CN111933514B - Method for preparing Ir (111) composite substrate for epitaxial single crystal diamond by electron beam evaporation process - Google Patents
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Abstract
The invention discloses a method for preparing an Ir (111) composite substrate for epitaxial monocrystal diamond by an electron beam evaporation process, and aims to solve the problem that alpha-Al is difficult to perform in the prior art 2 O 3 The technical problem of obtaining the (111) crystal face Ir epitaxial layer is that the preparation method comprises the following steps: 1. for alpha-Al 2 O 3 (0001) Carrying out ultrasonic cleaning; 2. alpha-Al is added 2 O 3 (0001) Fixing the Ir particle target in a sample holder, and placing the Ir particle target in a graphite crucible; 3. vacuumizing the cavity; 4. heating the sample to a certain temperature; 5. opening the high pressure of an electron gun and a target baffle, and depositing an Ir epitaxial layer on the surface of the sample; 6. closing the target baffle and the high pressure of the electron gun after the deposition is finished; 7. and (5) annealing treatment. The invention adopts the method for preparing (111) surface Ir epitaxial layer by electron beam evaporation method, the prepared Ir epitaxial layer and alpha-Al 2 O 3 The difference of the thermal expansion coefficients is smaller, the crystallization quality is better, and the binding force is stronger.
Description
Technical Field
The invention belongs to the field of preparation of heteroepitaxial single crystal diamond, and particularly relates to a method for preparing heteroepitaxial single crystal diamond by adopting an electron beam evaporation processWith Ir (111)/alpha-Al 2 O 3 (0001) A method of compounding a substrate.
Background
Compared with polycrystalline diamond, the single crystal diamond integrates excellent characteristics such as electricity, optics, mechanics, acoustics and thermology, has extremely important application prospect in the aspects of high-temperature, high-efficiency and ultra-high-power millimeter wave electronic devices, power electronic devices, biosensors, photoelectric detection and imaging, particle detection and imaging, aerospace and other systems, and is known as an ultimate semiconductor in the industry. At present, two key scientific and technical problems, namely high-quality growth of large-size single-crystal diamond and N-type effective doping of the single-crystal diamond, need to be solved to widely apply the single-crystal diamond.
The crystal face of diamond (001) is a dense arrangement face, so that the diamond is most suitable for producing high-quality epitaxial diamond films, the defect density is low, the growth quality is excellent, and heteroepitaxial single crystal diamond is obtained at present. (111) The crystal face is the most suitable crystal face for N-type and P-type doping, has NV color centers distributed in a preferred orientation, can form a heterojunction with a wurtzite structure semiconductor, but has high growth quality defect density and is easy to form twin crystals. How to realize effective doping of N-type while growing high quality single crystal diamond has become a hot research point in this field. Researchers have obtained high quality diamond without twins on Ir (111) substrates, and therefore performing diamond heteroepitaxial growth on (111) plane single crystal foreign substrates is an effective method for solving this problem, and the production of Ir (111) single crystal foreign substrates is the basis of the above work.
Disclosure of Invention
The invention aims to provide a method for preparing an Ir (111) composite substrate for heteroepitaxial single crystal diamond by an electron beam evaporation process in order to solve the technical problem that a (111) oriented Ir epitaxial layer is difficult to obtain on sapphire in the prior art.
The invention relates to Ir (111)/alpha-Al for preparing epitaxial monocrystal diamond by electron beam evaporation process 2 O 3 (0001) The method for compounding the substrate is realized according to the following steps:
1. alpha-Al is added 2 O 3 (0001) The substrate is sequentially subjected to ultrasonic cleaning in deionized water, absolute ethyl alcohol and acetone to obtain cleaned alpha-Al 2 O 3 (0001) A single crystal substrate;
2. the cleaned alpha-Al is added 2 O 3 (0001) The substrate is fixed in a groove of a sample holder, and then is placed in a cavity of electron beam evaporation equipment with a heating device (a rotary substrate heating table), and the Ir particle target material is placed in a graphite crucible;
3. sequentially starting the mechanical pump and the molecular pump of the electron beam evaporation equipment to ensure that the vacuum degree of the cavity is 8.0 multiplied by 10 -5 ～6.0×10 -4 Pa, starting a heating device, and starting temperature rise of the sample holder;
4. heating to ensure that the alpha-Al in the sample holder 2 O 3 (0001) The substrate temperature reaches 400-1000 ℃, the stable temperature is 5-10 min, then the power supply of the electron gun is turned on, the filament current of the electron gun is controlled to be 0.4-1.0A, and the alpha-Al with uniform surface temperature is obtained 2 O 3 (0001) A substrate;
5. opening the high pressure of the electron gun and the target material baffle, adjusting the beam current to 0.180-0.300A, controlling the evaporation rate, and obtaining the alpha-Al with uniform surface temperature 2 O 3 (0001) Depositing Ir epitaxial layer on the surface of the substrate to obtain alpha-Al with Ir epitaxial layer 2 O 3 (0001) A composite substrate;
6. after deposition is finished, reducing the beam current to 0, closing a target baffle and an electron gun system, closing a heating device of a sample holder, naturally cooling to room temperature, closing a molecular pump and a mechanical pump, inflating to atmospheric pressure, and taking out the composite substrate;
7. placing the cooled composite substrate in an infrared annealing furnace, controlling the annealing temperature to be 400-1000 ℃, and introducing N 2 As the protective gas, the gas flow rate is 20-40 sccm, the annealing time is controlled to be 0.5-2 h for annealing, and Ir (111)/alpha-Al is obtained after the annealing is finished 2 O 3 (0001) A composite substrate.
Compared with the traditional resistance heating type vacuum annealing process, the invention combines the infrared rapid annealing with the N 2 Atmosphere protection, adopting infrared heat radiation technology to make the heating rate higherThe annealing efficiency is improved, the thermal stress between the Ir epitaxial layer and the substrate is effectively relieved, most of strain energy is released, the film-substrate binding force between the Ir epitaxial layer and the substrate is enhanced, the abnormal growth behavior of Ir crystal grains in a high-temperature plasma environment is inhibited, and the diamond film is well prevented from falling off and cracking when the composite substrate is used in the epitaxial diamond growth process and the growth end cooling process; in addition, the annealing process has good effects of improving the crystallization quality of the Ir epitaxial layer, facilitating the crystallization of the (111) crystal face and reducing the mosaic degree of the Ir epitaxial layer. Compared with other crystal planes such as Ir (100) crystal plane and the like, ir (111) crystal plane is matched with alpha-Al under the temperature condition in the electron beam deposition process 2 O 3 (0001) The difference in surface energy of the facets is smaller and therefore epitaxial growth is easier to achieve under the "template" action of the substrate.
The invention relates to Ir (111)/alpha-Al for preparing epitaxial monocrystal diamond by adopting an electron beam evaporation process 2 O 3 (0001) The method for compounding the substrate mainly comprises the following beneficial effects:
1. based on alpha-Al 2 O 3 (0001) A method for preparing Ir (111) epitaxial layer by electron beam evaporation method is provided;
2. compared with the common epitaxial growth on other oxide substrates, the Ir epitaxial layer and the alpha-Al prepared by the method 2 O 3 The difference of thermal expansion coefficients is smaller, the thermal stress is smaller, and the binding force is stronger;
3. compared with the Ir layer prepared by a magnetron sputtering process or a molecular beam epitaxy process, the composite substrate prepared by combining the infrared rapid annealing process has the advantages of better crystallization quality, stronger binding force, simpler method and lower cost.
Drawings
FIG. 1 is an XRD phase structure diagram (out-of-plane orientation relationship) of Ir epitaxial layers prepared in examples.
Detailed Description
The first embodiment is as follows: the electron beam evaporation process of the embodiment prepares Ir (111)/alpha for epitaxial single crystal diamond-Al 2 O 3 (0001) The method of compounding the substrate is carried out according to the following steps:
1. alpha-Al is added 2 O 3 (0001) The substrate is sequentially subjected to ultrasonic cleaning in deionized water, absolute ethyl alcohol and acetone to obtain cleaned alpha-Al 2 O 3 (0001) A single crystal substrate;
2. the cleaned alpha-Al is added 2 O 3 (0001) The substrate is fixed in a groove of a sample holder, then the sample holder is placed in a cavity of electron beam evaporation equipment with a heating function, and an Ir particle target material is placed in a graphite crucible;
3. starting the mechanical pump and molecular pump of the electron beam evaporation equipment in sequence to make the vacuum degree of the cavity be 8.0 x 10 -5 ～6.0×10 -4 Pa, starting a heating device in the sample holder, and starting temperature rise of the sample holder;
4. heating to ensure that the alpha-Al in the sample holder 2 O 3 (0001) The substrate temperature reaches 400-1000 ℃, the stable temperature is 5-10 min, then the power supply of the electron gun is turned on, the filament current of the electron gun is controlled to be 0.4-1.0A, and the alpha-Al with uniform surface temperature is obtained 2 O 3 (0001) A substrate;
5. opening the high pressure of the electron gun and the target baffle, adjusting the beam current to 0.180-0.300A, controlling the evaporation rate, and obtaining the alpha-Al with uniform surface temperature 2 O 3 (0001) Depositing Ir epitaxial layer on the surface of the substrate to obtain alpha-Al with Ir epitaxial layer 2 O 3 (0001) A composite substrate;
6. after the deposition is finished, reducing the beam current to 0, closing the target baffle and the electron gun system, closing the heating device of the sample holder, naturally cooling to room temperature, closing the molecular pump and the mechanical pump, inflating to atmospheric pressure, and taking out the composite substrate;
7. placing the cooled composite substrate in an infrared annealing furnace, controlling the annealing temperature to be 400-1000 ℃, and introducing N 2 As the protective gas, the gas flow rate is 20-40 sccm, the annealing time is controlled to be 0.5-2 h for annealing, and Ir (111)/alpha-Al is obtained after the annealing is finished 2 O 3 (0001) A composite substrate.
Compared with oxides such as strontium titanate, magnesium oxide and YSZ, the sapphire is more stable in an H plasma environment, has a smaller thermal expansion coefficient, and has the advantage of depositing an Ir metal epitaxial layer.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the ultrasonic cleaning in deionized water, absolute ethyl alcohol and acetone in the first step is carried out for 10-30 min.
The third concrete implementation mode: this embodiment differs from the first or second embodiment in that the purity of the Ir particles in step two is greater than 99.99%.
The fourth concrete implementation mode is as follows: in a third step different from the first to third steps, the vacuum degree of the chamber is 3.0 × 10 -4 ～6.0×10 -4 Pa。
The fifth concrete implementation mode: in a fourth step different from the first to fourth step, the temperature is raised to make the alpha-Al in the sample holder 2 O 3 (0001) The substrate temperature reaches 600 ℃, and the temperature is stabilized for 5-10 min.
The sixth specific implementation mode is as follows: the difference between this embodiment and the first to the fifth embodiment is that the high voltage of the electron gun is controlled to be 8kV in the fifth step.
The seventh embodiment: the difference between the present embodiment and one of the first to fifth embodiments is that the deposition rate of the Ir epitaxial layer in the fifth step is controlled to be 0.04-0.10 nm/s.
The specific implementation mode eight: the difference between this embodiment mode and one of the first to seventh embodiment modes is that the thickness of the deposited Ir epitaxial layer in the fifth step is 120-200 nm.
The specific implementation method nine: the present embodiment is different from the first to eighth embodiments in that the temperature is raised to the annealing temperature at a temperature raising rate of 20 ℃/s to 35 ℃/s in the seventh step.
The detailed implementation mode is ten: the difference between the present embodiment and one of the first to ninth embodiments is that the cooling rate is controlled to be 2 ℃/s to 30 ℃/s after the annealing in the seventh step.
Example (b): this example is an electron beam evaporation process for preparing Ir (111)/α -Al for epitaxial single crystal diamond 2 O 3 (0001) Of composite substratesThe method is implemented according to the following steps:
1. polishing one side of the alpha-Al with the thickness of 0.5mm 2 O 3 (0001) The substrate is sequentially subjected to ultrasonic cleaning in deionized water, absolute ethyl alcohol and acetone for 15min to obtain cleaned alpha-Al 2 O 3 (0001) A single crystal substrate;
2. the cleaned alpha-Al is added 2 O 3 (0001) The substrate is fixed in a groove of a sample holder and then is placed in a cavity of electron beam evaporation equipment with a heating device, the heating device is a rotary substrate heating table, the heating device is positioned above the sample holder, and an Ir particle target material with the purity of 99.99 percent is placed in a graphite crucible;
3. sequentially starting the mechanical pump and the molecular pump of the electron beam evaporation equipment to ensure that the vacuum degree of the cavity is 4.0 multiplied by 10 -4 Pa, starting a heating device above the sample holder, and starting temperature rise of the sample holder;
4. raising the temperature to ensure that the alpha-Al in the sample holder 2 O 3 (0001) The substrate temperature reaches 600 ℃, the temperature is stabilized for 7min, then the power supply of the electron gun is turned on, the filament current of the electron gun is controlled to be 0.5A, and the alpha-Al with uniform surface temperature is obtained 2 O 3 (0001) A substrate;
5. opening the high voltage of the electron gun and the target material baffle, controlling the high voltage to be 8kV, controlling the beam current to be 0.19A, controlling the Ir deposition rate to be 0.04nm/s, and controlling the surface temperature to be uniform alpha-Al 2 O 3 (0001) Depositing an Ir epitaxial layer on the surface to obtain alpha-Al with the Ir epitaxial layer with the thickness of 160nm 2 O 3 (0001) A composite substrate;
6. after the deposition is finished, reducing the beam current to 0, closing the target baffle and the electron gun system, closing the heating device of the sample holder, naturally cooling to room temperature, closing the molecular pump and the mechanical pump, inflating to atmospheric pressure, and taking out the composite substrate;
7. placing the cooled composite substrate in an infrared annealing furnace, controlling the heating rate to be 30 ℃/s, controlling the annealing temperature to be 600 ℃, and introducing N 2 As the protective gas, the gas flow rate is 30sccm, the annealing time is controlled to be 1h, and Ir (111)/alpha-Al is obtained after the annealing is finished 2 O 3 (0001) A composite substrate.
alpha-Al as described in step one of this example 2 O 3 (0001) Commercially available from Shanghai Doubu optical materials, inc.
Ir (111)/α -Al prepared in this example 2 O 3 (0001) XRD phase analysis of the composite substrate gave out-of-plane orientation relationship, and as a result, as shown in FIG. 1, it was confirmed that there were Ir (111) and (222) peaks, and it was confirmed that this example achieved α -Al 2 O 3 (0001) Is grown epitaxially.
Claims (10)
1. The method for preparing the Ir (111) composite substrate for the epitaxial monocrystal diamond by the electron beam evaporation process is characterized by comprising the following steps of:
1. alpha-Al is added 2 O 3 (0001) The substrate is sequentially subjected to ultrasonic cleaning in deionized water, absolute ethyl alcohol and acetone to obtain cleaned alpha-Al 2 O 3 (0001) A single crystal substrate;
2. the cleaned alpha-Al is added 2 O 3 (0001) The substrate is fixed in a groove of a sample holder, then the sample holder is placed in a cavity of electron beam evaporation equipment with a heating device, and the Ir particle target material is placed in a graphite crucible;
3. starting the mechanical pump and molecular pump of the electron beam evaporation equipment in sequence to make the vacuum degree of the cavity be 8.0 x 10 -5 ～6.0×10 -4 Pa, starting a heating device, and starting temperature rise of the sample holder;
4. heating to ensure that the alpha-Al in the sample holder 2 O 3 (0001) The substrate temperature reaches 400-1000 ℃, the stable temperature is 5-10 min, then the power supply of the electron gun is turned on, the filament current of the electron gun is controlled to be 0.4-1.0A, and the alpha-Al with uniform surface temperature is obtained 2 O 3 (0001) A substrate;
5. opening the high pressure of the electron gun and the target baffle, adjusting the beam current to 0.180-0.300A, controlling the evaporation rate, and obtaining the alpha-Al with uniform surface temperature 2 O 3 (0001) Depositing an Ir epitaxial layer on the surface of the substrate to obtain the alpha-Al with the Ir epitaxial layer 2 O 3 (0001) A composite substrate;
6. after the deposition is finished, reducing the beam current to 0, closing the target baffle and the electron gun system, closing the heating device of the sample holder, naturally cooling to room temperature, closing the molecular pump and the mechanical pump, inflating to atmospheric pressure, and taking out the composite substrate;
7. placing the cooled composite substrate in an infrared annealing furnace, controlling the annealing temperature to be 400-1000 ℃, and introducing N 2 As the protective gas, the gas flow rate is 20-40 sccm, the annealing time is controlled to be 0.5-2 h for annealing, and Ir (111)/alpha-Al is obtained after the annealing is finished 2 O 3 (0001) A composite substrate.
2. The method for preparing the Ir (111) composite substrate for epitaxial single crystal diamond according to the electron beam evaporation process of claim 1, wherein the time for performing ultrasonic cleaning in deionized water, absolute ethyl alcohol and acetone in the step one is 10-30 min.
3. The method for preparing the Ir (111) composite substrate for epitaxial single crystal diamond according to claim 1, wherein the purity of the Ir particles in step two is greater than 99.99%.
4. The method for preparing Ir (111) composite substrate for epitaxial single crystal diamond according to claim 1 wherein the vacuum degree of the chamber is 3.0X 10 in the third step -4 ～6.0×10 -4 Pa。
5. The method for preparing Ir (111) composite substrate for epitaxial single crystal diamond according to claim 1 wherein the temperature is raised in the fourth step to make the sample holder alpha-Al 2 O 3 (0001) The substrate temperature reaches 600 ℃, and the stable temperature is 5-10 min.
6. The method for preparing Ir (111) composite substrate for epitaxial single crystal diamond according to claim 1 wherein the high voltage of the electron gun is controlled to 8kV in step five.
7. The method for preparing the Ir (111) composite substrate for epitaxial single crystal diamond according to the electron beam evaporation process of claim 1, wherein the deposition rate of the Ir epitaxial layer is controlled to be 0.04-0.10 nm/s in the step five.
8. The method for preparing Ir (111) composite substrate for epitaxial single crystal diamond according to the electron beam evaporation process of claim 1 wherein the thickness of the Ir epitaxial layer deposited in step five is 120-200 nm.
9. The method for preparing the Ir (111) composite substrate for epitaxial single crystal diamond according to the claim 1, wherein the temperature is raised to the annealing temperature at the temperature raising rate of 20 ℃/s-35 ℃/s in the seventh step.
10. The method for preparing the Ir (111) composite substrate for epitaxial single crystal diamond according to the claim 1, wherein the temperature reduction rate is controlled to be 2 ℃/s-30 ℃/s after the annealing in the seventh step.
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