CN113871303A - beta-Ga2O3Method for producing thin film and beta-Ga2O3Film(s) - Google Patents
beta-Ga2O3Method for producing thin film and beta-Ga2O3Film(s) Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 76
- 239000010408 film Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 40
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims abstract 35
- 238000006243 chemical reaction Methods 0.000 claims description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 229910052594 sapphire Inorganic materials 0.000 claims description 9
- 239000010980 sapphire Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 40
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
本发明公开了一种β‑Ga2O3薄膜的制备方法及β‑Ga2O3薄膜，该方法包括：选取具有一定偏角范围的偏角衬底；对所述偏角衬底进行退火处理；在所述偏角衬底上外延生长第一β‑Ga2O3层；采用脉冲式生长法在所述第一β‑Ga2O3层上外延生长第二β‑Ga2O3层，以得到β‑Ga2O3薄膜。本发明通过采用偏角衬底提高了外延薄膜平整度；同时配合脉冲式生长法极大地降低了薄膜表面的粗糙度，提升了β‑Ga2O3薄膜质量。
The invention discloses a preparation method of a β-Ga 2 O 3 film and a β-Ga 2 O 3 film. The method comprises: selecting an off-angle substrate with a certain off-angle range; annealing the off-angle substrate processing; epitaxially growing a first β-Ga 2 O 3 layer on the off-angle substrate; using a pulsed growth method to epitaxially grow a second β-Ga 2 O 3 on the first β-Ga 2 O 3 layer layer to obtain β-Ga 2 O 3 thin films. The invention improves the flatness of the epitaxial thin film by adopting the off-angle substrate; at the same time, the roughness of the thin film surface is greatly reduced and the quality of the β-Ga 2 O 3 thin film is improved by cooperating with the pulse growth method.
Description
Technical Field
The present invention belongs to the field of microelectronic technologyThe field, in particular to beta-Ga2O3Method for producing thin film and beta-Ga2O3A film.
Background
With the development of microelectronic technology and the wide application of high-breakdown and high-power devices, many challenges are encountered in the conventional narrow bandgap semiconductor materials such as silicon-based, in which the breakdown voltage is becoming one of the key factors for the performance of the device. As third generation semiconductor materials, beta-Ga2O3Has a band gap of about 5eV, and has a breakdown field strength of 2 times or more that of SiC or GaN. beta-Ga2O3The baligal figure of merit is also much greater than that of Si, SiC and GaN materials, and thus beta-Ga2O3The material has great potential in the application of high-power high-breakdown devices and solar blind detectors.
In recent years, beta-Ga has been centered around2O3The growth research of the thin film mainly relates to heterogeneous substrate epitaxy and homogeneous substrate epitaxy. Wherein the sapphire substrate is cheap and is compatible with beta-Ga2O3The thin film has high matching degree, so the thin film becomes the first choice for heteroepitaxy.
However, the existing beta-Ga2O3Heteroepitaxial films of thin films have a high number of defects and generally high surface roughness, resulting in beta-Ga2O3Thin films cannot be applied to electronic devices. However, homoepitaxy is affected by more experimental growth parameters, so that the exploration difficulty of the optimal growth conditions is high, and the flatness of the film is affected.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a beta-Ga compound2O3Method for producing thin film and beta-Ga2O3A film. The technical problem to be solved by the invention is realized by the following technical scheme:
beta-Ga2O3A method of making a film comprising:
selecting a deflection angle substrate with a certain deflection angle range;
annealing the deflection angle substrate;
epitaxially growing a first beta-Ga on the off-angle substrate2O3A layer;
applying pulsed growth method to the first beta-Ga2O3Epitaxially growing a second beta-Ga layer on the substrate2O3Layer to obtain beta-Ga2O3A film.
In one embodiment of the present invention, the material of the off-angle substrate is Ga2O3Or sapphire.
In one embodiment of the invention, the off-angle substrate has an off-angle in a range of 1.5-6 °.
In one embodiment of the present invention, annealing the off-angle substrate comprises:
placing the deflection substrate into a low-pressure MOCVD reaction chamber, setting the oxygen flow at 1000-1500sccm, the temperature at 900-950 ℃ and the pressure in the reaction chamber at 35-45 Torr;
and thermally annealing the off-angle substrate in the oxygen atmosphere for 20-30 min.
In one embodiment of the invention, a first β -Ga is epitaxially grown on the off-angle substrate2O3The layers include:
in p-beta-Ga2O3After the substrate is annealed, the temperature of the reaction chamber is reduced to 700-850 ℃, and the pressure in the reaction chamber is kept at 35-45 Torr;
simultaneously opening Ga source and O2Gas path, and Ga source flow is adjusted to 35-40sccm, O2The flow rate is 1800-;
epitaxially growing beta-Ga on the off-angle substrate under the process conditions2O3Film to form a first beta-Ga2O3A layer; wherein the growth time is 50-60 min.
In one embodiment of the present invention, the first β -Ga2O3The thickness of the layer was 500-600 nm.
In one embodiment of the invention, the first beta-Ga is pulsed with2O3Epitaxially growing a second beta-Ga layer on the substrate2O3A layer, comprising:
keeping other growth parameters unchanged, switching the film growth mode to be a pulse method, and adjusting Ga source and O2The pulse time ratio of (1: 1) to (1: 3);
growing for 30-50 cycles under the above conditions to grow in the first beta-Ga2O3Forming a second beta-Ga layer on the first beta-Ga layer2O3And (3) a layer.
In one embodiment of the present invention, the pulse time of the Ga source is 0.1min, and the O is2The pulse time of (3) is 0.2 or 0.3 min.
In one embodiment of the present invention, the second β -Ga2O3The thickness of the layer is 20-30 nm.
Another embodiment of the present invention also provides a beta-Ga compound2O3The film includes from bottom to top in proper order: off-angle substrate, first beta-Ga2O3Layer and second beta-Ga2O3Layer, wherein the second beta-Ga2O3The layer is prepared by a pulse growth method, and the beta-Ga2O3The films were prepared as described in the examples above.
The invention has the beneficial effects that:
the invention leads the subsequent epitaxial growth of the beta-Ga by adopting the deflection angle substrate2O3When the film is formed, the combination of the reaction atoms and the substrate sites can grow according to a two-dimensional step flow mode, so that the flatness of the epitaxial film is improved; meanwhile, a pulse type growth method is adopted at the final stage of epitaxial growth, each path of reaction source is staggered, the pulse time of each path of reaction source is adjusted, the transverse migration length of atoms on the surface is increased, the two-dimensional growth mode is further enhanced, the roughness of the surface of the film is greatly reduced, and the beta-Ga content is improved2O3Film quality.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 shows a beta-Ga compound provided by an embodiment of the present invention2O3A schematic diagram of a preparation method of the film;
FIGS. 2a-2b are timing diagrams of two growth modes of the pulse method provided by embodiments of the present invention;
FIGS. 3a-3c show a beta-Ga compound according to an embodiment of the present invention2O3The growth process of the film is shown schematically;
FIG. 4 shows a beta-Ga compound provided by an embodiment of the present invention2O3The film structure is shown schematically.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example one
Referring to fig. 1, fig. 1 shows a beta-Ga according to an embodiment of the present invention2O3The preparation method of the film is schematically shown and comprises the following steps:
s1: selecting a deflection angle substrate with a certain deflection angle range.
In this embodiment, the off-angle substrate may be β -Ga2O3The homogeneous substrate may be a heterogeneous substrate. Preferably, the material of the foreign substrate is sapphire (sapphire).
In general, a sapphire substrate with a zero off-angle can be divided into a-plane (11-20), c-plane (0001), m-plane (1-100) and r-plane (1102) substrates, and the off-angle substrate means that the substrate is not cut parallel to the corresponding crystal plane during the cutting process, but has a small angle deviation with the plane, and the inclined direction of the small angle is towards the other plane of the sapphire substrate. For example, the c-a sapphire off-angle substrate is cut at an angle of a sapphire c-plane inclined to an a-plane, and in addition, the c-m off-angle substrate and the c-r off-angle substrate are provided.
Off-angle substrates are commonly used to improve the crystallinity of epitaxial films because they are generally believed to enhance the step flow growth and control domain structure of the films. Atomic steps on the off-angle substrate surface act as preferential binding sites for the incoming adatoms, promoting step flow growth.
Further, the off-angle substrate selected for this embodiment has an off-angle in the range of 1.5 to 6 °.
After the substrate is identified, it needs to be cleaned for subsequent operations. Specifically, the cleaning process is as follows:
firstly, the selected substrate is put into a 20 percent HF acid solution to be soaked for 60s, and then H is used for sequentially2O2Alcohol and acetone washes and finally a rinse with running deionized water for 60 s.
S2: and annealing the deflection angle substrate.
Specifically, the cleaned off-angle substrate is placed into a low-pressure MOCVD reaction chamber, the oxygen flow is set to be 1000-1500sccm, the temperature is set to be 900-950 ℃, and the pressure of the reaction chamber is set to be 35-45 Torr.
And then, carrying out thermal annealing on the off-angle substrate in the oxygen atmosphere for 20-30min to expose the substrate atomic steps.
In this embodiment, by annealing the off-angle substrate, the atomic steps of the substrate can be exposed, so that in the subsequent epitaxial growth stage, the reactive atoms and the sites of the substrate are bonded and grow according to the step flow mode. And the step flow growth mode belongs to a two-dimensional growth mode, thereby being beneficial to improving the flatness of the epitaxial film.
S3: epitaxially growing a first beta-Ga on an off-angle substrate2O3And (3) a layer.
Preferably, this example uses MOCVD process to prepare beta-Ga2O3A film.
In particular, in p-beta-Ga2O3After the substrate is annealed, the temperature of the reaction chamber is reduced to 700 DEG and 850 ℃, and the pressure in the reaction chamber is kept at 35-45 Torr.
Then, Ga source and O are turned on simultaneously2Gas path, and Ga source flow is adjusted to 35-40sccm, O2The flow rate is 1800 and 2100 sccm.
Epitaxially growing beta-Ga on the off-angle substrate under the above process conditions2O3Film to form a first beta-Ga2O3A layer; wherein the growth time is 50-60 min.
It should be noted that the organic sources widely used for the Ga source at present mainly include both TEGa and TMGaWhereas TMGa needs to be stabilized in a bath at near-zero temperature to maintain a suitable vapor pressure, TEGa needs only to be maintained in a bath at near-room temperature, and TEGa has a slower reaction rate than TMGa, which is extremely effective in reducing the organic source and O2The pre-reaction reaching the surface of the substrate is beneficial to the migration of atoms on the surface of the substrate, and the generation of byproducts is reduced. Therefore, this embodiment prefers TEGa as the Ga source for growing beta-Ga2O3A film.
The first beta-Ga with the thickness of 500-600nm can be formed on the off-angle substrate by the method2O3And (3) a layer.
S4: pulse growth method is adopted to grow in the first beta-Ga2O3Epitaxially growing a second beta-Ga layer on the substrate2O3Layer to obtain beta-Ga2O3A film.
In this example, to further promote the incorporation of the thin film surface, the first β -Ga is grown2O3After the layer is formed, the film growth mode is switched to a pulse growth method, and the beta-Ga is continuously grown2O3Thereby obtaining beta-Ga with better quality2O3A film.
Specifically, the first β -Ga is formed at step S32O3After the layer is formed, other growth parameters are kept unchanged, the film growth mode is switched into a pulse method, and a Ga source and O are adjusted2The pulse time ratio of (a) to (b) is 1:1 to 1: 3.
More specifically, referring to fig. 2a-2b, fig. 2a-2b are timing diagrams of two growth modes of the pulse method provided by the embodiment of the present invention, wherein the pulse time of the Ga source shown in fig. 2a is 0.1min, O2Pulse time of (1) is 0.2min, i.e. Ga source and O2The pulse time ratio of (1: 2); the pulse time of the Ga source shown in FIG. 2b is 0.1min, O2Pulse time of (1) is 0.3min, i.e. Ga source and O2The pulse time ratio of (a) to (b) is 1: 3.
Growing under the above conditions for 30-50 cycles to grow on the first beta-Ga2O3Forming a second beta-Ga layer on the first beta-Ga layer2O3And (3) a layer. Wherein the second beta-Ga is formed2O3The thickness of the layer is 20-30nm。
The invention leads the subsequent epitaxial growth of the beta-Ga by adopting the deflection angle substrate2O3When the film is formed, the combination of the reaction atoms and the substrate sites can grow according to a two-dimensional step flow mode, so that the flatness of the epitaxial film is improved; meanwhile, a pulse type growth method is adopted at the final stage of epitaxial growth, each path of reaction source is staggered, the pulse time of each path of reaction source is adjusted, the transverse migration length of atoms on the surface is increased, the two-dimensional growth mode is further enhanced, the roughness of the surface of the film is greatly reduced, and the beta-Ga content is improved2O3Film quality.
Example two
The following is a detailed example of beta-Ga provided by the present invention2O3The method of producing the film will be described in detail.
Referring to FIGS. 3a-3c, FIGS. 3a-3c illustrate a beta-Ga compound according to an embodiment of the present invention2O3The growth process schematic diagram of the thin film comprises the following steps:
step 1: selecting beta-Ga with deflection angle of 3 degrees2O3The material acts as a substrate as shown in figure 3 a.
Step 2: reacting beta-Ga2O3Soaking the substrate in 20% HF acid solution for 60s, and soaking with H2O2Alcohol and acetone washes and finally a rinse with running deionized water for 60 s.
And step 3: and putting the cleaned substrate into a low-pressure MOCVD reaction chamber, setting the oxygen flow at 1500sccm, the temperature at 900 ℃ and the pressure in the reaction chamber at 40Torr, and thermally annealing the substrate in the oxygen atmosphere for 30min to expose the atomic steps of the substrate.
And 4, step 4: after the thermal annealing was completed, the temperature of the reaction chamber was lowered to 800 ℃ and the growth pressure was continuously maintained at 40 Torr.
And 5: simultaneous opening of TEGa and O2Gas path, adjusting TEGa flow to 40sccm, oxygen flow to 2000sccm, growing beta-Ga for 60min2O3Thin film epitaxial layer to form a first beta-Ga2O3Layer as shown in fig. 3 b.
Step 6: keeping other growth parameters unchanged, switching the film growth mode to a pulse method, adjusting TEGa pulse time to 0.1min, oxygen pulse time to 0.2min, and growing beta-Ga with 30-50 cycle periods2O3Layer to form a second beta-Ga2O3Layer as shown in fig. 3 b.
To this end, β -Ga is completed2O3And (3) preparing a film.
EXAMPLE III
On the basis of the first embodiment, the present embodiment provides a beta-Ga2O3The film includes from bottom to top in proper order: off-angle substrate, first beta-Ga2O3Layer and second beta-Ga2O3Layers as shown in fig. 4. Wherein the second beta-Ga2O3The layer is prepared by a pulsed growth method.
This example provides beta-Ga2O3The film adopts the off-angle substrate to lead the subsequent epitaxial growth of the beta-Ga2O3The film has better flatness; meanwhile, the pulse type growth method is adopted in the final stage of epitaxial growth, so that the roughness of the surface of the film is greatly reduced, and the beta-Ga content is improved2O3Film quality.
This example provides beta-Ga2O3The thin film prepared by the method provided by the first embodiment can be widely applied to electronic devices due to the good surface flatness.
It should be noted that while examples of parameters including particular values may be provided herein, it should be appreciated that the parameters need not be exactly equal to the corresponding values, but rather approximate the corresponding values within acceptable error tolerances or design constraints.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
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| CN114525585A (en) * | 2022-01-05 | 2022-05-24 | 西安电子科技大学 | Epitaxy of beta-Ga on diamond using pre-laid Ga layer2O3Preparation method and structure of film |
| CN115029778A (en) * | 2022-06-02 | 2022-09-09 | 西安电子科技大学 | Growth method of gallium oxide epitaxial film |
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