CN104499047A - Substrate for realizing heteroepitaxial growth of large-size monocrystal diamond and preparation method thereof - Google Patents
Substrate for realizing heteroepitaxial growth of large-size monocrystal diamond and preparation method thereof Download PDFInfo
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- CN104499047A CN104499047A CN201410794743.0A CN201410794743A CN104499047A CN 104499047 A CN104499047 A CN 104499047A CN 201410794743 A CN201410794743 A CN 201410794743A CN 104499047 A CN104499047 A CN 104499047A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
Abstract
The invention discloses a substrate for realizing heteroepitaxial growth of large-size monocrystal diamond and a preparation method thereof. The substrate sequentially comprises a Si substrate, a TiN monocrystal seed layer, a metallic oxide single crystal film layer and an iridium single crystal film layer. A laminated layer capable of realizing heteroepitaxial growth of large-size monocrystal diamond is designed and prepared, the TiN monocrystal seed layer is inserted to serve as an epitaxial template and a transition buffer layer, and the crystal orientation consistency and growth quality of the oxide and the whole substrate epitaxial layer are improved, so that a possibility is provided for growing the high-quality large-size monocrystal diamond. Moreover, due to the use of the TiN buffer layer, the whole epitaxial laminated structure can be formed on the basis of the Si substrate, so that the epitaxial cost is greatly reduced, the diamond grows on the basis of the Si substrate, and the substrate can be well matched with the electronic information industry.
Description
Technical field
The invention belongs to film and field of crystal growth, relate to a kind of monocrystal material heteroepitaxial growth substrate and preparation method thereof, particularly relate to a kind of rete and preparation method of Epitaxial Growth of Diamond substrate.
Background technology
Present stage, large-sized single-crystal diamond or the consistent accurate single-crystal diamond of crystal orientation orientation height, have irreplaceable keying action in high-tech areas such as precision sizing, information communication, space flight aerospace, sophisticated technologies.But prepare diamond many employings high temperature and high pressure method (HPHT) at present, the diamond of preparation is impure more, and defect concentration is high, second-rate, and size is less, and prepared diamond composition is in the downstream of industrial chain, and competitive power is not high.
And Microwave Irradiation Assisted Chemical vapour deposition (MPCVD) method adopts the hydrocarbon reactant gases of microwave-excitation, electrodeless pollution, the single-crystal diamond quality of preparation is high, and by adopting larger-size foreign substrate can realize the adamantine growth of large size single crystal.MPCVD legal system is divided into again isoepitaxial growth and heteroepitaxial growth for single-crystal diamond.The adamantine size of isoepitaxial growth limit by seed crystal size, and growth time longer after, the generation of crystal boundary can be caused and the diamond layer making thickness larger forms polycrystalline state gradually.And the substrate dimension of heteroepitaxial growth is unrestricted, be prepare the adamantine gordian technique of large size single crystal.In numerous foreign substrate materials, on metal iridium, heteroepitaxial growth diamond has unique nucleating mechanism, and along with the increase of diamond film thickness, the crystal boundary between different crystal grain can close gradually, and diamond layer is more prone to be transformed into single crystal forms.Therefore, on metal iridium substrate, heteroepitaxial growth large size single crystal diamond more and more receives publicity.
Meet the large size single crystal diamond of processing requirement for reaching preparation, need a kind of special hetero epitaxy substrate, this substrate comprises some single crystal transition layer.Substrate material conventional in the world has Si, c-BN and SiC etc., but the adamantine size that goes out of epitaxy and quality are all difficult to reach requirement.The rhythmo structure of Si/ metal oxide/iridium (Ir), because metal iridium has very high Enhancing Nucleation Density and excellent monocrystalline feature, the diamond quality grown thereon is high, is considered to best diamond heteroepitaxial growth substrate.And the epitaxial quality of metal oxide film on Si still can not reach requirement, become and prepare the adamantine critical bottleneck of large size single crystal, need to be optimized design to the transition layer rhythmo structure on silicon substrate, with the diamond epitaxial substrate meeting required standard to performance the best guaranteed.
Summary of the invention
For the problem that the oxidate quality of deposition on Si has much room for improvement, for obtaining satisfactory epitaxial substrate and multilayer single crystal transition layer, the invention provides adamantine substrate of a kind of heteroepitaxial growth large size single crystal and preparation method thereof, this substrate has new transition layer rhythmo structure, the quality of each layer in substrate can be improved, thus mate with Si substrate, and obtain the better large size single crystal diamond of epitaxial quality.
The target that the present invention will reach is achieved through the following technical solutions:
The adamantine substrate of a kind of heteroepitaxial growth large size single crystal, is followed successively by Si substrate, TiN single crystal seed layer, monocrystalline metal oxide thin film layer, iridium (Ir) monocrystal thin films layer from bottom to top.
The preparation method of the adamantine substrate of above-mentioned heteroepitaxial growth large size single crystal, comprises the steps:
The cutting of step one, Si substrate and surface treatment:
The monocrystalline silicon piece of (100) orientation is cut into the wafer of the desired size such as 10mm × 10mm or 12mm × 7mm, successively at acetone, dehydrated alcohol, each 5 ~ 10min of deionized water for ultrasonic cleaning, dry up with blower.
To immerse volume ratio through prewashed Si sheet is H
2o
2(concentration 30%): H
2in the solution of O=1:15 ~ 1:25, place 8 ~ 10min at 60 ~ 65 DEG C and carry out preoxidation.Immerse again by NH
4oH solution (concentration 28%), H
2o
2in the SC-1 solution of solution and deionized water 1:2:5 ~ 1:1:10 preparation by volume, heating in water bath is to 60 ~ 65 DEG C, and soak time is 8 ~ 10min.After soaking 3 ~ 5min with deionized water, immerse by HCl solution (concentration 49%), H
2o
2in the SC-2 solution of solution and deionized water 1:2:5 ~ 1:1:6 preparation by volume, be heated to 60 ~ 65 DEG C, soak time is 8 ~ 10min, after soaking 3 ~ 5min with deionized water again, immerse the DHF solution by HF solution (concentration 49%) and deionized water 1:5 ~ 1:6 preparation by volume, ambient temperatare puts 10 ~ 15min, then carries out rear cleaning.Cleaned Si sheet is put into dehydrated alcohol preserve.
This RCA treatment process (increase preoxidation process) improved contributes to the situation of the Si sheet surfaceness rising that improvement causes due to basic solution, reduces Si sheet surfaceness, makes its surface more smooth, be conducive to the high-quality growth of epitaxial film.
The growth of step 2, TiN single crystal seed layer:
Utilize the substrate Epitaxial growth TiN single crystal seed layer of epitaxial growth technology after step one processes as buffer layer, epitaxial growth parameters is underlayer temperature T
sub=550 ~ 650 DEG C, growth thickness is 5 ~ 10nm.
TiN has and Si and strontium titanate (SrTiO
3) etc. the same face-centred cubic structure of metal oxide, although lattice parameter (0.1543nm) mismatch of the lattice parameter of TiN (0.1421nm) and Si (100) is up to 25%, but because TiN and Si has good farmland coupling, can be good at a TiN epitaxy on a si substrate.
In addition, TiN inculating crystal layer, owing to having reductibility, can reduce the SiO that Si substrate generates because of oxidation well
x , ensure that the quality of Si substrate.Especially TiN not only with Si not responsiveness, and its material such as lattice parameter and multiple perovskite oxide comparison match, can as sealing coat, bottom electrode or buffer layer, epitaxy oxide film material on a si substrate.
Using Si sheet as epitaxial substrate, use pulsed laser deposition (PLD) or the equipment such as molecular beam epitaxy (MBE), with high-purity Ti target (99.99%) and high pure nitrogen for raw material, reaction grows TiN inculating crystal layer; Or with high-purity Ti N target (99.95%) for raw material, select the parameters such as different target-substrate distances, underlayer temperature, deposition and annealing time, depositing TiN single crystal seed layer.
The growth of step 3, monocrystalline metal oxide thin film layer:
On TiN inculating crystal layer, utilize the equipment epitaxial metal oxide film layer such as pulsed laser deposition (PLD) or molecular beam epitaxy (MBE), adopt this area conventional epitaxial growth processing condition, the metal oxide that can select comprises MgO, YSZ, SrTiO
3deng, thicknesses of layers is 60 ~ 120nm.
The Main Function of metal oxide film regulates lattice parameter, makes the lattice match of whole epitaxial substrate consistent with diamond height, to reduce the stress of Epitaxial Growth of Diamond, improve its growth quality.Meanwhile, its existence effectively can also separate Si substrate and Ir layer, the phase mutual diffusion of both preventions, improves the quality of substrate.
The growth of step 4, iridium (Ir) monocrystal thin films layer:
At metal oxide film Epitaxial growth iridium (Ir) monocrystal thin films layer, the gauge control of rete is at 50 ~ 100nm.
Select the most top layer using iridium (Ir) as epitaxial substrate, diamond will directly grow on this layer.Because the diamond grown on Ir has unique forming core pattern, after growing into certain size, crystal boundary can close, by polycrystalline to single crystal transition, the diamond grown is made to have highly consistent orientation, for the adamantine growth of large size single crystal provides possibility.
Iridium monocrystal thin films can with high-purity iridium target for raw material, select the equipment such as pulsed laser deposition (PLD), molecular beam epitaxy (MBE) or rf magnetron sputtering, deposit under higher temperature conditions, and carry out in-situ annealing, promote that atom presses the arrangement of lattice template.
The present invention has the following advantages:
1, design and prepared one can the adamantine lamination of heteroepitaxial growth large size single crystal in the present invention, especially, insert TiN single crystal seed layer wherein as epitaxial template and transition buffer layer, improve orientation consistent degree and the growth quality in the crystal orientation of oxide compound and whole substrate epitaxial layer, thus provide possibility for growing high-quality large size single crystal diamond;
2, the present invention is owing to employing TiN buffer layer, and whole epitaxial stacked structure can carry out based on Si substrate, and extension cost is reduced widely, simultaneously based on Si substrate growth diamond, can match with electronic information industry better.
Accompanying drawing explanation
Fig. 1 is the structural representation of hetero epitaxy substrate, in figure: 1-Si substrate, 2-TiN layer, 3-metal oxide layer, 4-Ir layer;
Fig. 2 is the process flow sheet preparing substrate;
Fig. 3 is Si sheet three-dimensional surface shape figure after process;
Fig. 4 is the three-dimensional surface shape figure in embodiment one after the growth of TiN inculating crystal layer;
Fig. 5 is the three-dimensional surface shape figure in embodiment two after the growth of TiN inculating crystal layer;
Fig. 6 is substrate Si surface X-ray small-angle diffraction (SXRD) collection of illustrative plates;
Fig. 7 is TiN seed crystal surface X-ray small-angle diffraction (SXRD) collection of illustrative plates in embodiment one;
Fig. 8 is TiN seed crystal surface X-ray small-angle diffraction (SXRD) collection of illustrative plates in embodiment two.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment one: present embodiments provide for the adamantine substrate of a kind of heteroepitaxial growth large size single crystal, as shown in Figure 1, Si substrate, TiN single crystal seed layer, monocrystalline metal oxide film, iridium (Ir) monocrystal thin films is followed successively by from bottom to top.
As shown in Figure 2, its preparation method comprises the steps:
The cutting of step one, Si substrate and surface treatment:
Utilize glass cutter or silicon chip cutter that the monocrystalline silicon piece of (100) orientation is cut into the wafer being of a size of 12mm × 7mm.Clean each 10min in acetone, dehydrated alcohol, deionized water for ultrasonic successively, dry up with blower.
Carry out pre-oxidation treatment to Si substrate, specific implementation method is: will immerse H through prewashed Si sheet
2o
2: H
2in the solution of O=1:20, being positioned over temperature is in the water-bath of 65 DEG C, and heat-up time is 10min.Successively Si sheet is immersed in SC-1, SC-2 and DHF solution again and cleans, after clean each 10min in acetone, dehydrated alcohol, deionized water for ultrasonic successively, put into dehydrated alcohol and store.Si sheet after process is carried out to the measurement (in Fig. 3, RMS=4.855nm) of surfaceness, and utilize X-ray small-angle diffraction (SXRD) instrument to obtain processing rear Si sheet surface SXRD collection of illustrative plates (Fig. 6).
The growth of step 2, TiN single crystal seed layer:
In impulse laser deposition system (PLD), carry out the growth of inculating crystal layer, choose high-purity Ti target (99.99%) and high pure nitrogen is raw material, reaction growth TiN inculating crystal layer.By changing underlayer temperature, N
2the parameters such as pressure, laser intensity, target-substrate distance, depositing time, obtain 6 groups of samples (comprising the Si sheet after the surface treatment not depositing inculating crystal layer) of different group.Concrete preparation parameter is as shown in table 1.
Table 1 TiN inculating crystal layer growth parameter(s)
| Group | Underlayer temperature (DEG C) | N 2Pressure (Pa) | Laser intensity (mJ) | Target-substrate distance (mm) | Depositing time (min) |
| 0 | —— | —— | —— | —— | 0 |
| 1 | 600 | 5 | 62 | 45 | 10 |
| 2 | 600 | 10 | 62 | 45 | 10 |
| 3 | 600 | 10 | 70 | 45 | 10 |
| 4 | 650 | 5 | 62 | 45 | 10 |
| 5 | 650 | 10 | 62 | 45 | 10 |
The analysis and test of extension TiN inculating crystal layer, can be divided into the following steps to carry out (experimental result being the 5th group of sample provided in figure):
2.1, scanning electronic microscope or transmission electron microscope is utilized to characterize the surface topography of film;
2.2, atomic force microscope or high-precision three-dimensional profile meter is utilized to characterize surfaceness and the three-dimensional appearance (Fig. 4) of inculating crystal layer;
2.3, x-ray photoelectron power spectrum (XPS) is utilized to characterize composition and the constituent content of seed crystal surface;
2.4, X-ray small-angle diffraction (SXRD) collection of illustrative plates is utilized to characterize the epitaxy situation (Fig. 7) of inculating crystal layer;
2.5, X-ray rocking curve (ω-scan) and azimuth sweep (φ-scan) is utilized to characterize the epitaxial quality (orientation consistence) of extension inculating crystal layer.
The growth of step 3, oxide monocrystal film:
Metal oxide STO (SrTiO
3) adopt molecular beam epitaxy (MBE) to be prepared.Target adopts SrO and TiO
2, control O
2pressure 0.01Pa, underlayer temperature 800 DEG C, controls the rotation of target disc, two kinds of targets is attached in substrate successively, and reaction generates SrTiO
3, the period is about 30min, makes the STO layer thickness grown be about 60 ~ 120nm.
The growth of step 4, iridium (Ir) monocrystal thin films:
Molecular beam epitaxy (MBE) is utilized to carry out the growth preparation of substrate the superiors Ir layer.Target adopts high pure metal iridium, and controlling air pressure is 10
-7pa, underlayer temperature is 950 DEG C, and the period is about 30min, and the Ir layer thickness grown is controlled at 50 ~ 100nm.
Step 5, the lattice perfection degree detecting iridium (Ir) layer and crystal lattice orientation:
Utilize X-ray rocking curve (ω-scan) the lattice perfection degree to Ir to test, obtain rocking curve halfwidth.Utilize X-ray diffraction (XRD) collection of illustrative plates to characterize the crystal lattice orientation of Ir, observe Ir layer crystal lattice and be (100) direction, show that the Ir crystal lattice orientation height that epitaxy goes out is consistent.It is good that above two kinds of test synthesis indicate the Ir layer quality that epitaxy goes out, and reaches required standard.
Embodiment two: present embodiment and embodiment one unlike, in the process of preparation TiN single crystal seed layer, have employed TiN as target, specifically comprise the steps:
The cutting of step one, Si substrate and surface treatment:
Utilize glass cutter or silicon chip cutter that the monocrystalline silicon piece of (100) orientation is cut into the wafer being of a size of 12mm × 7mm.After carrying out pre-treatment, the surface treatment such as pre-oxidation treatment and surface cleaning is carried out to Si substrate, put into dehydrated alcohol and store.
The growth of step 2, TiN single crystal seed layer:
In impulse laser deposition system (PLD), carry out the growth of inculating crystal layer, choose high-purity Ti N target (99.95%) for raw material growth TiN inculating crystal layer.By changing the parameters such as underlayer temperature, laser intensity, target-substrate distance, depositing time, obtain 5 groups of samples of different group.Concrete preparation parameter is as shown in table 2.
Table 2 TiN inculating crystal layer growth parameter(s)
| Group | Underlayer temperature (DEG C) | Laser intensity (mJ) | Target-substrate distance (mm) | Depositing time (min) |
| 1 | 600 | 62 | 45 | 5 |
| 2 | 600 | 62 | 45 | 10 |
| 3 | 600 | 70 | 45 | 10 |
| 4 | 650 | 70 | 45 | 5 |
| 5 | 650 | 70 | 45 | 10 |
The analysis and test of extension TiN inculating crystal layer, can be divided into the following steps to carry out (experimental result being the 5th group of sample provided in figure):
2.1, scanning electronic microscope or transmission electron microscope is utilized to characterize the surface topography of film;
2.2, atomic force microscope or high-precision three-dimensional profile meter is utilized to characterize surfaceness and the three-dimensional appearance (Fig. 5) of inculating crystal layer;
2.3, x-ray photoelectron power spectrum (XPS) is utilized to characterize composition and the constituent content of seed crystal surface;
2.4, X-ray small-angle diffraction (SXRD) collection of illustrative plates is utilized to characterize the epitaxy situation (Fig. 8) of inculating crystal layer;
2.5, X-ray rocking curve (ω-scan) and azimuth sweep (φ-scan) is utilized to characterize the epitaxial quality (orientation consistence) of extension inculating crystal layer.
The growth of step 3, oxide monocrystal film:
Metal oxide STO (SrTiO
3) adopt molecular beam epitaxy (MBE) to be prepared.Target adopts SrO and TiO
2, control O
2pressure 0.01Pa, underlayer temperature 800 DEG C, controls the rotation of target disc, two kinds of targets is attached in substrate successively, and reaction generates SrTiO
3, the period is about 30min, makes the STO layer thickness grown be about 60 ~ 120nm.
The growth of step 4, iridium (Ir) monocrystal thin films:
Molecular beam epitaxy (MBE) is utilized to carry out the growth preparation of substrate the superiors Ir layer.Target adopts high pure metal iridium, and controlling air pressure is 10
-7pa, underlayer temperature is 950 DEG C, and the period is about 30min, and the Ir layer thickness grown is controlled at 50 ~ 100nm.
Step 5, the lattice perfection degree detecting iridium (Ir) layer and crystal lattice orientation:
Utilize X-ray rocking curve (ω-scan) the lattice perfection degree to Ir to test, obtain rocking curve halfwidth.Utilize X-ray diffraction (XRD) collection of illustrative plates to characterize the crystal lattice orientation of Ir, observe Ir layer crystal lattice and be (100) direction, show that the Ir crystal lattice orientation height that epitaxy goes out is consistent.It is good that above two kinds of test synthesis indicate the Ir layer quality that epitaxy goes out, and reaches required standard.
Embodiment three: present embodiment and embodiment two unlike, step 3: metal oxide selects MgO, adopts pulsed laser deposition (PLD) to be prepared.Target adopts MgO target, control O
2pressure 0.01Pa, underlayer temperature 600 ~ 650 DEG C, laser energy is 3J/cm
2, the period is about 50min, makes the MgO layer thickness grown be about 60 ~ 120nm.
Embodiment four: present embodiment and embodiment two are unlike, step 3: metal oxide selects YSZ(yttrium stable zirconium oxide), adopt pulsed laser deposition (PLD) to be prepared.Target adopts ZrO
2and Y
2o
3ceramic powder, with different mass ratio (ZrO
2and Y
2o
3ceramic powder mass ratio is respectively 100:8,100:11,100:15) after ball milling, fire at 1500 DEG C and form.During deposition, control O
2pressure 0.01Pa, underlayer temperature 700 ~ 750 DEG C, laser energy is 5J/cm
2, the period is about 50min, makes the YSZ layer thickness grown be about 60 ~ 120nm.
Claims (10)
1. the adamantine substrate of heteroepitaxial growth large size single crystal, is characterized in that described substrate is followed successively by Si substrate, TiN single crystal seed layer, monocrystalline metal oxide thin film layer, iridium monocrystal thin films layer from bottom to top.
2. the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 1, is characterized in that described Si substrate is the monocrystalline silicon piece of (100) orientation.
3. the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 1, is characterized in that the thickness of described TiN single crystal seed layer is 5 ~ 10nm.
4. the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 1, is characterized in that the thickness of described monocrystalline metal oxide thin film layer is 60 ~ 120nm.
5. the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 1, is characterized in that described metal oxide is MgO, YSZ or SrTiO
3.
6. the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 1, is characterized in that the thickness of described iridium monocrystal thin films layer is 50 ~ 100nm.
7. the preparation method of the adamantine substrate of heteroepitaxial growth large size single crystal according to the arbitrary claim of claim 1-6, is characterized in that described preparation method's step is as follows:
The cutting of step one, Si substrate and surface treatment:
The monocrystalline silicon piece of (100) orientation is cut into the wafer of desired size, successively at acetone, dehydrated alcohol, each 5 ~ 10min of deionized water for ultrasonic cleaning, dry up with blower; Pre-oxidation treatment will be carried out through prewashed Si sheet;
The growth of step 2, TiN single crystal seed layer:
Utilize the substrate Epitaxial growth TiN single crystal seed layer of epitaxial growth technology after step one processes as buffer layer;
The growth of step 3, monocrystalline metal oxide thin film layer:
At TiN inculating crystal layer Epitaxial growth metallic oxide film;
The growth of step 4, iridium monocrystal thin films layer:
At metal oxide film Epitaxial growth iridium monocrystal thin films layer.
8. the preparation method of the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 7, is characterized in that described pre-oxidation treatment step is as follows:
(1) will immerse volume ratio through prewashed Si sheet is H
2o
2: H
2in the solution of O=1:15 ~ 1:25, place 8 ~ 10min at 60 ~ 65 DEG C and carry out preoxidation;
(2) immerse again by NH
4oH solution, H
2o
2in the SC-1 solution of solution and deionized water 1:2:5 ~ 1:1:10 preparation by volume, heating in water bath is to 60 ~ 65 DEG C, and soak time is 8 ~ 10min;
(3), after soaking 3 ~ 5min with deionized water, immerse by HCl solution, H
2o
2in the SC-2 solution of solution and deionized water 1:2:5 ~ 1:1:6 preparation by volume, be heated to 60 ~ 65 DEG C, soak time is 8 ~ 10min;
(4), after soaking 3 ~ 5min with deionized water again, immerse the DHF solution by HF solution and deionized water 1:5 ~ 1:6 preparation by volume, ambient temperatare puts 10 ~ 15min, then carries out rear cleaning;
(5) cleaned Si sheet is put into dehydrated alcohol to preserve.
9. the preparation method of the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 7, it is characterized in that the concrete steps of described step 3 are as follows: using Si sheet as epitaxial substrate, with high-purity Ti target and high pure nitrogen for raw material, reaction growth TiN inculating crystal layer.
10. the preparation method of the adamantine substrate of heteroepitaxial growth large size single crystal according to claim 7, is characterized in that the concrete steps of described step 3 are as follows: using Si sheet as epitaxial substrate, with high-purity Ti N target for raw material, and depositing TiN single crystal seed layer.
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| CN107268076A (en) * | 2017-07-28 | 2017-10-20 | 西安交通大学 | A kind of method based on heteroepitaxial growth single-crystal diamond |
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| CN111088523A (en) * | 2020-01-07 | 2020-05-01 | 北京科技大学 | Method for heteroepitaxial growth of large-size single crystal diamond |
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