CN109930122A - A method of it is heterogeneous to prepare homogeneity amorphous multilayer membrane change non crystalline structure - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000012528 membrane Substances 0.000 title claims abstract description 24
- 230000008859 change Effects 0.000 title claims abstract description 11
- 239000010410 layer Substances 0.000 claims abstract description 24
- 238000000151 deposition Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 10
- 239000002356 single layer Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- 239000000956 alloy Substances 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 11
- 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
- 239000000463 material Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 5
- 239000013077 target material Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000000284 resting effect Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 abstract description 13
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 29
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- 238000007747 plating Methods 0.000 description 3
- 229910005805 NiNb Inorganic materials 0.000 description 2
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- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000013461 design Methods 0.000 description 2
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Abstract
The invention discloses a kind of methods for preparing homogeneity amorphous multilayer membrane change non crystalline structure heterogeneity.Film is made of single amorphous of the same race completely, and multilayered structure is presented.This method is using magnetron sputtering technique, during sputter coating, using intermittent deposition technique, by controlling thickness in monolayer, change free volume content, and introduce amorphous/amorphous interface, make homogeneity film that the structure feature of " multilayer " be presented, increases the structural heterogeneity of noncrystal membrane.Membrane structure prepared by the present invention is fine and close, boundary layer is apparent, can be easy to control membrane structure by control different layer thickness, thus to increase the structural heterogeneity of noncrystal membrane, the mechanical property of Amorphous Films is improved, the controllable nano material of preparation mechanical property provides may.Meanwhile this method is easy to operate, cost is relatively low, is easy to industrially realize and promote.
Description
Technical field
The invention belongs to nanometer metallic film technical field, it is related to a kind of nanoscale multilayer films, especially one
The method of kind magnetron sputtering technique preparation homogeneity amorphous multilayer films.
Background technique
Different and crystalline material, amorphous alloy show the design feature of longrange disorder, shortrange order, there is no dislocation,
The crystal structure defects such as crystal boundary, twin.Special design feature assigns amorphous alloy many excellent performances, such as higher compression
It is intensity (accessible theoretical value), preferable elastic property (elastic limit strain is about 2%), good corrosion resistance, wear-resisting
Performance etc..But under room temperature, the deformation of amorphous alloy material is easy to concentrate on the partial cut region of 10-20nm, and
And shear band quickly rises in value extension, and localization deformation occurs, eventually leads to the fracture of material, shows poor plastic deformation ability
Power, the serious engineer application for restricting amorphous alloy.
The study found that improving the structural heterogeneity of amorphous alloy, deformation localization can be effectively suppressed, improve amorphous alloy
Mechanical property.Reason may be that heterojunction structure can effectively promote the generation of multiple shear bands, and main shear band is hindered to expand
Exhibition inhibits the localization degree of deformation.In current experiment and research, the method for improving amorphous alloy heterogeneity usually has: receiving
Rice alloying, rolling, shot-peening etc..But the above method all has some limitations: introducing is nanocrystalline, and it is whole to destroy material
The non crystalline structure of body；It rolls and has sprayed method and be not easy to realize and control, belong to later period modification technology.Therefore, a kind of protecting is found
Under the premise of holding whole non crystalline structure, the method for simply and effectively improving amorphous alloy structural heterogeneity, to raising amorphous alloy
Plastic deformation behavior be of great significance.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of Homogenotic nanometer amorphous multilayer films.Film completely by
Amorphous alloy component of the same race is constituted, and multilayered structure is presented.The membrane structure of technique preparation is fine and close, boundary layer detail, can be with
It is easy to be coated with time control amorphous thickness by control, to prepare the amorphous multi-layer thin of different modulating wavelength and modulation ratio
Film provides possibility for the controllable single phase nano amorphous alloy material of preparation mechanical property.Meanwhile this method is easy to operate, cost
It is low, it is easy to industrially realize and promote.
A kind of method for preparing homogeneity amorphous multilayer membrane change non crystalline structure heterogeneity of the present invention, comprising the following steps:
1) monocrystal silicon substrate is used respectively acetone and alcohol to be cleaned by ultrasonic 10-15min to be put into super after hair dryer dries up
In high vacuum magnetron sputtering apparatus base station, prepare plated film；
2) alloy target material sputtered will be needed to be placed on target seat, the power by adjusting power supply is 30W~150W, control
The sputter rate 4-10nm/min of target processed；Using high-purity argon gas as main ionization of gas, guarantee effective glow discharging process；
3) preparation of amorphous multilayer films uses intermittent depositional mode, every deposition 2-60min, pause sputtering 2-
30min keeps film and target cooling；Base station is rotated simultaneously, repetition is coated with the process of resting, and control is coated with total duration,
It is finally reached required film thickness and the number of plies and corresponding modulation ratio.
In step 2), the alloy target material uses any material that non crystalline structure can be obtained.
In step 2), obtained multilayered structure is same components.
In step 2), DC power supply or radio-frequency power supply can be selected.
In step 3), base station is to carry out under room temperature.
In step 3), amorphous layer thickness in monolayer is adjusted by sedimentation time.
The present invention provides a kind of homogeneous multilayer nanometer amorphous alloy thin membrane materials, improve the preparation of non crystalline structure heterogeneity
Method, using magnetron sputtering intermittent deposition technique.The thin-film material of this method preparation, is made of single amorphous of the same race completely, and
Multilayered structure is presented.Membrane structure is fine and close, boundary layer detail, can be easy to by controlling different layers plastics thickness control amorphous
Film microstructure and number of interfaces change the structural heterogeneity of noncrystal membrane, thus the homogeneity controllable for preparation mechanical property
Non-crystalline material provides may；Meanwhile this method is easy to operate, and it is at low cost, it is easy to industrially realize and promote.
Detailed description of the invention
Fig. 1 is CuZr homogeneity amorphous alloy multilayer film transmission electron microscope multilayered structure schematic diagram.
Fig. 2 is the CuZr homogeneity amorphous alloy multilayer film AFM energy loss distribution map of different thickness in monolayer
Fig. 3 is that different type CuZr homogeneity amorphous alloy Multilayer-film nanometer is pressed into pop-in statistical result
Specific embodiment
Magnetron sputtering technique is utilized the present invention provides a kind of, in combination with intermittent deposition technique, preparation has different knots
The method of the amorphous/amorphous multilayered film material of homogeneity of structure heterogeneity.The present embodiment uses common Cu50Zr50Amorphous alloy is made
For sputtering target material, the homogeneous multilayer amorphous alloy thin membrane material with different structure heterogeneity is prepared, changes amorphous alloy material
Mechanical property.By controlling sputtering time, the amorphous layer with diverse microcosmic structure is obtained, and introduce different interface numbers
Amount, to change the structural heterogeneity of noncrystal membrane.
It uses acetone and alcohol to be cleaned by ultrasonic 15min respectively single-sided polishing crystalline silicon substrates, is put into after hair dryer dries up
On superhigh vacuum magnetron sputtering equipment chip bench, the amorphous alloy target sputtered will be needed to be placed on target pedestal, open plating
Power supply processed, power control are deposited on single-sided polishing monocrystalline silicon substrate in 30~150W.
The preparation of multilayered structure noncrystal membrane uses intermittent deposition mode, deposits 2-60min, suspends 2-30min, to film
Next layer is carried out after cooling to be coated with.It is coated with process to rotate chip bench, guarantees the uniformity of sputtering sedimentation.
Sputtering pause process is repeated, until obtaining preset film thickness.
Amorphous target can use the common amorphous alloy material of CuZr, NiNb and ZrCuNiAlSi.
The modulation ratio of amorphous layer can be adjusted by sputtering time in coating process in film.
The method applied in the present invention, cardinal principle are: during magnetron sputtering plating, using interval process for plating,
Amorphous homogeneity film can be made multilayered structure occur, and there is different microstructures.Amorphous interface free volume content
More compared in amorphous layer, the structural heterogeneity of noncrystal membrane increases.In addition, due to temperature raising, amorphous during being coated with
Relaxation can occur for alloy, and the free volume content in amorphous is reduced.It is coated with the time by control, changes the modulation wavelength of amorphous layer
And modulation ratio, free volume relative amount in amorphous can be regulated and controled, improve structural heterogeneity.
Embodiment 1
The specific embodiment of homogeneous multilayer amorphous CuZr film:
1) successively it is cleaned by ultrasonic monocrystalline silicon piece 15min with acetone and absolute alcohol, after hair dryer dries up, it is true is put into superelevation
On empty magnetron sputtering apparatus chip bench, prepare plated film.
2) by Cu50Zr50Source target of the alloys target as noncrystal membrane, is placed on target seat, closes sputtering hatch door, takes out
Vacuum, until background vacuum reaches 3*10-7mba。
3) it uses high-purity argon gas as main ionization of gas (purity of argon gas for 99.99%), opens argon gas bottle valve,
Adjusting argon flow is 3.0ccm, guarantees effective glow discharging process.
4) sputtering uses intermittent depositing operation, technological parameter are as follows: Dc source power: 100W；The rotation of additional substrate platform；
Depositing temperature: room temperature.Under this parameter, one group of comparison example is prepared, noncrystal membrane thickness is 1 μm: a. every deposition 35min,
It closes power supply pause and is coated with 15min, deposition and pause are respectively up to 4 times (hereinafter this sample is named as 4L)；B. every deposition
12min closes power supply pause and is coated with 5min, and deposition and pause are respectively up to 12 times (hereinafter this sample is named as 12L)；
To the CuZr amorphous layer of different-thickness successively carry out high-resolution-ration transmission electric-lens microstructure, Fourier transformation spectrogram and
Annular threshold filtering processing analysis.It has been confirmed that free volume content is more, and thickness in the lesser amorphous alloy layer of thickness
Free volume content is less in biggish amorphous layer.
It is the transmission electron microscope sectional view of homogeneous multilayer CuZr noncrystal membrane shown in referring to Fig.1, film interface is high-visible.
It is the column map of the film AFM energy loss of different thickness in monolayer referring to shown in Fig. 2.Energy in amorphous alloy
Loss is related with regional area free volume content in structure, and the structure that energy loss distribution map can reflect amorphous alloy is special
Point.In the lesser film of thickness in monolayer (4L), the halfwidth of energy loss Gaussian distribution curve is smaller, shows this noncrystal membrane knot
Structure heterogeneity is smaller；And in the lesser film of thickness in monolayer (12L), the halfwidth of energy loss Gaussian distribution curve is larger, knot
Structure heterogeneity increases.Therefore, this result confirms to use intermittent magnetically controlled sputter method, changes two kinds of homogeneities for being coated with parameter preparation
Amorphous alloy multi-layer film structure is heterogeneous different.
Embodiment 2
1) successively it is cleaned by ultrasonic monocrystalline silicon piece 15min with acetone and absolute alcohol, after hair dryer dries up, it is true is put into superelevation
On empty magnetron sputtering apparatus chip bench, prepare plated film.
2) by Cu50Zr50Source target of the alloys target as noncrystal membrane, is placed on target seat, closes sputtering hatch door, takes out
Vacuum, until background vacuum reaches 3*10-7mba。
3) it uses high-purity argon gas as main ionization of gas (purity of argon gas for 99.99%), opens argon gas bottle valve,
Adjusting argon flow is 3.0ccm, guarantees effective glow discharging process.
4) sputtering uses intermittent depositing operation, technological parameter are as follows: Dc source power: 100W；The rotation of additional substrate platform；
Depositing temperature: room temperature.Under this parameter, one group of comparison example is provided, noncrystal membrane thickness is 1 μm:
A. every deposition 12min closes power supply pause and is coated with 5min, repeats 12 (hereinafter this examinations of this deposition sputtering process
Sample is named as S1)；
B. sputtering sedimentation 14min closes power supply pause and is coated with 10min, continues to deposit 57min, closes power supply pause and is coated with
30min.Repeat this deposition pause cyclic process twice (hereinafter this sample is named as S2)；
C. sputtering sedimentation 57min closes power supply pause and is coated with 30min, continues to deposit 14min, closes power supply pause and is coated with
10min.Repeat this deposition pause cyclic process twice (hereinafter this sample is named as S3).
Nanometer indentation is carried out to three samples, corresponding the maximum shear stress when first pop-in occurs for statistics.Nanometer
Stress needed for first pop-in corresponds to shear band forming core in process of press in, the regional area structure of this stress value and this indentation
It is related.Therefore the maximum shear stress distribution curve can reflect sample structure heterogeneity.When the slope of curve is larger, show in sample
Portion's structure is more similar, and structural heterogeneity is small；When opposite curve tangent slope is smaller, show to correspond to various structures spy in sample
Point, structural heterogeneity are big.
Therefore, figure it is seen that sample S1 is compared with other two samples, structural heterogeneity is larger；And sample S2 and
S3, only change adjacent two layers is coated with sequence, and other are coated with parameter and do not change, therefore internal structure in amorphous alloy film
Approximation, structural heterogeneity is close to unanimously.
This comparative example further confirms to regulate and control thickness, the number of plies, the tune of amorphous alloy layer using intermittent magnetically controlled sputter method
System ratio etc., thus it is possible to vary the structural heterogeneity of amorphous alloy film.
It should be noted that preparation method of the present invention, can be adapted for CuZr, NiNb, CuTa,
The non-crystalline materials such as ZrCuNiAlSi are not limited to the embodiment.
Method of the invention described above can prepare Homogenotic nanometer noncrystal membrane and change structural heterogeneity, thus effectively
Improvement non-crystalline material mechanical property.Simultaneously because being coated with the time can very easily control, convenient for effective control knot
Structure is heterogeneous, realizes industrialized production and popularization.
Claims (6)
1. a kind of method for preparing homogeneity amorphous multilayer membrane change non crystalline structure heterogeneity, which is characterized in that specifically include following
Step:
1) monocrystal silicon substrate is used acetone and alcohol to be cleaned by ultrasonic 10-15min respectively and it is true is put into superelevation after hair dryer dries up
In empty magnetron sputtering apparatus base station, prepare plated film；
2) alloy target material sputtered will be needed to be placed on target seat, the power by adjusting power supply is 30W~150W, controls target
Sputter rate 4-10nm/min；Using high-purity argon gas as main ionization of gas, guarantee effective glow discharging process；
3) preparation of amorphous multilayer films uses intermittent depositional mode, every deposition 2-60min, and pause sputters 2-30min,
Keep film and target cooling；Base station is rotated simultaneously, repetition is coated with the process of resting, and control is coated with total duration, finally reaches
To required film thickness and the number of plies and corresponding modulation ratio.
2. the method for preparation homogeneity amorphous multi-layer film structure according to claim 1, which is characterized in that in step 2), institute
Alloy target material is stated using any material that non crystalline structure can be obtained.
3. the method for preparation homogeneity amorphous multi-layer film structure according to claim 1, which is characterized in that in step 2), obtain
To multilayered structure be same components.
4. the method for preparation homogeneity amorphous multi-layer film structure according to claim 1, which is characterized in that, can in step 2)
Select DC power supply or radio-frequency power supply.
5. the method for preparation homogeneity amorphous multi-layer film structure according to claim 1, which is characterized in that in step 3), base
Bottom stage is to carry out under room temperature.
6. the method according to claim 1 for preparing amorphous/amorphous multi-layer film structure, which is characterized in that non-in step 3)
Crystal layer thickness in monolayer is adjusted by sedimentation time.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110724921A (en) * | 2019-10-12 | 2020-01-24 | 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 |
| CN113718200A (en) * | 2021-08-25 | 2021-11-30 | 西安交通大学 | Method for preparing gradient-structure amorphous film based on high-temperature ion irradiation |
| 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 |
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