CN109830429B - Method for depositing InGaN film on Si (100) substrate by double-optical-path pulse laser - Google Patents
Method for depositing InGaN film on Si (100) substrate by double-optical-path pulse laser Download PDFInfo
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Abstract
The invention relates to a double-optical-path pulse laser deposition device and a method for depositing an InGaN film on a Si (100) substrate, wherein the device can divide laser into two paths to irradiate a target material, and the specific method comprises the following steps: putting the cleaned Si (100) substrate on a substrate table, heating to 650-750 ℃, and preserving heat for 50-70 min; sequentially depositing TiN, AlN, GaN and InGaN layers, wherein the adopted laser energy is respectively 150-150 mJ, 50-150mJ, 200-300mJ and 100-200mJ, and the deposition time is respectively 10-30 min, 30-50 min, 50-70min and 50-70 min; the InGaN layer is formed by a double-optical-path process. The invention can improve the quality of the thin film crystal and greatly improve the efficiency of devices such as a semiconductor laser, a light emitting diode and a solar cell.
Description
Technical Field
The invention relates to a double-light-path Pulsed Laser Deposition (PLD) coating method and application thereof, in particular to a method for preparing an epitaxial film and a film photoelectric device, especially an InGaN solar cell.
Background
PLD technology has been developed with the development of laser technology. In the 60 s of the 20 th century, shortly after the first ruby laser in the world was produced, people found that when a solid material was irradiated with a laser beam, electrons, ions and neutral atoms escaped from the surface of the solid material, and a luminous plasma region with a temperature of 103-104K was formed near the surface, and then thought that if these ablations were condensed on a substrate, a thin film could be obtained, thus leading to the concept of laser coating. Research into the interaction of laser light with matter has thus begun.
At present, photovoltaic thin film devices such as solar cells, LEDs, and LDs are mainly manufactured using Metal Organic Chemical Vapor Deposition (MOCVD) and Molecular Beam Epitaxy (MBE) equipment, as typified by group III nitrides having excellent performance. MOCVD and MBE are used for epitaxial growth of III-group nitride films, the temperature is high, large thermal stress is introduced in high-temperature epitaxial growth, so that adverse effects including phase separation, difficult doping and serious interface reaction are generated in an epitaxial layer, the performance of the surface of a substrate is deteriorated, and the like, the crystal quality of the film is finally reduced, the quality of a film device is reduced, and the application and popularization of the device are not utilized.
Pulsed Laser Deposition (PLD) overcomes the deficiencies and problems of MOCVD, MBE. Its main advantages include the following: (1) the laser energy density is high, various targets which are difficult to melt can be evaporated, and the low-temperature epitaxial growth of the film is realized; (2) the technological parameters are convenient to adjust, the deposition rate is high, and the experimental period is short; (3) the development potential is large, and the compatibility is good; (4) the film has stable components and is easy to obtain the expected stoichiometric ratio; (5) a plurality of targets (4-6) can be placed at the same time, which is beneficial to preparing a multilayer film with complex components; (6) the cleaning treatment is very convenient, and different types of films can be prepared. The advantages of PLD make it an irreplaceable advantage to other techniques in high quality nitride epitaxial growth.
However, the currently mainstream pulse laser deposition equipment generally adopts a single light path design concept, has great limitations, and is difficult to prepare an alloy film with adjustable super doping and components. The double-light-path pulse laser deposition method of the invention can perfectly solve the problem.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks and deficiencies of the prior art, it is an object of the present invention to provide a dual-beam pulsed laser deposition apparatus that can play a key role in thin film epitaxy, and has incomparable advantages with other technologies, especially in the preparation of super-doped thin films.
The invention also aims to provide an application method of the coating equipment, and the thin film crystal prepared by the coating equipment has high quality, and can greatly improve the efficiency of devices such as semiconductor lasers, light emitting diodes and solar cells.
The purpose of the invention can be achieved by adopting the following technical scheme:
a double-optical-path pulse laser deposition device comprises a growth chamber cavity, wherein a base is arranged in a central area below the growth chamber cavity, four uniformly-arranged rotary tables for placing targets are arranged on the base, and the base and the rotary tables are driven by a driving mechanism to rotate respectively so that the targets can rotate along with the rotary tables; the lower side wall or the bottom wall of the growth chamber cavity is also provided with a valve which is respectively connected with the mechanical pump and the molecular pump so that the mechanical pump and the molecular pump can vacuumize the growth chamber cavity; an auxiliary gas pipeline is arranged at the middle lower position of the growth chamber cavity and used for supplementing O in time in the film coating process2And N2(ii) a Two quartz windows are respectively arranged on two sides of the upper wall of the growth chamber cavity, a focusing mirror and a reflecting mirror are arranged at the positions outside the growth chamber cavity corresponding to the quartz windows, high-energy laser provided by a solid laser sequentially passes through a laser beam splitter, the reflecting mirror, the focusing mirror and the quartz windows and then irradiates on a target material inside the growth chamber cavity, and plasma plumes generated by the target material are deposited on a substrate placed on a rotary substrate table.
The substrate is a Si (100) substrate.
The high-energy laser wavelength is 248 nm.
The shell of the growth chamber cavity is made of high-pressure-resistant alloy steel.
The invention also claims a GaN-based LED epitaxial wafer, a solar cell epitaxial wafer, an LD epitaxial wafer or a photoelectric detector epitaxial wafer obtained by epitaxy on a sapphire substrate and a Si (100) substrate by adopting the double-optical-path pulsed laser deposition equipment.
The invention also claims a method for depositing an InGaN film on a Si (100) substrate, comprising the following specific steps:
step 1: cleaning the surface of the Si (100) substrate;
step 2: opening a sample inlet and placing the cleaned Si (100) substrate on a rotary substrate table in a cavity of a growth chamber;
and step 3: heating the Si (100) substrate to 650-750 ℃ and preserving heat for 50-70 min;
and 4, step 4: depositing a TiN buffer layer on the substrate by laser aiming at the TiN target material, wherein the laser energy is 150 and 250mJ, and the deposition time is 10-30 min;
and 5: rotating the target material to an AlN target material and raising the temperature to 700-800 ℃ to grow an AlN buffer layer, wherein the laser energy is 50-150mJ, and the deposition time is 30-50 min;
step 6: rotating the target material to the GaN target material to grow the non-doped GaN buffer layer, wherein the laser energy is 200 and 300mJ, and the deposition time is 50-70 min;
and 7: annealing the prepared epitaxial layer at 700-800 ℃ for 50-70 min;
and 8: growing a super-doped InGaN layer by using double-light-path pulse laser, and respectively irradiating laser beams to an In target material and a GaN target material by using double light paths, wherein the laser energy is 100-200mJ, and the deposition temperature and time are respectively 450-550 ℃ and 50-70 min.
Preferably, in step 1, the cleaning process of the Si (100) substrate is specifically: and (2) putting the Si (100) substrate into deionized water, ultrasonically cleaning at room temperature to remove sticky particles on the surface of the Si (100) substrate, washing with absolute ethyl alcohol, hydrofluoric acid and acetone in sequence to remove surface organic matters, and drying with high-purity dry nitrogen.
Preferably, in step 4, the thickness of the TiN buffer layer is 30-80 nm; in step 5, the AlN buffer layer has a thickness of 50 to 100 nm; in step 6, the thickness of the non-doped GaN buffer layer is 300-500 nm; in step 8, the thickness of the super-doped InGaN layer is 50-150 nm.
The invention can realize redistribution of laser energy by using double-pulse laser beams, and is suitable for super doping in the field of semiconductors. Compared with the prior art, the invention has the following advantages:
1. the invention is an improved PLD with the functions and advantages of traditional PLD. Either a single light path may be used or dual light path deposition may be achieved.
2. The film crystal prepared by the double-light-path pulse laser deposition coating equipment has high quality, and the efficiency of devices such as semiconductor lasers, light emitting diodes and solar cells can be greatly improved.
3. The double-light-path pulse laser deposition coating equipment has the advantages of simple growth process and low cost, and is suitable for manufacturing solar cells, LEDs, LDs and photoelectric detectors with quantum well structures.
4. The invention can save equipment purchasing cost and is beneficial to reducing production cost.
Drawings
Fig. 1 is a schematic structural diagram of a dual-optical-path pulsed laser deposition apparatus according to the present invention. Labeled as: 1-laser beam splitter, 2-first reflector, 3-first focusing mirror, 4-rotary substrate table, 5-rotary table, 6-auxiliary gas pipeline, 7-plasma plume, 8-second focusing mirror, 9-second reflector, 10-growth chamber cavity, 11-mechanical pump connecting valve and 12-molecular pump connecting valve.
FIG. 2 is an X-ray diffraction pattern of the Si (100) substrate after the step 1 treatment of the example.
FIG. 3 is an X-ray diffraction pattern of TiN, AlN, GaN buffer layers grown through steps 7-9 of the example.
FIG. 4 is an atomic force microscope image of TiN, AlN, GaN buffer layers grown by the steps 7-9 of the example.
FIG. 5 is an X-ray photoelectron spectrum of TiN, AlN, GaN buffer layer grown through steps 7-9 of the example.
FIG. 6 is a scanning electron microscope image of the surface morphology of the InGaN thin film grown in step 11 of the embodiment.
FIG. 7 is an atomic force microscope surface topography of an InGaN thin film grown on a (100) plane Si substrate by epitaxy using a PLD dual optical path process in an embodiment.
FIG. 8 is a diagram showing the UV-VIS absorption spectrum of an InGaN thin film grown on a (100) plane Si substrate by epitaxy using a PLD two-optical path process in example.
Detailed Description
The invention is further described with reference to specific examples.
Referring to fig. 1, a dual optical path pulsed laser deposition apparatus includes a growth chamber cavity 10, a base is disposed in a central region below the growth chamber cavity 10, four uniformly arranged rotating discs 5 for placing a target are disposed on the base, and the base and the rotating discs 5 are driven by a driving mechanism to rotate respectively, so that the target can rotate with the rotating discs 5; a mechanical pump connecting valve 11 and a molecular pump connecting valve 12 are further arranged on the lower side wall or the bottom wall of the growth chamber cavity 10 so as to connect the mechanical pump and the molecular pump to vacuumize the growth chamber cavity 10; an auxiliary gas pipeline 6 is arranged at the middle lower position of the growth chamber cavity 10 and used for supplementing O in time in the film coating process2And N2(ii) a Two quartz windows are respectively arranged on two sides of the upper wall of a growth chamber cavity 10, a first focusing mirror 3, a first reflecting mirror 2, a second focusing mirror 8 and a second reflecting mirror 9 are arranged at positions outside the growth chamber cavity 10 corresponding to the quartz windows, 248nm high-energy laser provided by a solid laser is divided into two paths after passing through a laser beam splitter 1, one of the two paths sequentially passes through the first reflecting mirror 2, the first focusing mirror 3 and the quartz window and then irradiates on a target material inside the growth chamber cavity 10, and the other path sequentially passes through the second reflecting mirror 9, the second focusing mirror 8 and the quartz window and then irradiates on the target material inside the growth chamber cavity 10; the plasma plume 7 generated by the target is deposited on a Si (100) substrate placed on the rotating substrate table 4.
The outer shell of the growth chamber cavity 10 is made of high-pressure-resistant alloy steel. The laser adopted by the PLD deposition equipment is a KrF excimer laser.
The method for depositing the InGaN film on the Si (100) substrate comprises the following specific steps of:
step 1: cleaning a silicon wafer: (1) soaking in deionized water for 5min to remove dust on the surface; (2) placing the silicon wafer into a hydrogen peroxide solution, and ultrasonically oscillating for 5min to remove paraffin on the surface; (3) placing the silicon wafer into a 5% hydrofluoric acid solution for ultrasonic oscillation for 5min to remove impurity oxides on the surface; (4) then placing the mixture into acetone for ultrasonic oscillation for 5min to remove oil stains on the surface; (5) soaking in alcohol, ultrasonic vibrating for 5min, and removing organic substances on the surface; (6) washing with deionized water; (7) drying by a nitrogen gun;
step 2: when the pressures of the sample feeding chamber and the sputtering chamber show the same magnitude, pushing a sample into the sputtering cavity by using a sensor, and adjusting the distance between a target material and the substrate to be 5 cm;
and step 3: starting the mechanical pump as required, starting the molecular pump when the vacuum gauge is lower than 20Pa, and pumping the vacuum in the sputtering cavity to an ideal vacuum degree, generally to 10-5Pa；
And 4, step 4: when the vacuum degree of the sputtering cavity reaches a required value, heating the substrate, controlling the heating time and speed by a computer, heating to 700 ℃, and then preserving heat for one hour;
and 5: setting all parameters of laser, opening a laser to preheat for 8 minutes, rotating the target, putting down a baffle plate in front of a substrate, adjusting a light path through a reflecting and focusing mirror, and enabling a laser beam to be emitted into the surface layer of the target in a sputtering cavity at an optimal angle;
step 6: laser beams are emitted to the target through the quartz window and are pre-sputtered for 5min, and oxides on the surface layer of the target are eliminated through pre-sputtering;
and 7: extending the TiN buffer layer by adopting a PLD (programmable logic device) process, turning over a baffle right in front of the substrate, performing predeposition on the TiN substrate for 10min, and then beginning to deposit the TiN buffer layer, wherein the process conditions are as follows: the substrate temperature is 700 ℃, a TiN target with the purity of 99.99999 percent is bombarded by pulse laser to grow the TiN buffer layer, and N is introduced during the growth2The pressure of the reaction chamber is 8 x 10-5torr, wherein the radio frequency power is 300W, the laser energy is 200mJ, the laser frequency is 5Hz, and the deposition time is 20 min;
and 8: extending an AlN buffer layer by adopting a PLD process, wherein the process conditions are as follows: the substrate temperature is 750 ℃, the AlN buffer layer is grown by bombarding the AlN target with the purity of 99.99999 percent by adopting pulse laser, and N is introduced during growth2The pressure of the reaction chamber is 8 x 10- 5torr, wherein the radio frequency power is 300W, the laser energy is 100mJ, the laser frequency is 5Hz, and the deposition time is 40 min;
and step 9: extending a GaN buffer layer by adopting a PLD process, wherein the process conditions are as follows: the substrate temperature is 750 ℃, and a GaN buffer layer is grown by bombarding a GaN target with the purity of 99.99999 percent by adopting pulse laserIntroduction of N2The pressure of the reaction chamber is 8 x 10- 5torr, wherein the radio frequency power is 200W, the laser energy is 250mJ, the laser frequency is 5Hz, and the deposition time is 60 min;
step 10: annealing the prepared epitaxial layer at 750 ℃ for 1 h;
step 11: depositing an InGaN film by adopting a PLD (laser deposition) process, wherein the process conditions are as follows: the substrate temperature is 500 ℃, a GaN target with the purity of 99.99999 percent and a metal In target are bombarded by double-pulse laser beams to grow an InGaN film, and N is introduced during growth2The pressure of the reaction chamber is 8 x 10-5torr, wherein the radio frequency power is 300W, the laser energy is 150mJ, the laser frequency is 5Hz, and the deposition time is 60 min;
the feasibility and the effect of the present invention are further confirmed by the structure and performance test effects of the samples shown in fig. 2 to 8.
As shown in FIG. 2, the X-ray diffraction pattern of the Si substrate used in the present invention shows that the Si substrate has a preferred orientation of the (100) crystal plane.
Fig. 3 is an X-ray diffraction pattern of the epitaxial TiN, AlN, GaN buffer layer according to the present invention using PLD process, from which it can be seen that both TiN and AlN films preferentially grow along the (200) crystal plane, and the GaN film shows a weak diffraction peak at 2 θ of 36.9 °, corresponding to the cubic GaN (101) crystal plane, indicating that cubic GaN is obtained at this time.
FIG. 4 is an atomic force microscope surface topography of the TiN, AlN, GaN buffer layer of the invention using PLD process epitaxy, the scanning range is 2.5 μm × 2.5 μm. It can be seen that the surface of the film is relatively flat when the laser energy is low, but large size particles are sporadically distributed. When the laser energy is increased to 250mJ/p, a plurality of large particles appear on the surface of the GaN film, the deposition rate of the particles is increased due to the overhigh laser energy, and the first deposited particles are covered by the subsequent particles without having to migrate to the position with the minimum free energy, so that the grain size of the crystal grains on the surface of the film is increased, and the flatness of the surface of the film is reduced.
FIG. 5 is an X-ray photoelectron spectrum of a GaN film epitaxially grown on a TiN and AlN buffer layer of a (100) crystal plane Si substrate by a PLD process according to the present invention. It can be seen from the figure that except Ga, NPeaks other than O did not show diffraction peaks of other elements. It can also be seen that GaN film Ga3p3，Ga3p1XPS spectrum peak of (1), wherein Ga3p3，Ga3p1The binding energies of (A) and (B) are respectively 107.2eV and 108 eV. As can also be seen in figure 5 of the drawings,
heel
Corresponding to 1118.7eV and 1146.7eV, respectively, of the free gallium atom
The binding energy of (a) corresponds to a chemical shift of 1116.6eV and 1118.5eV and the binding energy of Ga-N bond corresponding to 1116.7eV and 1143.8eV, the binding energy of Ga atom is 1116.6eV, and beta-Ga is2O3The binding energies of (A) are 1119.5eV and 1146.4eV, and the above results all indicate the presence of Ga-N bonds in the obtained film. The XPS spectrum shows that slight shifts in Ga2p may be caused by Ga-O bonds.
FIG. 6 is a scanning electron microscope image of the surface morphology of an InGaN thin film grown on a (100) plane Si substrate by epitaxy using a PLD dual optical path process, from which it can be seen that the surface of the InGaN thin film is relatively flat and a few large particles can be seen, the particles are uniformly distributed and have a very small diameter.
FIG. 7 is an atomic force microscope surface morphology of an InGaN film grown on a (100) crystal plane Si substrate by epitaxy using a PLD (laser induced deposition) dual optical path process, the InGaN film surface is relatively flat, the sizes of crystal grains are relatively uniform, island-shaped crystal grains with large sizes exist on the film surface in a relatively flat area, probably because the diffusion speed of the crystal grains on the surface of a buffer layer becomes slow due to too long deposition time, the growth of InGaN crystal nuclei is not facilitated, and an amorphous InGaN film is easily generated.
FIG. 8 is a diagram of the UV-VIS absorption spectrum of an InGaN film grown on a (100) plane Si substrate by epitaxy using a PLD dual optical path process according to the present invention, from which it can be seen that the InGaN film absorbs light waves around 350 nm.
Claims (3)
1. A method for depositing InGaN film on a Si (100) substrate is completed by using double-optical-path pulse laser deposition equipment, the equipment comprises a growth chamber cavity, a base is arranged in the central area below the growth chamber cavity, four rotating discs which are uniformly arranged and used for placing a target material are arranged on the base, and the base and the rotating discs are driven by a driving mechanism to rotate respectively, so that the target material can rotate along with the rotating discs; the lower side wall or the bottom wall of the growth chamber cavity is also provided with a valve which is respectively connected with the mechanical pump and the molecular pump so that the mechanical pump and the molecular pump can vacuumize the growth chamber cavity; an auxiliary gas pipeline is arranged at the middle lower position of the growth chamber cavity and used for timely supplementing O2 and N2 in the film coating process; two quartz windows are respectively arranged on two sides of the upper wall of the growth chamber cavity, a focusing mirror and a reflecting mirror are arranged outside the growth chamber cavity and correspond to the quartz windows, high-energy laser provided by a solid laser sequentially passes through a laser beam splitter, the reflecting mirror, the focusing mirror and the quartz windows and then irradiates on a target material inside the growth chamber cavity, and plasma plumes generated by the target material are deposited on a substrate placed on a rotary substrate table;
the method is characterized by comprising the following specific steps of:
step 1: cleaning the surface of the Si (100) substrate;
step 2: opening a sample inlet and placing the cleaned Si (100) substrate on a rotary substrate table in a cavity of a growth chamber;
and step 3: heating the Si (100) substrate to 650-750 ℃ and preserving heat for 50-70 min;
and 4, step 4: depositing a TiN buffer layer on the substrate by laser aiming at the TiN target material, wherein the laser energy is 150 and 250mJ, and the deposition time is 10-30 min;
and 5: rotating the target material to an AlN target material and raising the temperature to 700-800 ℃ to grow an AlN buffer layer, wherein the laser energy is 50-150mJ, and the deposition time is 30-50 min;
step 6: rotating the target material to the GaN target material to grow the non-doped GaN buffer layer, wherein the laser energy is 200 and 300mJ, and the deposition time is 50-70 min;
and 7: annealing the prepared epitaxial layer at 700-800 ℃ for 50-70 min;
and 8: growing a super-doped InGaN layer by using double-light-path pulse laser, and respectively irradiating laser beams to an In target material and a GaN target material by using double light paths, wherein the laser energy is 100-200mJ, and the deposition temperature and time are respectively 450-550 ℃ and 50-70 min.
2. The method according to claim 1, wherein in step 1, the cleaning process of the Si (100) substrate is specifically: and (2) putting the Si (100) substrate into deionized water, ultrasonically cleaning at room temperature to remove sticky particles on the surface of the Si (100) substrate, washing with absolute ethyl alcohol, hydrofluoric acid and acetone in sequence to remove surface organic matters, and drying with high-purity dry nitrogen.
3. The method of claim 1, wherein in step 4, the TiN buffer layer has a thickness of 30-80 nm; in step 5, the AlN buffer layer has a thickness of 50 to 100 nm; in step 6, the thickness of the non-doped GaN buffer layer is 300-500 nm; in step 8, the thickness of the super-doped InGaN layer is 50-150 nm.
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