CN107268076A - A kind of method based on heteroepitaxial growth single-crystal diamond - Google Patents
A kind of method based on heteroepitaxial growth single-crystal diamond Download PDFInfo
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- CN107268076A CN107268076A CN201710633557.2A CN201710633557A CN107268076A CN 107268076 A CN107268076 A CN 107268076A CN 201710633557 A CN201710633557 A CN 201710633557A CN 107268076 A CN107268076 A CN 107268076A
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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
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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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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- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
It is to ride in the upper diamond layer of growth regulation one of the first iridium metals layer with the first iridium metals layer in the iridium metals of hetero-epitaxy Grown first layer the invention discloses a kind of method based on heteroepitaxial growth single-crystal diamond；The first diamond layer and the first iridium metals layer for ensureing growth are not influenceed by lattice mismatch, patterned second iridium metals layer is grown on the first diamond layer, the diamond layer of growth regulation two on patterned second iridium metals layer, second diamond layer contacts growth with the second iridium metals layer and the first diamond layer, now the second diamond layer is in free growth state, there is no the influence of lattice mismatch, obtain growing the hetero-epitaxy substrate for having two layers of diamond layer and two layers of iridium metals layer, second diamond layer is separated with the first diamond layer and the second iridium metals layer and can obtain single-crystal diamond, using hetero-epitaxy substrate as support, carry out the growth of single-crystal diamond, diamond device cost of manufacture can be reduced, be conducive to having given play to diamond excellent specific property.
Description
Technical field
The present invention relates to single-crystal diamond heterogeneous epitaxial technology, and in particular to one kind is based on heteroepitaxial growth single crystal diamond
The method of stone.
Background technology
Due to the electrical and optical property that single-crystal diamond is excellent, and it is micro- in device for high-power power electronic, high-frequency high-power
Have broad application prospects in terms of the semiconductor devices such as wave device.But traditional diamond uses the method next life of homoepitaxy
Long single-crystal diamond, this growth single-crystal diamond method is needed with diamond as epitaxial substrate, and diamond substrate price is held high
Expensive, size is limited, is unfavorable for the large-scale application of diamond device.Because the lattice between diamond and hetero-epitaxy substrate loses
With larger, heteroepitaxial growth is still very challenging.
The content of the invention
It is an object of the invention to provide a kind of method based on heteroepitaxial growth single-crystal diamond, to overcome existing skill
The deficiency of art.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of method based on heteroepitaxial growth single-crystal diamond, comprises the following steps：
Step 1), in the iridium metals of hetero-epitaxy Grown first layer；
Step 2), the first iridium metals layer on the diamond layer of growth regulation one；
Step 3), grow on the first diamond layer patterned second iridium metals layer；
Step 4), the second iridium metals layer on the diamond layer of growth regulation two, obtaining growth has two layers of diamond layer and two layers
The hetero-epitaxy substrate of iridium metals layer；
Step 5), the second diamond layer and the first diamond layer and the second iridium metals layer separated and can obtain single crystal diamond
Stone.
Further, step 1) in hetero-epitaxy substrate be Si, MgO, Al2O3Or SrTiO3。
Further, step 1) in, before the iridium metals of growth regulation one layer, first to hetero-epitaxy substrate hetero-epitaxy first
Substrate passes sequentially through acetone, alcohol, deionized water and is respectively cleaned by ultrasonic 5-10min, is then dried under an inert gas.
Further, it is characterised in that the first iridium metals layer pattern and the second iridium metals layer pattern are identical.
Further, step 2) and step 4) in microwave plasma chemical gas is coordinated using bias enhanced nucleation technology
Phase deposition technique grows diamond layer on iridium metals layer.
Further, step 3) in stand-by figure is made on diamond layer first with photoetching technique, then using magnetic control
Sputtering or electron beam evaporation method deposit iridium metals layer on substrate.
Further, step 5) in, the second diamond layer and the first diamond layer and the second iridium metals layer are passed through into machinery
Polishing, ICP etching methods or RIE etching methods remove the first diamond layer and the second iridium metals layer can obtain single crystal diamond
Stone.
Compared with prior art, the present invention has following beneficial technique effect：
A kind of method based on heteroepitaxial growth single-crystal diamond of the present invention, first in hetero-epitaxy Grown the
One iridium metals layer；Then it is to ride in the upper diamond layer of growth regulation one of the first iridium metals layer with the first iridium metals layer；Ensure growth
The first diamond layer and the first iridium metals layer do not influenceed by lattice mismatch, then grow on the first diamond layer patterned the
Two iridium metals layer, the diamond layer of growth regulation two, the second diamond layer and the second iridium metals on patterned second iridium metals layer
Layer and the first diamond layer contact growth, and now the second diamond layer is in free growth state, the influence without lattice mismatch,
Obtain growing the hetero-epitaxy substrate for having two layers of diamond layer and two layers of iridium metals layer；Finally by the second diamond layer and the first gold medal
Hard rock layer and the layer separation of the second iridium metals can obtain single-crystal diamond, using hetero-epitaxy substrate to rely on, carry out single crystal diamond
The growth of stone, can reduce diamond device cost of manufacture, be conducive to having given play to diamond excellent specific property.
Brief description of the drawings
Fig. 1 is structural representation of the embodiment of the present invention.
In figure, 1, hetero-epitaxy substrate；2nd, the first iridium metals layer；3rd, the first diamond layer；4th, the second iridium metals layer；5th,
Two diamond layers.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings：
A kind of method based on heteroepitaxial growth single-crystal diamond, comprises the following steps：
Step 1), the iridium metals of growth regulation one layer 2 on hetero-epitaxy substrate 1；
Step 2), the first iridium metals layer 2 on the diamond layer 3 of growth regulation one；
Step 3), grow on the first diamond layer 3 patterned second iridium metals layer 4；
Step 4), the second iridium metals layer 4 on the diamond layer 5 of growth regulation two, obtaining growth has two layers of diamond layer and iridium
The hetero-epitaxy substrate of metal level；
Step 5), the second diamond layer 5 and the first diamond layer 3 and the second iridium metals layer 4 separated and can obtain monocrystalline
Diamond.
Step 1) in hetero-epitaxy substrate be Si, MgO, Al2O3Or SrTiO3；
Step 1) before the iridium metals of growth regulation one layer 2, hetero-epitaxy substrate hetero-epitaxy substrate first is led to successively first
Cross acetone, alcohol, deionized water and be respectively cleaned by ultrasonic 5-10min, be then dried under an inert gas.
Step 2) in, coordinate MPCVD methods to grow gold on the first iridium metals layer using bias enhanced nucleation technology (BEN)
Hard rock layer, design parameter is as shown in table 1；
Table 1
Step 3) in, stand-by figure is made on the first diamond layer using photoetching technique, then using magnetron sputtering or electricity
Beamlet method of evaporating deposits the second iridium metals layer on substrate；
Step 2) and step 4) grown using bias enhanced nucleation technology (BEN) or MPCVD methods on iridium metals layer
One layer of diamond layer.
In step 2) in, diamond nucleating growth on iridium, the existing Heteroepitaxy in vertical direction has horizontal direction again
Free growth because being the influence that heteroepitaxial growth has lattice mismatch, the diamond grown in vertical direction has more
Defect and dislocation, based on this diamond layer, growing high quality diamond layer.
Step 5) in, the second diamond layer and the first diamond layer and the second iridium metals layer are passed through into mechanical milling method, ICP
Etching method or RIE etching methods separate except the first diamond layer and the second iridium metals layer can obtain single-crystal diamond.
Embodiment
As shown in Figure 1：
1, from hetero-epitaxy substrate of the MgO substrates as growth diamond,
2nd, it is cleaned by ultrasonic each 5min of MgO substrates successively with acetone, alcohol, deionized water, is then dried up with nitrogen；
3rd, bar shaped tpo substrate shape is gone out using photoetching making：MgO substrates are arranged on photoresist spinner, in MgO substrate surfaces drop
Enter photoresist, then by photoresist spinner uniform rotation be obtain it is uniform, do not have defective photoresist film；Photoresist is used for just
Property photoresist SUN-110P；Photoresist spinner rotating speed is that 2000 turns/min-3000 turns/min；The MgO substrates for obtaining photoresist film are entered
Row front baking：Sample is placed on 90-110 DEG C of warm table, 85-95s is toasted；By the solvent in front baking volatilization photoresist film,
Reduce pollution of the dust to photoresist film, simultaneously because the stress that photoresist film rotates at a high speed and produced, improves photoresist film
Adhesion between substrate；, will be selected on the MgO substrates after front baking and mask plate with microscope using URE2000 litho machines
Figure is aligned, the ultraviolet photoetching 175-185s for being then 360-370nm with wavelength, and sample is removed after terminating, it should be noted that
Short wavelength light source can not be contacted and to avoid re-expose；MgO substrates after exposure are placed in developer for positive photoresist no less than 55s,
30s is no less than with deionized water rinsing, developer residual is removed, then it is that can obtain after photoetching with figure to be dried up with nitrogen
Whether MgO substrates, the figure observed under the microscope after photoetching is complete；
4th, the first iridium metals layer is deposited using magnetron sputtering technique, the first iridium metals layer is striped stride distribution, adjacent two
Individual iridium metals layer strip shape body spacing is 5um, and single iridium metals layer strip shape body width is in Ar atmosphere in 5um, magnetron sputtering process
Lower progress is enclosed, power is 20-180W, and sputtering pressure is 1.1-1.3Pa, and sputter gas flow is 40sccm, iridium metals thickness degree
For 20nm；
5th, microwave plasma CVD (MPCVD) skill is coordinated using using bias enhanced nucleation technology (BEN)
Art, the first diamond layer on containing the first iridium metals layer, design parameter is as shown in table 1,
6th, repeat step 4 and step 5 on the first diamond layer, obtaining growing has two layers of diamond layer and iridium metals layer
MgO substrates,
7th, obtain growing the MgO substrates for having two layers of diamond layer and iridium metals layer, by the second diamond layer and the first Buddha's warrior attendant
Rock layers and the second iridium metals layer remove the first diamond layer and second by mechanical milling method, ICP etching methods or RIE etching methods
Iridium metals layer can obtain single-crystal diamond.
Claims (7)
1. a kind of method based on heteroepitaxial growth single-crystal diamond, it is characterised in that comprise the following steps：
Step 1), in the iridium metals of hetero-epitaxy Grown first layer；
Step 2), the first iridium metals layer on the diamond layer of growth regulation one；
Step 3), grow on the first diamond layer patterned second iridium metals layer；
Step 4), the second iridium metals layer on the diamond layer of growth regulation two, obtaining growth has two layers of diamond layer and two layers of iraurite
Belong to the hetero-epitaxy substrate of layer；
Step 5), the second diamond layer and the first diamond layer and the second iridium metals layer separated and can obtain single-crystal diamond.
2. a kind of method based on heteroepitaxial growth single-crystal diamond according to claim 1, it is characterised in that step
1) the hetero-epitaxy substrate in is Si, MgO, Al2O3Or SrTiO3。
3. a kind of method based on heteroepitaxial growth single-crystal diamond according to claim 1, it is characterised in that step
1) in, before the iridium metals of growth regulation one layer, acetone, wine are passed sequentially through to hetero-epitaxy substrate hetero-epitaxy substrate first first
Essence, deionized water are respectively cleaned by ultrasonic 5-10min, are then dried under an inert gas.
4. a kind of method based on heteroepitaxial growth single-crystal diamond according to claim 1, it is characterised in that it is special
Levy and be, the first iridium metals layer pattern and the second iridium metals layer pattern are identical.
5. a kind of method based on heteroepitaxial growth single-crystal diamond according to claim 1, it is characterised in that step
2) and step 4) in microwave plasma CVD technology is coordinated in iridium metals layer using bias enhanced nucleation technology
Upper growth diamond layer.
6. a kind of method based on heteroepitaxial growth single-crystal diamond according to claim 1, it is characterised in that step
3) make stand-by figure on diamond layer first with photoetching technique, then existed using magnetron sputtering or electron beam evaporation method
Iridium metals layer is deposited on substrate.
7. a kind of method based on heteroepitaxial growth single-crystal diamond according to claim 1, it is characterised in that step
5) in, by the second diamond layer and the first diamond layer and the second iridium metals layer by mechanical milling method, ICP etching methods or
RIE etching methods remove the first diamond layer and the second iridium metals layer can obtain single-crystal diamond.
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Cited By (9)
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|---|---|---|---|---|
| CN109234806A (en) * | 2018-11-21 | 2019-01-18 | 中国科学院大学 | A kind of method of the plasma-deposited single-crystal diamond of dual band radio frequency |
| CN109355702A (en) * | 2018-12-19 | 2019-02-19 | 长沙新材料产业研究院有限公司 | A method of for reducing CVD diamond synthesis impurity content |
| CN111051257A (en) * | 2017-09-08 | 2020-04-21 | J2原料公司 | Diamond and heteroepitaxial method of forming diamond |
| CN111321466A (en) * | 2020-03-25 | 2020-06-23 | 武汉大学 | Method for growing large-size single crystal diamond and composite substrate for growth |
| CN111936676A (en) * | 2018-03-28 | 2020-11-13 | 索泰克公司 | Method for manufacturing diamond or iridium material single crystal layer and substrate for epitaxially growing diamond or iridium material single crystal layer |
| CN112831834A (en) * | 2020-12-31 | 2021-05-25 | 西安交通大学 | Preparation method for heteroepitaxial growth of diamond (111) film on Ru (0001) film |
| CN113467095A (en) * | 2021-06-08 | 2021-10-01 | 西安交通大学 | Non-imaging laser homogeneous system and method for manufacturing homogeneous element |
| CN113529166A (en) * | 2021-07-02 | 2021-10-22 | 吉林大学 | Method for growing large-area diamond single crystal |
| CN114016128A (en) * | 2021-10-21 | 2022-02-08 | 西安交通大学 | Method for copying and growing heteroepitaxial monocrystal diamond |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111051257B (en) * | 2017-09-08 | 2022-12-09 | J2原料公司 | Diamond and heteroepitaxial method of forming diamond |
| CN111051257A (en) * | 2017-09-08 | 2020-04-21 | J2原料公司 | Diamond and heteroepitaxial method of forming diamond |
| US11198950B2 (en) | 2017-09-08 | 2021-12-14 | M7D Corporation | Diamonds and hetero-epitaxial methods of forming diamonds |
| US11905619B2 (en) | 2017-09-08 | 2024-02-20 | M7D Corporation | Diamonds and hetero-epitaxial methods of forming diamonds |
| CN111936676A (en) * | 2018-03-28 | 2020-11-13 | 索泰克公司 | Method for manufacturing diamond or iridium material single crystal layer and substrate for epitaxially growing diamond or iridium material single crystal layer |
| US11935743B2 (en) | 2018-03-28 | 2024-03-19 | Soitec | Method for manufacturing a monocrystalline layer of diamond or iridium material and substrate for epitaxially growing a monocrystalline layer of diamond or iridium material |
| CN109234806A (en) * | 2018-11-21 | 2019-01-18 | 中国科学院大学 | A kind of method of the plasma-deposited single-crystal diamond of dual band radio frequency |
| CN109355702A (en) * | 2018-12-19 | 2019-02-19 | 长沙新材料产业研究院有限公司 | A method of for reducing CVD diamond synthesis impurity content |
| CN111321466A (en) * | 2020-03-25 | 2020-06-23 | 武汉大学 | Method for growing large-size single crystal diamond and composite substrate for growth |
| CN112831834A (en) * | 2020-12-31 | 2021-05-25 | 西安交通大学 | Preparation method for heteroepitaxial growth of diamond (111) film on Ru (0001) film |
| CN113467095A (en) * | 2021-06-08 | 2021-10-01 | 西安交通大学 | Non-imaging laser homogeneous system and method for manufacturing homogeneous element |
| CN113467095B (en) * | 2021-06-08 | 2023-06-30 | 西安交通大学 | Non-imaging type laser homogenizing system and manufacturing method of homogenizing element |
| CN113529166A (en) * | 2021-07-02 | 2021-10-22 | 吉林大学 | Method for growing large-area diamond single crystal |
| CN114016128A (en) * | 2021-10-21 | 2022-02-08 | 西安交通大学 | Method for copying and growing heteroepitaxial monocrystal diamond |
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