CN100366786C - Novel metallic film preparation technology on liquid phase substrate surface - Google Patents
Novel metallic film preparation technology on liquid phase substrate surface Download PDFInfo
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- CN100366786C CN100366786C CNB2005100604619A CN200510060461A CN100366786C CN 100366786 C CN100366786 C CN 100366786C CN B2005100604619 A CNB2005100604619 A CN B2005100604619A CN 200510060461 A CN200510060461 A CN 200510060461A CN 100366786 C CN100366786 C CN 100366786C
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- metallic film
- substrate surface
- phase substrate
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Abstract
The present invention relates to technology for growing a metallic film at the liquid phase substrate surface. The present invention is characterized in that a liquid phase material is used as a substrate, wherein the saturated vapor pressure of the liquid phase material is smaller than vacuum evaporation air pressure; metal atoms are evaporated by the energy of the argon ion of high speed motion or a tungsten filament which is heated by current; then, the evaporated metal atoms are deposited to the liquid phase substrate surface, and grow into a (polycrystal) metallic film having a crystal grain structure by diffusion, nucleation, rotation and coacervation. The present invention has the advantages of simple preparation progress and low cost. The grown film has a unique microstructure, the size of crystal grains in the film can be adjusted from 10<1> nm to 10<2> nm, and the crystal grains are distributed evenly. The shape of the upper and the lower surface of the film forms a rough fractional dimension structure, a fractional dimension D is approximate to 2.2, and the film basically does not have internal stress.
Description
Technical field
The invention belongs to nano particle, nanocrystal, have the preparing technical field of the metallic film that freely supports final condition, being specifically related to the liquid phase material is substrate, the technology of preparing of preparation magnetic and non-magnetic metal film under the different base temperature.
Background technology
In the past few decades, membrane science and technical study have obtained brilliant achievement, new function film with various unique functions emerges in an endless stream, as sub-films of novel photoelectric such as huge magnetic impedance (GMR) multilayer film of finding at sophisticated superconducting thin film, the eighties grow up about the seventies superlattice film, the beginning of the nineties and the zinc oxide that occurs recent years, organic semiconductors etc., obtained using widely in high-tech areas such as modern microelectronics, information, space flight, medical treatment; Membrane theory research is (as the internal stress effect of film, diffusion, nucleation, cohesion and the membrane formation mechanism etc. of spontaneous radiation theory, atom and the cluster thereof of the associated effect of electron spinning, nanocrystal film between the multilayer film) also obtained many important breakthroughs, greatly widened membrane science and Study on Technology field, laid a solid foundation for Jie on the horizon sees the molecular device epoch.
Usually people are accustomed to adopting all kinds of solid surface as film substrate, and it not only can control the microtexture of film effectively, makes it to meet the requirement of technical project, also stabilizing films microtexture and physicals has been played crucial effect.But because lattice mismatch, film and the not first-class factor of base material thermal expansivity, therefore also be very restricted at the grow membrane system (especially monocrystal thin films) of high crystalloid of solid substrate surface, the various physical propertys of film also are subjected to the influence of substrate to a great extent.
Zhejiang University discloses a kind of employing liquid phase substrate (diffusion pump silicone oil etc.) deposition magnetic, and (Fe is Ni) with non magnetic (Au, Ag, Al, Cu) technology of metallic film [leaf Gao Xiang etc.: Phys.Rev.B54,14754 (1996); Phys.Rev.Lett., 81,622 (1998); Physics Letters A 312,119-122 (2003); Phys.Rev.B68,193403 (2003); Physics Letters A 318,457 (2003)], not only solved preferably such as lattice mismatch, film and base material thermal expansivity differ, problem such as the demoulding difficulty is big, found that also this type of film has unique physical property at aspects such as membrane formation mechanism, microstructure, the distribution of film internal stress and evolution, electronic transport characteristic, low temperature quantum effects, it is a kind of novel novel thin film that has unique microstructure and freely support final condition (internal stress free substantially).And this type of film is in general high vacuum (～10
-4Pa) under the condition, adopt ordinary methods such as vacuum-evaporation, magnetron sputtering to be prepared from, method is simple, and is with low cost, helps suitability for industrialized production.But to how the above-mentioned metallic film preparation method's of specific implementation details and key parameter are not open.Minimum sedimentation rate when for example, growing the differing materials film; The selection of liquid phase base material; Experiment synoptic diagram etc.
Summary of the invention
The magnetic with unique nano particle (or crystal grain) structure and basic internal stress free that the present invention prepares under liquid phase substrate surface and nearly room temperature condition and the purpose of non-magnetic metal film provide a kind of method that can prepare the novel metallic film with unique microstructures and unique physical effect with the vacuum evaporation method of routine, the new Application Areas of developing thin film technique, optimal preparation technology reduces industrial cost.
The present invention is to be substrate with saturated vapor pressure less than the liquid phase material of baric minimum in the vacuum chamber, adopt magnetron sputtering or hot evaporation coating method, make the atoms metal evaporation with the argon ion of high-speed motion or by the heat energy of the tungsten filament after the current flow heats, the atoms metal that is evaporated then deposits to the liquid phase substrate surface, again by diffusion, nucleation, rotation, cohesion, grow into the metallic film with polycrystalline structure, concrete processing step is as follows:
A, cleaning sanding slide glass, smear the liquid phase material that a layer thickness is 0.1～0.2mm thereon, then slide glass is packed on the substrate holder of vacuum-evaporator unit, liquid level is isolated substrate and evaporation source towards evaporation source (position up and down between slide glass and the evaporation source is not limit) with baffle plate;
B, usefulness mechanical pump and molecular pump evacuated chamber to 1 * 10
-4Pa～6 * 10
-4The vacuum tightness of Pa;
C, the substrate of heating liquid phase make it temperature between 5～50 ℃, and this moment, the vapour pressure of liquid phase material was lower than the interior air pressure of vacuum chamber;
The material of d, little heating different metal evaporation source made it degasification 3 minutes, increased tungsten filament electric current or sputtering power then to the metallic substance start vaporizer, opened baffle plate after the rate stabilization to be evaporated and began the growing metal film.Adopt the speed and the thickness of crystal oscillator thickness tester and baffle controls film growth;
E, when metallic film grows into certain thickness, cut off the power supply of evaporation source, finish growth, treat the molecular pump stall after, in vacuum chamber, slowly charge into atmosphere, take out sample;
F, carry out demoulding, obtain magnetic or non-magnetic metal film with the method for smooth glass surface adhering film.
The material of different metal evaporation source of the present invention is that purity is a kind of among 99.9%～99.99% nonmagnetic substance Au, Ag, Al, Cu or magneticsubstance Fe, the Ni.
The technology of preparing of liquid phase substrate surface novel metallic film of the present invention, the gas pressure in vacuum during growing film are～6 * 10
-4Pa.
The saturated vapor pressure of liquid phase base material of the present invention is lower than the air pressure in the vacuum chamber, can adopt glass, gallium a kind of of diffusion pump silicone oil, liquid crystal, the thawing of various models.
Nominal growth velocity at liquid phase substrate surface metallic film of the present invention is: the nominal sedimentation rate 2.0nm＞f＞0.005nm/s of magnetic metallic film; Non-magnetic metal depositing of thin film speed 2.0nm＞f＞0.001nm/s.The evaporated metal atom can be attracted to the liquid phase substrate surface and can not enter among the liquid phase substrate at this moment.
Magnetic of the present invention or non-magnetic metal film have quasi-circular island and branch shape island non-crystalline state cluster structure; Along with the film nominal thickness increases, can form have netted, vesicular, the continuous film structure of nano-sized particles, nano-sized grains, its upper and lower surface is coarse and be Fractal dimension structure, grain-size is from 10
1～10
2Nm is adjustable.
Metallic film method for demoulding of the present invention is simple and easy to operate: (1) removes to adhere to the metallic film that is grown in the liquid phase substrate surface with the flat surface of the slide glass that cleans up, film just can be adsorbed on smooth slide surface tightly, after drying with acetone and washed with de-ionized water, film just by demoulding to clean smooth slide surface, what this moment, we saw is the lower surface of film; (2) up with the pellicular front of sample; Gradually the sample crystalline substance is sunk to clean acetone liquid, film just can swim in the acetone surface, pick up film with clean smooth slide surface then, after drying with acetone and washed with de-ionized water, film just by demoulding to clean smooth slide surface, what this moment, we saw is the upper surface of film.
Technology of preparing of the present invention can adopt different types of liquid phase material, and its surface tension, viscosity factor etc. do not have special requirement.Sometimes in order to change the physical property of liquid phase substrate, the liquid phase substrate of optionally can littlely heating, but, must guarantee that the vapour pressure of liquid phase substrate is less than the air pressure in the vacuum chamber 1 * 10 no matter whether heat
-4Pa.For the structural membrane sample, the purity of evaporating materials should be better than 99.9%; And for the function film sample, the purity requirement of evaporating materials should be better than 99.99%.
Distance between evaporation source of the present invention and the substrate holder is answered 10～15cm, thereby guarantees that the liquid phase substrate can not change its physics and chemical property because of the thermal radiation of evaporation source during whole evaporation.
Wherein the slide glass purging method is as follows:
Slide glass is put into acetone to be soaked 24 hours;
Slide glass is put into ultrasonic cleaner, scrubbing one hour;
Wash repeatedly with deionized water;
At last in the vertical laminar flow clean bench with the slide glass airing.
The present invention adopts vacuum-evaporation (or magnetron sputtering) method, and (Fe is Ni) with non magnetic (Au, Ag, Al, Cu) metallic film in liquid phase substrate (diffusion pump silicone oil etc.) surface growth magnetic.The evaporated metal atom is attracted to the liquid phase substrate surface and can enter among the liquid phase substrate, their diffusions randomly, nucleation, rotation, merging, cohesion then, the final metallic film of densification continuously that forms.According to the nominal thickness difference of film, film can have quasi-circular cluster, branch shape cluster, netted, porous and shape pattern continuously, and the continuous film upper and lower surface is coarse and be Fractal dimension structure, and film is generally polycrystalline structure, and grain-size is from 10
1～10
2Nm is adjustable, and crystal grain is evenly distributed.Because this type of film is to be grown on the liquid phase substrate surface, so through after the relaxation time of several hrs, basic internal stress free in the film.
The technology of preparing of liquid phase substrate surface growing metal film of the present invention, preparation technology is simple, and cost is low; The film of being grown has unique microtexture, and grain-size is from 10 in the film
1～10
2Nm is adjustable, and is evenly distributed; Film upper and lower surface pattern is coarse Fractal dimension structure, fractal dimension D ≈ 2.2; Demoulding is simple, easily the upper and lower surface of film is studied and is used; Basic internal stress free in the film.Found multiple new physical influence at aspects such as membrane formation mechanism, microstructure, internal stress evolution, low temperature magnetic propertiess.
Description of drawings:
Fig. 1 liquid phase substrate surface vacuum evaporation deposition metallic film synoptic diagram
1 crystal oscillator thickness tester among the figure, 2 electric furnaces, 3 slide glasss, 4 liquid phase substrates, 5 baffle plates, 6 evaporated metal materials, 7 heating tungsten filaments, 8 connect molecular pump
Embodiment
Embodiment 1:
(a) with reference to Fig. 1, in the vacuum chamber of vacuum-evaporator unit, by the sanding slide glass 3 of smearing the thick liquid phase substrate 4 of one deck 0.2mm, the substrate holder that electric furnace 2 constitutes, the liquid phase substrate can be adopted glass, gallium a kind of of diffusion pump silicone oil, liquid crystal, thawing, by evaporated metal material 6, heating tungsten filament 7 constitutes evaporation sources, and the material of metal evaporation sources can adopt a kind of among nonmagnetic substance Au, Ag, Al, Cu or magneticsubstance Fe, the Ni of purity 99.9%～99.99%.Liquid level is not towards evaporation source (position up and down between them is limit) on the substrate holder, and the distance between village's underframe and the evaporation source is 10～15cm, and with baffle plate 5 they separated.Crystal oscillator thickness tester 1 is installed near the sample, cooperates evaporation source tungsten filament current control and baffle plate, is used for controlling sedimentation rate; Vacuumize by connecing molecular pump 8.
(b) with mechanical pump and molecular pump evacuated chamber to 1 * 10
-4Pa～6 * 10
-4The vacuum tightness of Pa.
(c) electric furnace heating can make the liquid phase base reservoir temperature adjustable between 5～50 ℃, and the vapour pressure of liquid phase substrate this moment is the air pressure in the vacuum chamber still;
(d) increase the tungsten filament electric current evaporated metal material is heated slightly, removed its surface adsorption gas 3 minutes.Increase the tungsten filament electric current then to the metallic substance start vaporizer.Control tungsten filament electric current is opened baffle plate and is begun the growing metal film after the rate stabilization to be evaporated, and according to practical situation control growth for Thin Film speed and thickness; The nominal sedimentation rate 2.0nm＞f＞0.005nm/s of magnetic metallic film; Non-magnetic metal depositing of thin film speed 2.0nm＞f＞0.001nm/s.
(e) when metallic film grows into certain thickness, cut off the tungsten filament power supply, finish growth, treat the molecular pump stall after, in vacuum chamber, slowly charge into atmosphere, take out sample.
(f) with the sample demoulding to preprepared clean smooth substrate surface, and dry with acetone and washed with de-ionized water.Film can have quasi-circular cluster, branch shape cluster, netted, porous and shape pattern continuously, and the continuous film upper and lower surface is coarse and be Fractal dimension structure, and film is a polycrystalline structure, and grain-size is from 10
1～10
2Nm is adjustable, and the polycrystalline metallic film homogeneous grain size of preparation gained is controlled, and upper and lower surface is coarse and be branch dimension pattern, internal stress free almost in the film.
Adopt radio frequency magnetron sputtering method at liquid phase substrate surface deposited iron film:
(a) in the vacuum chamber of rf magnetron sputtering, diffusion pump silicone oil is adopted in the liquid phase substrate, sputtering target material (being thin-film material) is for purity equals 99.99%, diameter is that 81.5mm, thickness are Armco magnetic iron (Fe) sheet material of 0.5mm, distance=10cm between substrate holder and the sputtering source, and with baffle plate they are separated.
(b) with mechanical pump and molecular pump evacuated chamber to 6 * 10
-4The vacuum tightness of Pa.
(c) the electric furnace heating can make silicone oil adjustable between 5～50 ℃, and the vapour pressure of silicone oil substrate this moment is lower than the air pressure in the vacuum chamber;
(d) increase sputtering power to the 10W, make iron target open surface degassing and pre-sputter 3 minutes.Open baffle plate then and begin plated film.With crystal oscillator thickness tester control growth for Thin Film speed is 0.005nm/s; Grain-size is from 10 in the film
1～10
2Nm is adjustable;
(e) when metallic film grows into certain thickness, cut off shielding power supply and argon gas source, finish growth, treat the molecular pump stall after, in vacuum chamber, slowly charge into atmosphere, take out sample.
(f) with the iron thin film demoulding to preprepared clean smooth substrate surface, and dry with acetone and washed with de-ionized water.The Armco magnetic iron film of preparation gained, upper and lower surface is coarse and be branch dimension pattern, internal stress free almost in the film.
Claims (9)
1. the preparation method of a liquid phase substrate surface metallic film, the liquid phase material that it is characterized in that being lower than with saturated vapor pressure the vacuum chamber internal gas pressure is substrate, adopt magnetron sputtering or hot evaporation coating method, the atoms metal of the material of different metal evaporation source is deposited to the liquid phase substrate surface, again by diffusion, nucleation, rotation, cohesion, grow into metallic film with polycrystalline structure, the material of described different metal evaporation source is a kind of of nonmagnetic substance Au, Ag, Al, Cu or magneticsubstance Fe, Ni, and processing step is as follows:
A, cleaning sanding slide glass are smeared the liquid phase material that a layer thickness is 0.1～0.2mm thereon, and as the liquid phase substrate, on the substrate holder of the vacuum-evaporator unit of then slide glass being packed into, liquid level is isolated substrate and evaporation source towards evaporation source with baffle plate;
B, usefulness mechanical pump and molecular pump evacuated chamber to 1 * 10
-4Pa～6 * 10
-4The vacuum tightness of Pa;
C, the substrate of heating liquid phase make it temperature between 5～50 ℃, and this moment, the vapour pressure of liquid phase material was lower than the interior air pressure of vacuum chamber;
The material of d, heating different metal evaporation source made it degasification after 3 minutes, increase tungsten filament electric current or sputtering power to the metallic substance start vaporizer, open baffle plate after the rate stabilization to be evaporated and begin the growing metal film, adopt the speed and the thickness of crystal oscillator thickness tester and baffle controls film growth;
E, when metallic film grows into when setting thickness, cut off the power supply of evaporation source, finish growth, treat the molecular pump stall after, in vacuum chamber, slowly charge into atmosphere, take out sample;
F, carry out demoulding, obtain magnetic or non-magnetic metal film with the method for smooth glass surface adhering film.
2. the preparation method of liquid phase substrate surface metallic film according to claim 1 is characterized in that the evaporation source of described vacuum-evaporator unit and the distance between the substrate holder are 10～15cm.
3. the preparation method of liquid phase substrate surface metallic film according to claim 1, the material that it is characterized in that described different metal evaporation source is that purity is a kind of of 99.9%～99.99% nonmagnetic substance Au, Ag, Al, Cu or magneticsubstance Fe, Ni.
4. the preparation method of liquid phase substrate surface metallic film according to claim 1, the saturated vapor pressure that it is characterized in that described liquid phase base material is lower than the vacuum chamber internal gas pressure, a kind of for the gallium of glass, liquid gallium or the molten state of the diffusion pump silicone oil of various models, liquid crystal, thawing.
5. the preparation method of liquid phase substrate surface metallic film according to claim 1 is characterized in that the cleaning step of described slide glass:
Slide glass is put into acetone to be soaked 24 hours;
Slide glass is put into ultrasonic cleaner, scrubbing one hour;
Wash repeatedly with deionized water;
In the vertical laminar flow clean bench, slide glass is carried out drying treatment at last.
6. the preparation method of liquid phase substrate surface metallic film according to claim 1, the gas pressure in vacuum when it is characterized in that growing film is 6 * 10
-4Pa.
7. the preparation method of liquid phase substrate surface metallic film according to claim 1 is characterized in that the sedimentation rate 2.0nm/s＞f＞0.005nm/s of described magnetic metallic film; Non-magnetic metal depositing of thin film speed 2.0nm/s＞f＞0.001nm/s.
8. the preparation method of liquid phase substrate surface metallic film according to claim 1 is characterized in that described magnetic or non-magnetic metal film have quasi-circular island and branch shape island non-crystalline state cluster; Along with film thickness increases, form has netted, vesicular, the continuous film structure of nano-sized particles, nano-sized grains, its upper and lower surface is coarse and be Fractal dimension structure, fractal dimension D ≈ 2.2, grain-size is from 10
1～10
2Nm is adjustable.
9. the preparation method of liquid phase substrate surface metallic film according to claim 1, it is characterized in that described metallic film method for demoulding: (1) removes to adhere to the metallic film that is grown in the liquid phase substrate surface with the flat surface of the slide glass that cleans up, film just can be adsorbed on smooth slide surface tightly, after drying with acetone and washed with de-ionized water, film just by demoulding to clean smooth slide surface; (2) up with the pellicular front of sample, gradually sample is sunk to clean acetone liquid, film just can swim in the acetone surface, picks up film with clean smooth slide surface then, after drying with acetone and washed with de-ionized water, film just by demoulding to clean smooth slide surface.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073774B (en) * | 2014-03-28 | 2017-06-30 | 能源X控股有限公司 | A kind of device for preparing nano-porous structure film and its application |
| CN104532192B (en) * | 2014-12-19 | 2018-01-30 | 深圳市华星光电技术有限公司 | Evaporation coating device |
| CN105671510B (en) * | 2016-04-07 | 2018-01-23 | 中国计量大学 | A kind of Liquid matrix deposited metal membrane separation device |
| CN110016650B (en) * | 2019-03-27 | 2021-07-16 | 吉林大学 | Method for regulating and controlling surface roughening rate of film in situ in large range |
| EP3715499A1 (en) * | 2019-03-29 | 2020-09-30 | Picosun Oy | Substrate coating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046356A (en) * | 1990-03-22 | 1990-10-24 | 四川大学 | The preparation method of film of multicomponent metal oxide |
| US20050011758A1 (en) * | 2002-06-18 | 2005-01-20 | Hannstar Display Corp. | Magnetic control oscillation-scanning sputter |
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2005
- 2005-08-23 CN CNB2005100604619A patent/CN100366786C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046356A (en) * | 1990-03-22 | 1990-10-24 | 四川大学 | The preparation method of film of multicomponent metal oxide |
| US20050011758A1 (en) * | 2002-06-18 | 2005-01-20 | Hannstar Display Corp. | Magnetic control oscillation-scanning sputter |
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