CN102925869B - Method for preparing amorphous/nanometer crystal multilayer-structure film - Google Patents
Method for preparing amorphous/nanometer crystal multilayer-structure film Download PDFInfo
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Abstract
The invention discloses a method for preparing an amorphous/nanometer crystal multilayer-structure film. The amorphous/nanometer crystal multilayer-structure film is characterized in that the amorphous/nanometer crystal multilayer-structure film is composed of two entirely different crystal structures of a nanometer crystal structure and an amorphous structure, and has a multilayer structure composed of alternately overlapped amorphous layers and nanometer crystal layers. The amorphous/nanometer crystal multilayer-structure film prepared by the method has a compact film structure and clear interface layers. The method realizes control of a blending proportion of amorphous layers and nanometer crystal layers by control of thickness sizes (reaching to nanoscale) of different film layers thereby changing a blending proportion and even gradually changing a blending proportion, provides a novel research method for shear band deformation and size effects of a micro-amorphous alloy, provides a novel approach for improvement of mechanical properties such as ductility and toughness of an amorphous alloy thereby providing possibility for preparation of a mechanical property-controllable amorphous/nanometer crystal composite material, has simple processes and a low cost, and can be industrialized and popularized easily.
Description
Technical field
The invention belongs to metallic film material technical field, relate to a kind of amorphous/nanometer crystal multilayer-structurefilm film, especially a kind of magnetron sputtering technique prepares the method for amorphous/nanometer crystal multilayer-structurefilm film.
Background technology
The glass be made up of metallic bond is called metallic glass.Different from crystalline material, the arrangement of metallic glass interior atoms has the feature of longrange disorder, short range order, and its inside does not have crystal boundary, there is not the crystal structure defects etc. such as dislocation.So metallic glass has much outstanding performance, such as: close to the compressive strength of theoretical value, good elasticity performance (elastic limit strain about 2%), good soft magnetic performance, corrosion resistance nature wear resisting property etc.In addition, it is pointed out that the viscous deformation of metallic glass is considered to the VISCOUS FLOW of supercooled liquid, and its deformational behavior has a very large change when temperature is increased to close to marquis during supercooling liquid phase region, even can carry out superplasticity processing.This excellent thermoplasticity working ability of metallic glass, what make many complex-shaped mini components is processed into possibility.
In recent years, along with the great-leap-forward development of research means and nano-fabrication technique, the behavior of amorphous material under nanoscale by large quantity research, and is widely used in MEMS, information apparatus, the contour new opplication field of senser element.At present, Pd base (Pd76Cu7Si17) and Zr base (Zr75Cu19Al6) film metal glass have been used in MEMS with its excellent processing characteristics and mechanical property.Research finds, along with the size of amorphous metal material constantly reduces, can show many totally different new phenomenons.Therefore, under nano-scale yardstick, the deformational behavior of metallic glass and mechanical property, become the study hotspot of current material educational circles.
Metallic glass inside is not similar to the structural unit such as dislocation, crystal boundary in crystalline material, and the carrier of its distortion is considered to the shearing transformation range be made up of 10 to 100 atoms.But in the middle of common experiment, the size of specimen sample is large more than this intrinsic scantlings of the structure.And the width of the shear zone that produces in partial cut process of metallic glass (being generally considered to be 10 to 1000nm), there is very large difference in the feature pitch between the displacement of shearing and shear zone and specimen size.Due to these difference in size, other exists, in various Experiments of Machanics, really there is obvious dimensional effect.If identical experiment is carried out on the sample that size is less, the dependent variable that each shear zone adapts to is certain, and the significant interval so between shear zone also can reduce accordingly.Therefore, there is certain proportionlity in the spacing between shear zone and the size of sample.Similar, the shear displacemant of single shear zone also can change accordingly to some extent along with sample size.The fracture of metallic glass is considered to occur when reaching a critical displacement level by a shear zone usually, and therefore this spatial distribution of shear zone and the dimensional effect of shear displacemant have very important influence to Materials Fracture intensity.
In addition, due under room temperature condition, the non-homogeneous viscous deformation of metallic glass is mainly by the formation of shear zone, and fast breeding, propagates, finally cause the fracture of test sample.The distortion of crystalline material then there will not be shear zone, therefore, its deformation behavior is observed can not there is interference to the shear zone of metallic glass, and the amorphous metal thin-film material so being reached nanoscale by preparation size has important Research Significance for the deformation behavior of announcement non-crystaline amorphous metal under miniature scale.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, a kind of method preparing amorphous/nanometer crystal multilayer-structurefilm film is provided, the method adopts magnetron sputtering technique, make the film of preparation (nanocrystalline by two kinds of diverse crystalline structure, amorphous) form, and present the multilayered structure that amorphous layer and nano-crystalline layers alternately alternate.Membrane structure prepared by the method is fine and close, interfacial layer is clear, can easily via control different layers film thickness size (size can reach Nano grade), control the modulation ratio of amorphous layer, nano-crystalline layers, the modulation ratio changes such as realization, or even gradual change modulation ratio change etc., for the shear zone deformation behavior of research non-crystaline amorphous metal under microsize and its dimensional effect provide a kind of new research method
The object of the invention is to solve by the following technical programs:
This method preparing amorphous/nanometer crystal multilayer-structurefilm film, comprises the following steps:
1) single-sided polishing monocrystalline silicon substrate is used respectively acetone and alcohol ultrasonic cleaning 15 ~ 30 minutes, after hair dryer dries up, put on superhigh vacuum magnetron sputtering equipment chip bench, prepare plated film;
2) using the quinary alloy target that is made up of Zr, Al, Cu, Ni, Si as the source target obtaining noncrystal membrane layer, be placed on No. 1 target seat, and source metal target is placed on No. 2 target seats, sputtering power is 30W ~ 100W, the sputtering raste of target is controlled by the power of power supply in adjustment, sedimentation rate is 2nm/min ~ 4nm/min, and the sedimentation rate of nano-crystal film is 8nm/min ~ 10nm/min; Adopt high-purity Ar as main ionization of gas, gas velocity is 6.3sccm, ensures effective glow discharging process;
3), during silicon chip sputtering sedimentation, direct current pulse power source is adopted; The preparation of amorphous layer adopts intermittent deposition mode often to deposit 5 ~ 10min, suspends sputtering 15min and film is cooled completely; The preparation of nano-crystalline layers, deposits every layer of about 5 ~ 30min, then suspends sputtering 10 ~ 30min, film is cooled completely, for the preparation of amorphous layer is prepared; Chip bench is rotated simultaneously, and apply the negative bias of 80 ~ 100V, obtain the nano-crystalline layers that crystal grain is tiny; Repeat the preparation of amorphous layer, nano-crystalline layers, finally reach required thickness and the number of plies, and corresponding modulation ratio.
Further, above step 2) in, described source target is respectively 61%, 7.5%, 17.5%, 10%, the 4% quinary alloy target suppressed by the pure element powder of purity more than 99.999% according to the atomicity percentage composition of Zr, Al, Cu, Ni, Si; The purity of high-purity Ar is 99.99%.
Above step 2) in, described source metal target adopts any metallic substance.
The present invention has following beneficial effect:
The film prepared of the method that the present invention prepares amorphous/nanometer crystal multilayer-structurefilm film is made up of two kinds of diverse crystalline structure (nanocrystalline, amorphous), and presents the multilayered structure that amorphous layer and nano-crystalline layers alternately alternate.Multilayer films prepared by the method, interface clear layer, amorphous layer, nano-crystalline layers structure are clear and definite, can make by controlling each rete thickness size (precision can reach Nano grade) easily obtained multilayered structure reach the amorphous layer of expection and nano-crystalline layers etc. modulation ratio, the modulation ratio of even gradual change.Thus, for the shear zone deformation behavior of research non-crystaline amorphous metal under microsize and its dimensional effect provide a kind of new research method, and provide a kind of new approach for the improvement of the mechanical properties such as non-crystaline amorphous metal plasticity and toughness.Thus provide possibility for the controlled amorphous/nanocrystalline matrix material of preparation mechanical property.Meanwhile, the method is simple to operate, and cost is lower, is easy to industrially realize and promote.
Accompanying drawing explanation
Fig. 1 is ZrCuNiAlSi amorphous/nanocrystalline W bilayer film profile scanning Electronic Speculum microtexture schematic diagram;
Fig. 2 is ZrCuNiAlSi amorphous/nanocrystalline W bilayer film X-ray diffraction analysis schematic diagram;
Fig. 3 is the ZrCuNiAlSi amorphous/nanocrystalline W multilayer film profile scanning Electronic Speculum microtexture schematic diagram of different modulating ratio.(a) amorphous layer 5nm, nano-crystalline layers 5nm, (b) amorphous layer 5nm, nano-crystalline layers 50nm, (c) amorphous layer 50nm, nano-crystalline layers 50nm, (d) amorphous layer 100nm, nano-crystalline layers 50nm;
Fig. 4 is under high multiple, and modulation ratio is the ZrCuNiAlSi amorphous/nanocrystalline W multilayer film profile scanning Electronic Speculum microtexture schematic diagram of 5:5;
The ZrCuNiAlSi amorphous/nanocrystalline W multilayer film high-resolution-ration transmission electric-lens microtexture schematic diagram of Fig. 5 to be modulation ratio be 5:5.
Embodiment
The method applied in the present invention; cardinal principle is: in magnetron sputtering membrane process; adopt intermittent deposition technique; film growth is made to be in lower temperature all the time; the various film layer structure of effective protection is not destroyed (if successive sedimentation plated film; hold very much and cause film temperature rising that amorphous layer structure is destroyed; nano-crystalline layers coarse grains); make can form negative mixture heat between sputtered atom by specific element proportioning, and utilize this unbalanced atomic deposition mode of magnetron sputtering and effectively obtain non-crystal structure film.In addition, arranged by the difference controlling the series of experiments parameter such as rotating speed, bias voltage, power in sputter procedure, then can realize amorphous layer film and nano-crystalline layers film, alternately alternate, thus make the constitutional features presenting " multilayer " of film.Further, under special parameter, film growth size is controlled, and modulation rate such as to reach at the desired result such as ratio or gradient scale.It is pointed out that the series of experiments parameters such as power bias voltage need to be limited, if deposition process energy is excessive, inner nanocrystalline precipitation can make non-crystal structure be destroyed.By the exploration of many experiments parameter, final acquisition interface is clear, the amorphous metal that structure is clear and definite/nanocrystalline multilayer film.
The method specifically comprises the following steps:
1) single-sided polishing monocrystalline silicon substrate is used respectively acetone and alcohol ultrasonic cleaning 15 ~ 30 minutes, after hair dryer dries up, put on superhigh vacuum magnetron sputtering equipment chip bench, prepare plated film;
2) by Zr
61al
7.5cu
17.5ni
10si
4(at%) as the source target obtaining noncrystal membrane layer, be placed in (source target is the quinary alloy target suppressed according to atomic percent by the pure element powder of purity more than 99.999%) on No. 1 target seat, and source metal target is placed in (source metal target can adopt any metallic substance) on No. 2 target seats, sputtering power is 30W ~ 100W, the sputtering raste of target is controlled by the power of power supply in adjustment, sedimentation rate is 2nm/min ~ 4nm/min, and the sedimentation rate of nano-crystal film is 8nm/min ~ 10nm/min; Adopt high-purity Ar as main ionization of gas (purity of Ar is 99.99%), gas velocity is 6.3sccm, ensures effective glow discharging process;
3), during silicon chip sputtering sedimentation, direct current pulse power source is adopted; The preparation of amorphous layer adopts intermittent deposition mode often to deposit 5 ~ 10min, suspends sputtering 15min and film is cooled completely; The preparation of nano-crystalline layers, deposits every layer of about 5 ~ 30min, then suspends sputtering 10 ~ 30min, film is cooled completely, for the preparation of amorphous layer is prepared; Chip bench is rotated simultaneously, and apply the negative bias of 80 ~ 100V, obtain the nano-crystalline layers that crystal grain is tiny; Repeat the preparation of amorphous layer, nano-crystalline layers, finally reach required thickness and the number of plies, and corresponding modulation ratio.
Below in conjunction with drawings and Examples, the present invention is described in further detail:
The present embodiment adopts Zr
61al
7.5cu
17.5ni
10si
4(at%) as the source target obtaining noncrystal membrane layer, using metal W as the source metal target obtaining nano-crystalline thin rete, amorphous/nanocrystalline multilayered film material is prepared.It should be noted that, preparation method of the present invention, nano-crystalline layers can be suitable for any material, be not limited to this embodiment.
The specific embodiment of multilayer ZrCuNiAlSi amorphous/nanocrystalline W film material:
1) with diamond blade, the monocrystalline silicon piece of single-sided polishing is cut into desired size, then ultrasonic cleaning 20 minutes distinguished by use acetone and raw spirit, after hair dryer dries up, put on superhigh vacuum magnetron sputtering equipment chip bench.
2) according to Zr
61al
7.5cu
17.5ni
10si
4(at%) atomic percent, uses the quinary alloy target gained quinary alloy target of the pure element powder compacting of purity more than 99.999% to be placed on No. 1 target seat, is placed in by metal W target on No. 2 target seats, closes sputtering hatch door, vacuumize.
3) when background vacuum reaches 3 × 10
-7during mba, open argon bottle valve, adjustment argon flow amount is 6.3sccm, opens pulse dc power, and regulating power is 30W, prepares sputtering.
4) deposition process parameters of amorphous layer: DC-pulse source power: 50W, substrate bias does not add, and additional substrate platform rotates, depositing temperature: room temperature.Under this parameter, often deposit 5min, powered-down suspends plated film 15min, and film cooling to be deposited is to room temperature, and repeated deposition process is until required amorphous thickness.
5) deposition process parameters of nano-crystalline layers: DC-pulse source power: 50W, applies the negative bias of 80V, and additional substrate platform rotates, depositing temperature: room temperature.Under this parameter, still adopt intermittent type plated film often to deposit 5min, powered-down suspends plated film 15min, after film cooling to be deposited, again carries out the deposition of thin crystal layer, until the thickness of required nano-crystalline layers.
6) repeating step 4), 5) just can obtain different modulating ratio, the amorphous/nanocrystalline multilayer film of specific dimensions.
Accompanying drawing 1 is for being ZrCuNiAlSi amorphous/nanocrystalline W bilayer film profile scanning Electronic Speculum microtexture schematic diagram.As can be seen from the figure, film combines better on base material, and bilayer film cross section is high-visible, top layer ZrCuNiAlSi noncrystal membrane, and thickness is 208.4nm, and nanocrystalline W layer film thickness is 246.2nm, and rete is fine and close, grows into film surface from substrate always.
Accompanying drawing 2 is ZrCuNiAlSi amorphous/nanocrystalline W bilayer film X-ray diffraction analysis schematic diagram.Utilize small angle x-ray diffraction (SAXD) can detect the principle of the material of top layer tens nanometer, can in order to detect the atomic structure of amorphous layer film inside.By using wide angle X-ray diffraction analysis, we can detect the interior atoms structure of the nanocrystalline W layer of more deep layer.XRD result shows, does not characterize the mutually strong diffraction peak of crystal in amorphous layer, and near 37 degree, only occurred the diffraction peak of a wide and disperse, what really demonstrate amorphous layer inside has non-crystal structure.Detect W layer, find that multiple strong diffraction peak has appearred in W layer film inside, carrying out demarcation to it can draw, W layer film inside is made up of α, β phase.
Accompanying drawing 3 is the ZrCuNiAlSi amorphous/nanocrystalline W multilayer film profile scanning Electronic Speculum microtexture schematic diagram for different modulating ratio.Multilayer film prepared as we can see from the figure has layered structure clearly, wherein white is W layer, and black layer is ZrCuNiAlSi amorphous layer, and can Repetitive controller, the ZrCuNiAlSi amorphous/nanocrystalline W multilayer film of preparation different modulating ratio, its dimensional precision reaches Nano grade.Accompanying drawing 4 is that wherein modulation ratio is the profile scanning Electronic Speculum microtexture schematic diagram of the ZrCuNiAlSi amorphous/nanocrystalline W multilayer film of 5nm:5nm, multilayered structure clear and definite as we can see from the figure, and film is fine and close, and matrix associativity is better.Accompanying drawing 5 for modulation ratio be the ZrCuNiAlSi amorphous/nanocrystalline W multilayer film high-resolution-ration transmission electric-lens microtexture schematic diagram of 5:5.As can be seen from the figure, the 5:5 multilayer film thickness size control of preparation is accurate, and interface is clear, amorphous, and nanocrystalline rete alternately alternates, and interference mutually, does not reach the requirement expected and accurately control size and the structure of noncrystal membrane.
These, illustrate that method of the present invention can be prepared size control and be accurate to nanoscale, amorphous, nanocrystalline structure clear and definite above, the novel ZrCuNiAlSi amorphous/nanocrystalline multilayered film material that quality is higher.Meanwhile, because interval time is relative with sedimentation rate fixing, writing and setting by related computer program, is convenient to realize suitability for industrialized production and popularization.
Claims (3)
1. prepare a method for amorphous/nanometer crystal multilayer-structurefilm film, it is characterized in that, comprise the following steps:
1) single-sided polishing monocrystalline silicon substrate is used respectively acetone and alcohol ultrasonic cleaning 15 ~ 30 minutes, after hair dryer dries up, put on superhigh vacuum magnetron sputtering equipment chip bench, prepare plated film;
2) using the quinary alloy target that is made up of Zr, Al, Cu, Ni, Si as the source target obtaining noncrystal membrane layer, be placed on No. 1 target seat, and source metal target is placed on No. 2 target seats, sputtering power is 30W ~ 100W, the sputtering raste of target is controlled by the power of power supply in adjustment, sedimentation rate is 2nm/min ~ 4nm/min, and the sedimentation rate of nano-crystal film is 8nm/min ~ 10nm/min; Adopt high-purity Ar as main ionization of gas, gas velocity is 6.3sccm;
3), during silicon chip sputtering sedimentation, direct current pulse power source is adopted; The preparation of amorphous layer adopts intermittent deposition mode often to deposit 5 ~ 10min, suspends sputtering 15min and film is cooled completely; The preparation of nano-crystalline layers, deposits every layer of 5 ~ 30min, then suspends sputtering 10 ~ 30min, film is cooled completely, for the preparation of amorphous layer is prepared; Chip bench is rotated simultaneously, and apply the negative bias of 80 ~ 100V, obtain the nano-crystalline layers that crystal grain is tiny; Repeat the preparation of amorphous layer, nano-crystalline layers, finally reach required thickness and the number of plies, and corresponding modulation ratio.
2. the method preparing amorphous/nanometer crystal multilayer-structurefilm film according to claim 1, it is characterized in that, step 2) in, described source target is respectively 61%, 7.5%, 17.5%, 10%, the 4% quinary alloy target suppressed by the pure element powder of purity more than 99.999% according to the atomicity percentage composition of Zr, Al, Cu, Ni, Si; The purity of high-purity Ar is 99.99%.
3. the method preparing amorphous/nanometer crystal multilayer-structurefilm film according to claim 1, is characterized in that, step 2) in, described source metal target adopts any metallic substance.
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| CN109207949B (en) * | 2018-10-23 | 2020-06-16 | 宁波工程学院 | Method for plating non-uniform multilayer film |
| CN109468590A (en) * | 2018-12-23 | 2019-03-15 | 深圳市千禾盛科技有限公司 | A kind of laminated film |
| CN111206213B (en) * | 2020-02-25 | 2021-08-13 | 西安交通大学 | AlN amorphous film and preparation method thereof |
| CN112921267B (en) * | 2020-06-08 | 2023-06-09 | 自贡市量子金属制造有限公司 | TiVZrCrAl high-entropy alloy coating on ball valve round head surface and preparation method thereof |
| 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 |
| 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 |
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| CN101736302A (en) * | 2009-12-18 | 2010-06-16 | 西安交通大学 | Preparation method of homogeneous multilayer nanometer metallic film material |
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Non-Patent Citations (1)
| Title |
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| On the amorphous and nanocrystalline Zr–Cu and Zr–Ti co-sputtered thin films;C.J. Chen et al.;《Journal of Alloys and Compounds》;20081212;第2009卷(第483期);337-340 * |
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