloy target material is made of any material capable of obtaining an amorphous structure.
In step 2), the resulting multilayer structure is of the same composition.
In the step 2), a direct current power supply or a radio frequency power supply can be selected.
In the step 3), the substrate stage is carried out at normal temperature.
In step 3), the thickness of the single layer of the amorphous layer is adjusted by the deposition time.
The invention provides a homogeneous multilayer nano amorphous alloy film material, and a preparation method for improving the heterogeneity of an amorphous structure, wherein a magnetron sputtering intermittent deposition process is adopted. The film material prepared by the method is completely composed of the same single amorphous and has a multilayer structure. The film has compact structure and fine interface layer, and the microstructure and the interface quantity of the amorphous film can be easily controlled by controlling the thickness of different layers of films, so that the structural heterogeneity of the amorphous film is changed, and the possibility is provided for preparing homogeneous amorphous materials with controllable mechanical properties; meanwhile, the method is simple to operate, low in cost and easy to realize and popularize industrially.
Drawings
FIG. 1 is a schematic view of a multilayer structure of a CuZr homogeneous amorphous alloy multilayer film transmission electron microscope.
FIG. 2 is an AFM energy loss distribution diagram of CuZr homogeneous amorphous alloy multi-layer films with different single-layer thicknesses
FIG. 3 shows the statistical results of nano-indentation pop-in of different CuZr homogeneous amorphous alloy multilayer films
Detailed Description
The invention provides a method for preparing homogeneous amorphous/amorphous multilayer film materials with different structural heterogeneity by utilizing a magnetron sputtering technology and simultaneously combining an intermittent deposition process. This example uses common Cu50Zr50The amorphous alloy is used as a sputtering target material to prepare homogeneous multilayer amorphous alloy film materials with different structural heterogeneity, and the mechanical properties of the amorphous alloy materials are changed. By controlling the sputtering time, amorphous layers having different microstructures are obtained, andand different interface numbers are introduced, so that the structural heterogeneity of the amorphous film is changed.
Ultrasonically cleaning a single-side polished crystalline silicon substrate for 15min by using acetone and alcohol respectively, drying the substrate by using a hair dryer, putting the substrate on an ultrahigh vacuum magnetron sputtering device, arranging an amorphous alloy target to be sputtered on the target base, turning on a plating power supply, controlling the power to be 30-150W, and depositing on the single-side polished crystalline silicon substrate.
The preparation of the multilayer amorphous film adopts an intermittent deposition mode, the deposition is carried out for 2-60min, the suspension is carried out for 2-30min, and the next layer of plating is carried out after the film is cooled. The substrate table is rotated in the plating process, so that the uniformity of sputtering deposition is ensured.
The sputtering pause process is repeated until a predetermined film thickness is obtained.
The amorphous target can be made of CuZr, NiNb and ZrCuNiAlSi common amorphous alloy materials.
The modulation ratio of the amorphous layer in the film can be adjusted by the sputtering time in the film coating process.
The method adopted by the invention has the main principle that: in the magnetron sputtering film plating process, an intermittent plating process is adopted, so that the amorphous film with the same quality has a multilayer structure and different microstructures. The content of free volume at the amorphous interface is more than that in the amorphous layer, and the structural heterogeneity of the amorphous film is increased. In addition, the amorphous alloy relaxes due to the temperature rise during the plating process, and the free volume content in the amorphous alloy decreases. By controlling the plating time and changing the modulation wavelength and the modulation ratio of the amorphous layer, the relative content of free volume in the amorphous can be regulated and controlled, and the structural heterogeneity can be improved.
Example 1
The specific process of the homogeneous multilayer amorphous CuZr film comprises the following steps:
1) ultrasonically cleaning a monocrystalline silicon wafer for 15min by using acetone and absolute ethyl alcohol in sequence, drying the monocrystalline silicon wafer by using a hair drier, and putting the monocrystalline silicon wafer on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare for coating.
2) Mixing Cu50Zr50The alloy target is used as a source target material of an amorphous film, is arranged on a target material seat and is closed to sputteringInjecting a hatch, vacuumizing until the background vacuum degree reaches 3 x 10-7mba。
3) High-purity argon is used as main ionized gas (the purity of the argon is 99.99%), an argon bottle valve is opened, the flow of the argon is adjusted to be 3.0ccm, and an effective glow discharge process is guaranteed.
4) The sputtering adopts an intermittent deposition process, and the process parameters are as follows: power of the direct current power supply: 100W; rotating the additional substrate table; deposition temperature: and (4) room temperature. At this parameter, a set of comparative examples were prepared, the amorphous films all having a thickness of 1 μm: a. every 35min of deposition, the power supply is turned off and the plating is suspended for 15min, and the deposition and the suspension are respectively carried out for 4 times (hereinafter, the sample is named as 4L); b. the power supply is turned off and the plating is suspended for 5min every 12min of deposition, and the deposition and suspension are respectively carried out for 12 times (hereinafter, the sample is named as 12L);
and sequentially carrying out high-resolution transmission electron microscope microstructure, Fourier transform spectrogram and annular threshold filtering treatment analysis on the CuZr amorphous layers with different thicknesses. It was confirmed that the amorphous alloy layer having a smaller thickness had a larger free volume content, and the amorphous layer having a larger thickness had a smaller free volume content.
Referring to FIG. 1, which is a transmission electron microscope cross-sectional view of a homogeneous multilayer CuZr amorphous film, the film interface is clearly visible.
Referring to fig. 2, a histogram of AFM energy loss for thin films of different monolayer thicknesses is shown. The energy loss in the amorphous alloy is related to the free volume content of a local area in the structure, and the energy loss distribution diagram can reflect the structural characteristics of the amorphous alloy. In the film (4L) with smaller monolayer thickness, the half-height width of the energy loss Gaussian distribution curve is smaller, which indicates that the structural heterogeneity of the amorphous film is smaller; in the case of a film (12L) having a smaller monolayer thickness, the half-height width of the energy loss Gaussian distribution curve is larger, and the structural heterogeneity is increased. Therefore, the results prove that the heterogeneity of the two homogeneous amorphous alloy multilayer film structures prepared by changing the plating parameters by adopting the intermittent magnetron sputtering method is different.
Example 2
1) Ultrasonically cleaning a monocrystalline silicon wafer for 15min by using acetone and absolute ethyl alcohol in sequence, drying the monocrystalline silicon wafer by using a hair drier, and putting the monocrystalline silicon wafer on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare for coating.
2) Mixing Cu50Zr50The alloy target is used as a source target material of the amorphous film, is arranged on the target material seat, the sputtering cabin door is closed, and the vacuum pumping is carried out until the background vacuum degree reaches 3 x 10-7mba。
3) High-purity argon is used as main ionized gas (the purity of the argon is 99.99%), an argon bottle valve is opened, the flow of the argon is adjusted to be 3.0ccm, and an effective glow discharge process is guaranteed.
4) The sputtering adopts an intermittent deposition process, and the process parameters are as follows: power of the direct current power supply: 100W; rotating the additional substrate table; deposition temperature: and (4) room temperature. Given a set of comparative examples at this parameter, the amorphous films are all 1 μm thick:
a. the power is turned off and the plating is suspended for 5min every 12min of deposition, and the deposition sputtering process is repeated 12 times (hereinafter the sample is named as S1);
b. sputtering for 14min, turning off power supply, suspending plating for 10min, continuing to deposit for 57min, and turning off power supply, suspending plating for 30 min. This deposition pause cycle was repeated twice (hereinafter this sample was designated as S2);
c. sputtering and depositing for 57min, turning off the power supply, suspending plating for 30min, continuing to deposit for 14min, and turning off the power supply, suspending plating for 10 min. This deposition pause cycle was repeated twice (hereinafter this sample was designated as S3).
The three samples were nanoindented and the maximum shear stress corresponding to the first pop-in was counted. The first pop-in during nanoimprinting corresponds to the stress required for nucleation of shear banding, and this stress value is related to the local area structure of the nanoimprinting. The maximum shear stress profile may therefore reflect the structural heterogeneity of the sample. When the slope of the curve is larger, the internal structure of the sample is more similar, and the structural heterogeneity is small; when the slope of the tangent of the opposite curve is small, the sample is corresponding to various structural characteristics, and the structural heterogeneity is large.
Therefore, as can be seen from fig. 2, sample S1 has greater structural heterogeneity than the other two samples; in contrast, in samples S2 and S3, only the plating sequence of two adjacent layers is changed, and other plating parameters are not changed, so the internal structure of the amorphous alloy film is similar, and the structural heterogeneity is close to unity.
The comparison example further proves that the structural heterogeneity of the amorphous alloy film can be changed by regulating the thickness, the number of layers, the modulation ratio and the like of the amorphous alloy layer by adopting an intermittent magnetron sputtering method.
It should be noted that the preparation method adopted in the present invention can be applied to amorphous materials such as CuZr, NiNb, CuTa, zrcainiali, and the like, and is not limited to this example.
The method can prepare the homogeneous nano amorphous film and change the structural heterogeneity, thereby effectively improving the mechanical property of the amorphous material. Meanwhile, the plating time can be easily controlled, so that the structural heterogeneity can be effectively controlled, and the industrial production and popularization are realized.
Claims (6)
1. A method for preparing a homogeneous amorphous multilayer film to change the heterogeneity of an amorphous structure is characterized by comprising the following steps:
1) ultrasonically cleaning a monocrystalline silicon substrate with acetone and alcohol for 10-15min respectively, blow-drying with a hair dryer, and placing on a substrate table of ultrahigh vacuum magnetron sputtering equipment to prepare for coating;
2) arranging a certain alloy target to be sputtered on a target seat, and controlling the sputtering rate of the target to be 4-10nm/min by adjusting the power of a power supply to be 30-150W; high-purity argon is used as a main ionized gas, so that an effective glow discharge process is ensured;
3) the amorphous multilayer structure film is prepared by adopting the same target material intermittent deposition mode, and the sputtering is suspended for 2-30min every time the deposition is carried out for 2-60min, so that the film and the target material are cooled; and simultaneously, rotating the substrate table, repeating the plating stop process, and controlling the total plating time to finally reach the required film thickness and layer number and the corresponding modulation ratio.
2. The method according to claim 1, wherein in step 2), the alloy target is made of any material capable of obtaining an amorphous structure.
3. The method for producing a homoamorphous multilayer film structure according to claim 1, wherein in step 3), the obtained multilayer structure is of the same composition.
4. The method for preparing a homoamorphous multilayer film structure according to claim 1, wherein in step 2), a direct current power supply or a radio frequency power supply can be used.
5. The method for producing a homoamorphous multilayer film structure according to claim 1, wherein in step 3), the substrate stage is performed at normal temperature.
6. The method for producing an amorphous/amorphous multilayer film structure according to claim 1, wherein in the step 3), the thickness of the amorphous layer monolayer is adjusted by a deposition time.
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| CN110724921B (en) * | 2019-10-12 | 2021-04-06 | 华中科技大学 | Intermittent magnetron sputtering method for improving disorder of amorphous material |
| CN112662928A (en) * | 2020-12-16 | 2021-04-16 | 西安交通大学 | Amorphous-coated nanocrystalline dual-phase high-strength high-entropy alloy film and preparation method thereof |
| CN113802100A (en) * | 2021-08-25 | 2021-12-17 | 西安交通大学 | Method for regulating and controlling processing hardening capacity of amorphous/amorphous nano multilayer film |
| CN113718200B (en) * | 2021-08-25 | 2022-06-07 | 西安交通大学 | Method for preparing gradient-structure amorphous film based on high-temperature ion irradiation |
| CN115595542A (en) * | 2022-10-25 | 2023-01-13 | 吉林大学（Cn） | Superhard nano heterogeneous medium-entropy alloy film and preparation method thereof |
| CN117904581B (en) * | 2024-03-15 | 2024-06-14 | 中南大学 | High-strength and high-toughness nano multilayer metal composite material and gradient interface design method thereof |
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