CN101748366A - Ultra-fine grain metal membrane or ultra-fine grain alloy membrane and preparation method thereof - Google Patents
Ultra-fine grain metal membrane or ultra-fine grain alloy membrane and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ultra-fine grain metal membrane or an ultra-fine grain alloy membrane and a preparation method thereof. The method for preparing the ultra-fine grain metal membrane comprises the following steps: 1), selecting a substrate, and cleaning and drying the substrate; 2), adopting a physical vapor deposition process to grow a layer of membrane of metal In, Sn, Zn or Bi; 3), performing surface oxidation on the membrane of the step 2); and repeating the step 2) and the step 3) until the membrane reaches the required thickness. The grain size of the metal or alloy membrane obtained by adopting the method is between 5 and 50 nanometers; the method has the advantages of simple and controlled process, uniform sizes and shapes of products and low cost; and the ultra-fine grain membrane can be obtained without needing to improve the conventional equipment.
Description
Technical field
The invention belongs to the thin-film material preparation field, be specifically related to a kind of ultrafine grain metal or alloy film material and preparation method thereof.
Background technology
At photoelectron and semiconductor applications, the metal or alloy film is with a wide range of applications, and for example can be used as electrode materials, is used to prepare gray scale mask or is prepared into nesa coating etc. after the thermal oxidative treatment to the special metal film.Because the grain-size of this metal or alloy film directly has influence on it and uses, the researchist is devoted to reduce the grain fineness number of film always, referring to S.Hishita et al., Thin solidfilms, 464,146 (2004).Yet; at present still can't prepare ultra-fine crystalline substance and metallic film that thickness is bigger; this is because very serious such as In, Sn, the slaking in deposition process of this metalloid film of Zn, Bi; therefore cause easily that film morphology is discontinuous, grain fineness number is big and roughness is big; in addition; along with the increase of film thickness, it is big that the grain fineness number of thin-film material can become usually.Therefore how to obtain existing little grain fineness number and surface topography continuous, the thin-film material that can obtain any thickness again is a great problem in metal or alloy film preparation field always.
Summary of the invention
Therefore, the objective of the invention is to overcome the defective of above-mentioned prior art, thereby a kind of ultrafine grain metal or alloy firm and preparation method thereof are provided, wherein metal or alloy refers to metal In, Sn, Zn, Bi or InSn alloy.
The objective of the invention is to be achieved through the following technical solutions:
According to a first aspect of the invention, provide a kind of method for preparing ultra-fine grain metal membrane, this method may further comprise the steps:
Step 1): choose substrate, it is cleaned and drying treatment;
Step 2): adopt physical gas-phase deposition, growth layer of metal In, Sn, Zn or Bi film;
Step 3): film surface oxidation step 2);
Repeating step 2) and step 3) step 4):, reach desired thickness until film.
In technique scheme, described step 3) comprises: abolish vacuum, make step 2) film contact with atmosphere.
In technique scheme, described step 3) comprises: stop deposition and feed oxidizing gas to deposition space, make step 2) the film surface atomic shell oxidized.
In technique scheme, the time of described feeding oxidizing gas is 30 seconds to 2 minutes, and the dividing potential drop of described oxidizing gas is 0.1Pa～100Pa.
In technique scheme, described step 3) comprises: feed oxidizing gas to deposition space in deposition process, make step 2) the film surface atomic shell oxidized.
In technique scheme, the time of described feeding oxidizing gas is 30 seconds to 2 minutes, and the dividing potential drop of described oxidizing gas is 0.1Pa～100Pa.
In technique scheme, described substrate is glass material substrate, monocrystal chip or high molecular polymer substrate.
According to a second aspect of the invention, provide a kind of ultra-fine grain metal membrane according to method for preparing.
According to a third aspect of the present invention, provide a kind of method for preparing ultra-fine peritectic alloy film, this method may further comprise the steps:
Prepare the In film as stated above; And
Adopt physical gas-phase deposition growth one deck Sn film.
According to a fourth aspect of the present invention, provide a kind of ultra-fine peritectic alloy film according to method for preparing.
According to a fifth aspect of the present invention, provide a kind of method of preparation ultra-fine brilliant electrically conducting transparent indium tin oxide (ITO) film, this method may further comprise the steps:
Prepare the InSn alloy firm as stated above;
Heat this alloy firm.
According to a sixth aspect of the invention, provide a kind of ultra-fine brilliant electrically conducting transparent indium tin oxide (ITO) film according to method for preparing.
Compared with prior art, the present invention has the following advantages:
1.In, Sn, Zn, Bi, the grain-size of InSn metallic film can reach and be lower than 10nm, and is evenly distributed;
2. preparation method's simple controllable, production cost is low.
Description of drawings
It is following that embodiments of the present invention is further illustrated with reference to accompanying drawing, wherein:
Fig. 1 is the structural representation according to metallic film of the present invention;
Fig. 2 is X-ray diffraction (XRD) figure according to the Sn film of the embodiment of the invention 1;
Fig. 3 is the scanning electron microscope surface topography map (SEM) according to the Sn film of the embodiment of the invention 1;
Fig. 4 a is the SEM figure according to 7 layers of Sn film of the embodiment of the invention 2;
Fig. 4 b is the SEM figure according to 4 layers of Sn film of the embodiment of the invention 3;
Fig. 4 c is the SEM figure according to 2 layers of Sn film of the embodiment of the invention 4;
Fig. 4 d is the SEM figure according to 1 layer of Sn film of the embodiment of the invention 5;
Fig. 5 is the SEM figure according to the In thin-film material of the embodiment of the invention 8;
Fig. 6 is the SEM figure according to the InSn thin-film material of the embodiment of the invention 10.
Embodiment
Embodiment 1:
The method for preparing the Sn thin-film material according to embodiments of the invention 1 comprises:
Step 1): choose cover glass as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back and use dry gas to dry up, in vacuum oven with dry under 120 ℃ of-200 ℃ of temperature, take out after being cooled to room temperature;
Step 2): in the cover glass substrate of as above handling 1, adopt rf magnetron sputtering deposition the first layer metal Sn film, mode of deposition: sputtering power 20W, Ar flow are 2.0sccm, and deposition pressure is 0.5-0.6Pa, depositing time 100s, obtaining the metal Sn film thickness is 5nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out cover glass, make metallic film contact 5 seconds with atmosphere, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) deposition is 3 times, promptly obtains the thick Sn film of 20nm.
Fig. 1 is the structural representation according to metallic film material of the present invention, and wherein 1 is substrate, 2,3,4......n be illustrated respectively on the substrate 1 the layer of sedimentary film.Fig. 2 is X-ray diffraction (XRD) figure according to the Sn film of the embodiment of the invention 1, and measured as can be seen thin-film material has the diffraction peak of each crystal face in the corresponding Sn single crystal particle from this XRD figure, proves that product is the Sn monocrystalline.Fig. 3 is the scanning electron microscope surface topography map of this Sn film, and as we can see from the figure, its grain-size is roughly the same, and grain size is about 10nm, and surface topography is continuous.
Embodiment 2:
The method for preparing the Sn thin-film material according to embodiments of the invention 2 comprises:
Step 1): choose the single crystalline Si sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt AC magnetic controlled sputtering sedimentation the first layer metal Sn film in the Si substrate of as above handling, obtaining the metal Sn film thickness is 3nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out the Si sheet, make metallic film contact 10 seconds with atmosphere after, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) deposition is 7 times, promptly obtains the thick Sn metallic film of 21nm.
Fig. 4 a is that as can be seen from the figure its grain size is about 5nm according to the scanning electron microscope surface topography map of the Sn film of the embodiment of the invention 2, the continuous and homogeneous of surface topography.
Embodiment 3:
The method for preparing the Sn thin-film material according to embodiments of the invention 3 comprises:
Step 1): choose the single crystalline Si sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt AC magnetic controlled sputtering sedimentation the first layer metal Sn film in the Si substrate of as above handling, obtaining the metal Sn film thickness is 5nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out the Si sheet, make metallic film contact 10 seconds with atmosphere after, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) deposition is 4 times, promptly obtains the thick Sn metallic film of 20nm.
Fig. 4 b is that its grain size is about 10nm according to the scanning electron microscope surface topography map of the Sn film of the embodiment of the invention 3.
Embodiment 4:
The method for preparing the Sn thin-film material according to embodiments of the invention 4 comprises:
Step 1): choose the single crystalline Si sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt AC magnetic controlled sputtering sedimentation the first layer metal Sn film in the Si substrate of as above handling, obtaining the metal Sn film thickness is 10nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out the Si sheet, make metallic film contact 10 seconds with atmosphere after, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) deposition is 2 times, promptly obtains the thick Sn metallic film of 20nm.
Fig. 4 c is that its grain size is about 30nm according to the scanning electron microscope surface topography map of the Sn film of the embodiment of the invention 4.
Embodiment 5:
The method for preparing the Sn thin-film material according to embodiments of the invention 5 comprises:
Step 1): choose the single crystalline Si sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt AC magnetic controlled sputtering sedimentation the first layer metal Sn film in the Si substrate of as above handling, obtaining the metal Sn film thickness is 20nm, magnetron sputtering equipment is abolished vacuum after, take out the Si sheet, promptly obtain the thick Sn metallic film of 20nm.
Fig. 4 d is that its grain size is about 50nm according to the scanning electron microscope surface topography map of the Sn film of the embodiment of the invention 5.Comparison diagram 4a to Fig. 4 d can find: be approximately 20nm in overall film thickness, every sedimentation experiment condition is identical, and only have under the different situation of the deposition number of plies, thickness increase (being respectively 3nm, 5nm, 10nm, 20nm) along with every tunic, it is coarse that film surface becomes gradually, crystal particle scale increases, and surface topography is no longer continuous, and grain-size is homogeneous no longer also.
Embodiment 6:
The method for preparing the Sn thin-film material according to embodiments of the invention 6 comprises:
Step 1): choose the gallium nitride single crystal sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with dry gas, take out dry in vacuum oven again, cooling back;
Step 2): adopt rf magnetron sputtering deposition the first layer metal Sn film in the Si substrate of as above handling, obtaining the metal Sn film thickness is 50nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out cover glass, make metallic film contact 20 seconds with atmosphere, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) deposit 1 time, promptly obtain the thick Sn metallic film of 100nm, record its grain size and be about 100nm.
Embodiment 7:
The method for preparing the Sn thin-film material according to embodiments of the invention 7 comprises:
Step 1): choose silica glass as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt magnetically controlled DC sputtering deposition the first layer metal Sn film in the Si substrate of as above handling, obtaining the metal Sn film thickness is 10nm;
Step 3): stop sputter, feed pure oxygen in the sediment chamber, oxygen partial pressure is 5Pa, and the feeding time is 30 seconds, makes metallic film surface atom layer oxidized; Vacuumize after having led to oxygen, reach the deposition needed vacuum tightness after, repeating step 2), promptly obtain the thick Sn metallic film of 20nm.Record that the Sn grain size is about 30nm in the product.
Embodiment 8:
The method for preparing the In thin-film material according to embodiments of the invention 8 comprises:
Step 1): choose PC synthetic glass sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): in the PC synthetic glass sheet substrate of as above handling, adopt rf magnetron sputtering deposition the first layer metal In film, mode of deposition: sputtering power 30W, Ar flow are 25.0sccm, and deposition pressure is 0.06-0.08Pa, depositing time 68s, obtaining the metal Sn film thickness is 3nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out PC synthetic glass sheet, make metallic film contact 30 seconds with atmosphere, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) deposit 6 times, promptly obtain the thick In metallic film of 21nm, record its grain size and be about 10nm.
Embodiment 9:
The method for preparing the In thin-film material according to embodiments of the invention 9 comprises:
Step 1): choose the gan sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt ion sputtering method deposition the first layer metal In film in the gan sheet substrate of as above handling, obtaining the metal In film thickness is 5nm;
Step 3): after magnetron sputtering equipment abolished vacuum, take out the gan sheet, make metallic film contact 30 seconds with atmosphere, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, repeating step 2) 4 times, promptly obtain the thick In metallic film of 20nm, record its grain size and be about 30nm.
Embodiment 10:
The method for preparing the Zn thin-film material according to embodiments of the invention 10 comprises:
Step 1): choose the single crystalline Si sheet as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): in the Si substrate of as above handling, adopt electron beam deposition method deposition the first layer metal Zn film, mode of deposition: electric current 80A, depositing time 100s, obtaining metal Zn film thickness is 5nm;
Step 3): set by step 2) repeated deposition is three times, and feeds pure oxygen to deposition space in each deposition process, and the time is 1min, oxygen partial pressure remains on 10Pa, thereby make the oxidation of surface atom layer, promptly obtain the thick Zn metallic film of 20nm, its grain size is about 30nm.
Embodiment 11:
The method for preparing the Zn thin-film material according to embodiments of the invention 11 comprises:
Step 1): choose cover glass as substrate 1, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): in the cover glass substrate of as above handling, adopt hot evaporation coating method deposition the first layer metal Zn film, mode of deposition: heating current 50A, deposition pressure is 0.02-0.03Pa, depositing time 200s, obtaining metal Zn film thickness is 4nm;
Step 3): stop hot evaporation, feed pure oxygen to deposition chamber, the time is 1min, and the maintenance oxygen partial pressure is 10Pa, with the oxidation of surface atom layer; Vacuumize after having led to oxygen, reach the deposition needed vacuum tightness after, repeating step 2) deposition 4 times, promptly obtain the thick Zn metallic film of 20nm, record its grain size and be about 20nm.
Embodiment 12:
The method for preparing the Bi thin-film material according to embodiments of the invention 12 comprises:
Step 1): choose gallium arsenide single-crystal wafer as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): on the gallium arsenide single-crystal wafer of as above handling, adopt pulsed laser deposition method deposition the first layer metal Bi film, mode of deposition: power 60W, deposition pressure is 0.60-0.75Pa, depositing time 45s, obtaining metal Bi film thickness is 3nm;
Step 3): stop deposition, feed pure oxygen in pulsed laser deposition equipment, the time is 2min, and the maintenance oxygen partial pressure is 50Pa, and the surface atom layer is carried out oxidation; Vacuumize after having led to oxygen, reach the deposition needed vacuum tightness after, repeating step 2) deposition 6 times, promptly obtain the thick Sn metallic film of 21nm, record its grain size and be about 5nm.
Embodiment 13:
The method for preparing the Bi thin-film material according to embodiments of the invention 13 comprises:
Step 1): choose the Si single-chip as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): on the gallium arsenide single-crystal wafer of as above handling, adopt the long-pending method deposition of electron beam evaporation the first layer metal Bi film, mode of deposition: electric current 60A, deposition pressure is 0.60-0.75Pa, depositing time 45s, obtaining metal Bi film thickness is 5nm;
Step 3): set by step 2) repeated deposition is three times, and is feeding pure oxygen in each deposition process in electron beam evaporation equipment, and the time is 2min, the maintenance oxygen partial pressure is 5Pa, with the oxidation of surface atom layer, promptly obtain the thick Bi metallic film of 20nm, its grain size is about 10nm.
Embodiment 14:
The method for preparing the ITO transparent conductive film according to embodiments of the invention 14 comprises:
Step 1): choose cover glass as substrate, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen, take out dry in vacuum oven again, cooling back;
Step 2): adopt hot vapor deposition the first layer metal In film in the cover glass substrate of as above handling, thickness is 6nm;
Step 3): after hot evaporated device abolished vacuum, take out cover glass, make metallic film contact 20 seconds with atmosphere, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, according to step 2) repeated deposition twice, promptly obtain the thick In metallic film of 18nm;
Step 4): continue the thick Sn film of deposition 2nm, promptly obtain In and Sn volume ratio and be 9: 1 InSn alloy firm; (record its grain size and be about 10nm);
Step 5): this film is put into box-type furnace, heated 1 hour down, can obtain corresponding ITO transparent conductive film at 500 ℃.
Embodiment 15:
The method for preparing the ITO transparent conductive film according to embodiments of the invention 15 comprises:
Step 1): choose PMMA synthetic glass sheet as substrate 1, adopt conventional semi-conductor cleaning that this substrate is cleaned up, clean up the back taking-up and dry up with nitrogen;
Step 2): adopt radio frequency magnetron sputtering method metal refining In film in the PMMA synthetic glass sheet substrate of as above handling, thickness is 5nm;
Step 3): after rf magnetron sputtering equipment abolished vacuum, take out cover glass, metallic film is contacted the several seconds with atmosphere, put it into equipment again, vacuumize, after reaching the needed vacuum tightness of deposition, according to this step 2) repeated deposition four times, promptly obtain the thick In metallic film of 25nm;
Step 4): deposit thickness is the Sn metallic film of 5nm, promptly obtains In and Sn volume ratio and be 5: 1 InSn alloy firm; (record its grain size and be about 10nm);
Step 5): this film is put into box-type furnace, heated 1 hour down, can obtain corresponding ITO transparent conductive film at 500 ℃.
With embodiment 1～15 resulting final product row in the following Table 1.
Table 1
From embodiment 1 to 15 as can be seen, the present invention adopts following three kinds of modes to be implemented in film surface oxidation in the preparation process: after (1) abolishes vacuum with sedimentary environment, substrate taken out together with metallic film contact, make under the 1atm normal atmosphere metal material surface atom oxidized with air is of short duration; (2) to the deposition space aerating oxygen, make metallic film place oxygen atmosphere to realize that the surface atom layer is oxidized, and then descend the deposition of thin film or when stopping deposit film; (3) or at the feeding oxidizing gas of deposition process discontinuous, make the several layers of atom in metallic film surface oxidized.Wherein, the film-formation result of mode (1) is better, because can be rapidly and obtain oxidation fully at a normal atmosphere lower surface atom, and the advantage of mode (2), (3) be that technology is continuous, does not need to interrupt and manual operation.
In the above among the embodiment, sample and atmosphere duration of contact only are schematically, are generally the several seconds get final product, to realize the oxidized purpose of several atomic shells of very thin surface, just put back at once and can be effective after taking out sample in generally testing.The speed of carrying out oxidation owing to contact atmosphere surface is very fast, and the present invention only needs several atomic shells of very thin surface oxidized, so be oxidable finishing in the short period of time, the time is long more nonsensical, therefore preferably between 5 to 20 seconds.No matter be mode (2) or (3), the dividing potential drop of aerating oxygen is generally high more good more, but on the one hand owing to equipment claimed in the deposition process keeps vacuumizing always, therefore when using molecular pump etc. that vacuum tightness is had the equipment of requirement, it is desired than high atmospheric pressure that the sediment chamber can not reach, oxygen partial pressure can only reach tens handkerchiefs (if having only mechanical pump, then can reach higher air pressure) at most; On the other hand, the air pressure in the sediment chamber is too high, in the time of can causing equipment to recover deposition the required time that vacuumizes longer, therefore, consider above two aspect factors, the dividing potential drop scope of institute's aerating oxygen is preferred at 0.1Pa-100Pa.In addition, logical oxygen time range was generally 30 seconds-2 minutes, preferably can reach oxidation effectiveness about 1 minute, and overlong time is nonsensical.
For those having ordinary skill in the art will appreciate that, the substrate that the foregoing description adopted is only for schematic, can also adopt glass material substrate or the monocrystal chip except that single crystalline Si sheet, gallium arsenide substrate, gan substrate except that cover glass, slide glass, silica glass or remove PMMA, the high molecular polymer substrate that the PC substrate is outer.In above-mentioned technical scheme, can also adopt the physical gas-phase deposition except that magnetically controlled DC sputtering, rf magnetron sputtering, ion sputtering, electron beam evaporation, hot evaporation, pulsed laser deposition method.Described oxidizing gas is the mixed gas of oxygen, pressurized air or oxygen and nitrogen.During deposition InSn alloy firm, sedimentary sequence can be put upside down, promptly deposit In behind the deposition Sn earlier, and the two can be arbitrary proportion.
Because the film crystal particle scale along with the thickness of film increases and the slaking increase, therefore in the present invention by reducing film thickness control crystal particle scale, comes crystal grain thinning by the ratio that improves nucleation rate and grain growth speed.In the present invention, the metallic film surface that is exposed in the oxygen atmosphere (for example air or oxidizing gas) will form the very thin zone of oxidation of one deck, this can stop the continued growth of metal grain, can " freeze " nuclear of also not growing up, the deposition process that makes next step is forming core again, and repeat this process, prepare the metal or alloy film of ultra-fine crystalline substance thus.The metal or alloy film of this ultra-fine crystalline substance has lot of advantages, for example can directly be used in fields such as transmitter, ito thin film, photoelectric device, and the gas sensing property and the grain size of respective metal oxide compound are inversely proportional to, and can improve the gray level of metallic film and resolving power etc.In addition, adopt preparation method of the present invention can realize that the film crystal particle scale is adjustable between 5nm-100nm, film thickness is adjustable between 3nm-1 μ m, and do not need to introduce other element dopings in the whole preparation process, need not base material is carried out temperature adjustment (heating or cooling), therefore have advantages such as simple and convenient, low cost.Can be on the basis of existing equipment instrument realize that by simple adjustment operation large-area pattern continuously and the granularity thin-film material of homogeneous substantially.
Although the present invention is made specific descriptions with reference to the above embodiments, but for the person of ordinary skill of the art, should be appreciated that and to make amendment based on content disclosed by the invention within spirit of the present invention and the scope or improve not breaking away from, these modifications and improving all within spirit of the present invention and scope.
Claims (13)
1. method for preparing ultra-fine grain metal membrane, this method may further comprise the steps:
Step 1): choose substrate, it is cleaned and drying treatment;
Step 2): adopt physical gas-phase deposition, growth layer of metal In, Sn, Zn or Bi film;
Step 3): film surface oxidation step 2);
Repeating step 2) and step 3) step 4):, reach desired thickness until film.
2. method according to claim 1 is characterized in that, described step 3) comprises: abolish vacuum, make step 2) film contact with atmosphere.
3. method according to claim 1 is characterized in that, described step 3) comprises: stop deposition and feed oxidizing gas to deposition space, make step 2) the film surface atomic shell oxidized.
4. method according to claim 3 is characterized in that, the time of described feeding oxidizing gas is 30 seconds to 2 minutes, and the dividing potential drop of described oxidizing gas is 0.1Pa～100Pa.
5. method according to claim 1 is characterized in that, described step 3) comprises: feed oxidizing gas to deposition space in deposition process, make step 2) the film surface atomic shell oxidized.
6. method according to claim 5 is characterized in that, the time of described feeding oxidizing gas is 30 seconds to 2 minutes, and the dividing potential drop of described oxidizing gas is 0.1Pa～100Pa.
7. method according to claim 1 is characterized in that, described substrate is glass material substrate, monocrystal chip or high molecular polymer substrate.
8. method according to claim 7 is characterized in that, described glass material substrate comprises common lid slide, slide glass or silica glass; Described monocrystal chip comprises single crystalline Si sheet, gallium arsenide substrate, gan substrate; Described high molecular polymer substrate comprises PMMA, the PC substrate.
9. ultra-fine grain metal membrane according to each described method preparation in the claim 1 to 8.
10. method for preparing ultra-fine peritectic alloy film, this method may further comprise the steps:
Prepare the In film by each described method in the claim 1 to 8; And
Adopt physical gas-phase deposition growth one deck Sn film.
11. ultra-fine peritectic alloy film according to the described method preparation of claim 10.
12. a method for preparing ultra-fine brilliant electrically conducting transparent indium tin oxide (ITO) film, this method may further comprise the steps:
Prepare the InSn alloy firm by the described method of claim 10;
Heat this alloy firm.
13. ultra-fine brilliant electrically conducting transparent indium tin oxide (ITO) film according to the described method preparation of claim 12.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147061A (en) * | 2013-03-21 | 2013-06-12 | 上海理工大学 | Method for preparing amorphous transparent zinc oxide film |
| CN105048103A (en) * | 2015-06-25 | 2015-11-11 | 电子科技大学 | Preparing method for ultrathin metallic film for absorbing terahertz waves |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147061A (en) * | 2013-03-21 | 2013-06-12 | 上海理工大学 | Method for preparing amorphous transparent zinc oxide film |
| CN103147061B (en) * | 2013-03-21 | 2015-07-08 | 上海理工大学 | Method for preparing amorphous transparent zinc oxide film |
| CN105048103A (en) * | 2015-06-25 | 2015-11-11 | 电子科技大学 | Preparing method for ultrathin metallic film for absorbing terahertz waves |
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