CN111725298B - Rutile titanium dioxide single crystal film-substrate material heterostructure and preparation method thereof - Google Patents
Rutile titanium dioxide single crystal film-substrate material heterostructure and preparation method thereof Download PDFInfo
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- CN111725298B CN111725298B CN202010545318.3A CN202010545318A CN111725298B CN 111725298 B CN111725298 B CN 111725298B CN 202010545318 A CN202010545318 A CN 202010545318A CN 111725298 B CN111725298 B CN 111725298B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000013078 crystal Substances 0.000 title claims abstract description 63
- 239000000758 substrate Substances 0.000 title claims abstract description 50
- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 14
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010410 layer Substances 0.000 claims description 45
- 239000010408 film Substances 0.000 claims description 29
- 150000002500 ions Chemical class 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000005468 ion implantation Methods 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000002513 implantation Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 239000012790 adhesive layer Substances 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000000861 blow drying Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000007747 plating Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 230000032900 absorption of visible light Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
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- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0603—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by particular constructional design considerations, e.g. for preventing surface leakage, for controlling electric field concentration or for internal isolations regions
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract
The invention discloses a rutile titanium dioxide single crystal film-substrate material heterostructure and a preparation method thereof, wherein the heterostructure is composed of a rutile titanium dioxide single crystal film (2) with submicron thickness and a silicon dioxide substrate layer (3), and further comprises a first bonding layer (41) and a second bonding layer (42) which are arranged below the silicon dioxide substrate layer (3), a copper-tin compound bonding layer (7) which is arranged between the first bonding layer (41) and the second bonding layer (42), and a rutile titanium dioxide single crystal block body (8) which is arranged below the second bonding layer (41). The rutile titanium dioxide single crystal film-substrate material heterostructure prepared by the invention not only has the rutile titanium dioxide film with good single crystal property, but also can be prepared into various heterostructures by selecting proper substrate materials according to application requirements, overcomes the difficulty of an epitaxial growth method for preparing the single crystal film heterostructure, and lays a foundation for the application of the rutile titanium dioxide film in photoelectric devices.
Description
Technical Field
The invention relates to the field of manufacturing of photoelectric integrated devices, in particular to a submicron rutile titanium dioxide single crystal film-substrate material heterostructure prepared by combining ion implantation with a copper-tin bonding technology and a preparation method thereof.
Background
The manufacturing and performance improvement of micro-nano photoelectric devices play a crucial role in promoting the development of hotspot fields such as electronic communication, quantum information, photoelectric detection and the like, and the preparation of a material single crystal film heterostructure is a key factor for realizing the high-performance micro-nano photoelectric devices, for example, a silicon wafer film heterostructure (SOI) on an insulating substrate which is widely applied to a semiconductor integrated device is used for adjusting the refractive index contrast of a silicon wafer film and a substrate material by selecting the substrate material, and further, the integrated photoelectric devices with excellent performance, such as an optical filter, an optical switch, an optical modulator and other functional devices, are prepared by combining with a Micro Electro Mechanical System (MEMS); the successful preparation of the lithium niobate single crystal thin film heterostructure (LNOI) realizes an important breakthrough in the application of micro-nano photoelectric devices, realizes high-speed electro-optical modulation by manufacturing a high-Q-value micro-ring resonator on the LNOI, and firstly manufactures a wide-spectrum optical frequency comb source with the spectrum bandwidth exceeding 80nm on the basis of the high-speed electro-optical modulation, and performs optical frequency measurement and optical frequency comb source with precise time measurementThe method has wide application in the fields of spectral analysis, optical communication, optical ranging and the like. However, the application of SOI devices is limited by the absorption of visible light by silicon wafers, and the Q value of the micro-ring resonator is difficult to further increase due to the small refractive index of lithium niobate, so that more thin film structures of photoelectric materials with excellent performance need to be expanded. Rutile titanium dioxide (r-TiO) with advantages of large refractive index, wide light transmission range, good nonlinear effect and the like2) The defects of SOI and LNOI structures in photoelectric application can be overcome, the Whispering Gallery Mode Resonator (WGMR) with visible light wave band, small size and high Q value can be manufactured on the film heterostructure through the micro-nano processing technology, and the method has important application value in the fields of optical fiber communication, nano lasers, photoelectric detection and the like. However, the conventional methods for preparing epitaxial growth films, such as sputtering, chemical vapor deposition, sol-gel, etc., are difficult to obtain rutile titanium dioxide single crystal film structures.
At present, most rutile titanium dioxide films prepared by epitaxial growth methods are polycrystalline or amorphous structures, and the single crystal property of the films is the premise of ensuring the application performance of the films. Although the single crystal film of rutile titanium dioxide can be grown by homoepitaxy by using a Metal Organic Chemical Vapor Deposition (MOCVD) method, a single crystal film heterostructure meeting the application requirements of photoelectric devices cannot be realized.
Disclosure of Invention
The invention aims to provide a rutile titanium dioxide single crystal film-substrate material heterostructure and a preparation method thereof, which utilize the technical means of combining ion implantation with copper-tin bonding to realize the preparation of a large-size and high-quality submicron rutile titanium dioxide single crystal film heterostructure bound on substrate materials such as silicon dioxide and the like.
The invention is realized by the following technical scheme:
a method for preparing a heterostructure of a rutile titanium dioxide single crystal film-substrate material comprises the following steps:
step 1, injecting He ions with the energy of 200keV into the rutile titanium dioxide single crystal block material along the crystal direction under the condition of low-temperature liquid nitrogen, wherein the injection dose is 8 multiplied by 1016Ion/cm, the implantation surface is polished and the implantation direction is parallel to rutile titanium dioxide [001 ]]The crystal orientation, the injected ions are gathered into bubbles in the damage layer area at the end of the range;
and 3, after cleaning, starting coating: firstly, depositing a substrate layer on the injection surface of a rutile titanium dioxide sample, and then finishing metal coating of copper, tin and the like on the substrate layer and the surface of another prepared rutile titanium dioxide single crystal block material;
and 5, after copper-tin bonding, carrying out annealing treatment to realize film stripping. Samples of rutile titanium dioxide bound to a substrate material were tested at 400oC, annealing for 10 hours under the temperature condition, and after the temperature is reduced to the room temperature, stripping the rutile titanium dioxide single crystal film to finish the preparation of the heterostructure consisting of the rutile titanium dioxide single crystal film and the substrate material.
In the step 2, the injected gold red titanium dioxide sample is cleaned by adopting a chemical solvent ultrasonic cleaning mode, and the specific operation is as follows: and respectively carrying out ultrasonic treatment on the acetone and the isopropanol for 5-10 minutes, then carrying out ultrasonic treatment on the acetone and the isopropanol for 5-10 minutes by using deionized water, blow-drying by using a nitrogen gun, soaking in concentrated sulfuric acid for 5-10 minutes, and then washing for more than 4 times by using the deionized water until the surface is free of dirt.
In the step 3, the coating is started, specifically comprising the following steps: firstly, depositing a silicon dioxide substrate layer with the thickness of 2 microns on the injection surface of rutile titanium dioxide by using a plasma enhanced chemical vapor deposition method; then, sequentially plating a chromium layer with the thickness of 100 nanometers and a copper layer with the thickness of 5 micrometers on the surfaces of the deposited silicon dioxide substrate and the other untreated rutile titanium dioxide block material through magnetron sputtering; finally, a 1.5 micron thick tin layer was evaporated again on the copper layer by a thermal evaporator.
The copper-tin compound bonding in the step 4 is realized by the following specific processes: quickly heating to 150 deg.C from room temperatureoC, at 150oC, pressing the ion implantation sample of the rutile titanium dioxide and the coating surface of the pure sample together, keeping the constant temperature for 5 minutes, and then continuously heating to 270 DEG CoC, the rate of temperature rise is 5oC/min, at 270oAnd C, keeping the temperature constant for 20-30 minutes, and then naturally cooling to room temperature to complete copper-tin bonding.
The rutile titanium dioxide single crystal film-substrate material heterostructure prepared by the preparation method of the rutile titanium dioxide single crystal film-substrate material heterostructure further comprises a first bonding layer 41 and a second bonding layer 42 which are arranged below the silicon dioxide substrate layer 3, a copper-tin compound bonding layer 7 which is arranged between the first bonding layer 41 and the second bonding layer 42, and a rutile titanium dioxide single crystal block body 8 which is arranged below the second bonding layer 41.
Compared with the prior art, the invention has the advantages and positive effects that:
the rutile titanium dioxide single crystal film-substrate material heterostructure prepared by the invention not only has a rutile titanium dioxide film with good single crystal property, but also can be prepared into various heterostructures by selecting proper substrate materials according to application requirements, thereby overcoming the challenges and difficulties of an epitaxial growth method for preparing the single crystal film heterostructure and laying a solid foundation for the application of the rutile titanium dioxide film on photoelectric devices.
Drawings
FIG. 1 is a schematic diagram of a rutile titanium dioxide single crystal thin film-substrate heterostructure prepared by ion implantation combined with copper-tin bonding technology according to the present invention;
FIG. 2 is a schematic diagram of the method for preparing a rutile titanium dioxide single crystal film heterostructure by combining ion implantation with copper-tin bonding technology according to the present invention;
FIG. 3 is a cross-sectional view of a scanning electron microscope of a rutile titanium dioxide single crystal film prepared by ion implantation combined with copper-tin bonding in an embodiment of the present invention;
reference numerals:
1. the rutile titanium dioxide injection sample comprises 2 rutile titanium dioxide single crystal thin films, 3 silicon dioxide substrate layers, 4 chromium layers, 41 first bonding layers, 42 first bonding layers, 5 copper layers, 6 tin layers, 7 copper-tin compound bonding layers, 8 rutile titanium dioxide single crystal blocks, 9 damage layers.
Detailed Description
The technical solution of the present invention is described in detail below with reference to the accompanying drawings and examples.
FIG. 1 shows a schematic diagram of the heterostructure of a rutile titanium dioxide single crystal thin film-substrate material of the present invention. The structure consists of a sub-micron thick rutile titanium dioxide single crystal thin film 2 and a silicon dioxide substrate layer 3, the substrate material comprising, in addition to a thin layer of material (such as a thin layer of silicon dioxide) required to form a heterostructure of greater refractive index difference, first and second adhesive layers 41, 42 (e.g. chromium layers), a copper-tin compound bonding layer 7 and a bulk body 8 of rutile titanium dioxide single crystal.
As shown in fig. 2, which is a schematic flow chart of the present invention for preparing a rutile titanium dioxide single crystal thin film-substrate material heterostructure by combining ion implantation with copper-tin bonding, light ions (H ions or He ions) with low energy and high dose are implanted into a rutile titanium dioxide single crystal bulk material under normal temperature or low temperature conditions, during annealing, the implanted ions and the formed defects are converged together to form larger bubbles, and the rutile titanium dioxide single crystal thin film bound on the substrate material such as silicon dioxide is peeled off by the stress action exerted by the substrate material with copper-tin bonding, thereby completing the preparation of the heterostructure. The process specifically comprises the following steps:
step 1, light ions (such as H ions or He ions) with the energy of 200keV are adopted to be injected into the titanium dioxide single crystal block material of the rutile crystal phase along the crystal orientation under the condition of low-temperature liquid nitrogen, and the injection dosage is 8 multiplied by 1016Ions per square centimeter; when ions are implanted into the rutile titanium dioxide single crystal block material, the implanted ions are He ions or H ions, the implanted surface is a polished surface, and the implantation direction is parallel to the rutile titanium dioxide [001 ]]A crystal orientation;
if the room temperature is selected for ion implantation, the density range of the implanted beam current is required to be 1-3 microamperes/square centimeter so as to reduce the crystal surface damage caused by thermal deposition and the damage to the single crystallinity of the stripped film; if low-temperature ion implantation is selected, the ion beam current density is not limited;
the energy of the implanted ions determines the thickness of the stripped monocrystalline film, the thinner the energy is, for example, the implantation of He ions with 200keV energy can strip the rutile titanium dioxide monocrystalline film with submicron thickness of about 700 nm;
the larger the dose of the implanted ions, the more defects caused by the ions in the damaged layer, and more bubbles can be formed in the annealing process, but the larger the dose of the implanted ions can damage the single crystallinity of the film to be stripped.
And 3, after cleaning, performing film coating treatment on the injection surface of the sample and the surface of another untreated rutile titanium dioxide single crystal block material (the tangential direction of the rutile titanium dioxide single crystal block material is consistent with that of the sample). First, a 2 micron thick silicon dioxide substrate layer was deposited on the rutile titanium dioxide implantation surface by Plasma Enhanced Chemical Vapor Deposition (PECVD); secondly, sequentially plating a chromium layer with the thickness of 100 nanometers and a copper layer with the thickness of 5 micrometers on the deposited silicon dioxide substrate and the other rutile titanium dioxide block material through magnetron sputtering; finally, a tin layer with the thickness of 1.5 microns is evaporated on the copper layer through a thermal evaporation instrument.
And 4, after all the coating is finished, pressing the coating surfaces of the rutile titanium dioxide ion implantation sample and the pure sample together in a nitrogen environment, and realizing copper-tin bonding through high-temperature annealing treatment. Quickly heating to 150 deg.C from room temperatureoC, at 150oKeeping the temperature of the C constant for 5 minutes, and then continuously heating to 270 DEG CoC, the rate of temperature rise is 5oC/min, at 270oAnd C, keeping the temperature constant for 20-30 minutes, and then naturally cooling to room temperature to complete copper-tin bonding.
And 5, after copper-tin bonding, carrying out annealing treatment to realize film stripping. Samples of rutile titanium dioxide bound to a substrate material were tested at 400oC, annealing for 10 hours at the temperature, and peeling the film after the temperature is reduced to room temperature.
Claims (5)
1. A method for preparing a heterostructure of a rutile titanium dioxide single crystal film-substrate material is characterized by comprising the following steps:
step 1, injecting He ions with the energy of 200keV into the rutile titanium dioxide single crystal block material along the crystal direction under the condition of low-temperature liquid nitrogen, wherein the injection dose is 8 multiplied by 1016Ion/cm, the implantation surface is polished and the implantation direction is parallel to rutile titanium dioxide [001 ]]The crystal orientation, the injected ions are gathered into bubbles in the damage layer area at the end of the range;
step 2, after ion implantation is finished, cleaning the implanted rutile titanium dioxide sample to remove organic and inorganic stains on the surface of the sample and ensure the surface of the sample to be flat and clean;
and 3, after cleaning, starting coating: firstly, depositing a substrate layer on the injection surface of a rutile titanium dioxide sample, and then finishing metal coating of copper, tin and the like on the substrate layer and the surface of another prepared rutile titanium dioxide single crystal block material;
step 4, after finishing all coating operations, pressing the coating surfaces of the rutile titanium dioxide sample and the pure sample which are subjected to ion implantation into one in a nitrogen environmentFirstly, the copper-tin compound bonding is realized through heating treatment, and the heating range is between room temperature and 300 DEG CoC, keeping the temperature for 5-60 minutes;
step 5, after copper-tin bonding, film stripping is realized through annealing treatment, and the rutile titanium dioxide sample bound with the substrate material is treated at 400 DEGoC, annealing for 10 hours under the temperature condition, and after the temperature is reduced to the room temperature, stripping the rutile titanium dioxide single crystal film to finish the preparation of the heterostructure consisting of the rutile titanium dioxide single crystal film and the substrate material.
2. The method for preparing the heterostructure of rutile titanium dioxide single crystal thin film-substrate material in claim 1, wherein in the step 2, the cleaning treatment of the injected rutile titanium dioxide sample adopts a chemical solvent ultrasonic cleaning mode, and the specific operations are as follows: and respectively carrying out ultrasonic treatment on the acetone and the isopropanol for 5-10 minutes, then carrying out ultrasonic treatment on the acetone and the isopropanol for 5-10 minutes by using deionized water, blow-drying by using a nitrogen gun, soaking in concentrated sulfuric acid for 5-10 minutes, and then washing for more than 4 times by using the deionized water until the surface is free of dirt.
3. The method for preparing a heterostructure of rutile titanium dioxide single crystal thin film-substrate material in claim 1, wherein in the step 3, the coating is started by the following specific operations: firstly, depositing a silicon dioxide substrate layer with the thickness of 2 microns on the injection surface of rutile titanium dioxide by using a plasma enhanced chemical vapor deposition method; then, sequentially plating a chromium layer with the thickness of 100 nanometers and a copper layer with the thickness of 5 micrometers on the surfaces of the deposited silicon dioxide substrate and the other untreated rutile titanium dioxide block material through magnetron sputtering; finally, a 1.5 micron thick tin layer was evaporated again on the copper layer by a thermal evaporator.
4. The method for preparing the heterostructure of rutile titanium dioxide single crystal thin film-substrate material of claim 1, wherein the step 4 of realizing the bonding of the copper-tin compound comprises the following specific steps: quickly heating to 150 deg.C from room temperatureoC, at 150oC, pressing the ion implantation sample of the rutile titanium dioxide and the coating surface of the pure sample together, keeping the constant temperature for 5 minutes, and then continuously heating to 270 DEG CoC, the rate of temperature rise is 5oC/min, at 270oAnd C, keeping the temperature constant for 20-30 minutes, and then naturally cooling to room temperature to complete copper-tin bonding.
5. A rutile titanium dioxide single crystal thin film-substrate material heterostructure manufactured by the rutile titanium dioxide single crystal thin film-substrate material heterostructure manufacturing method according to any of claims 1 to 4, wherein the heterostructure is a heterostructure constituted by a submicron-thickness rutile titanium dioxide single crystal thin film (2) and a silica substrate layer (3), and further comprises first and second adhesive layers (41), (42) under the silica substrate layer (3), a copper-tin compound bonding layer (7) between the first and second adhesive layers (41), (42), and a rutile titanium dioxide single crystal bulk (8) under the second adhesive layer (41).
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CN105002471A (en) * | 2015-06-08 | 2015-10-28 | 山东大学 | Method for preparing KTiOPO4 single crystal thin film through ion implantation in combination with chemical etching |
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