CN102268650B - Magnetron sputtering method for preparing indium nitride thin film - Google Patents
Magnetron sputtering method for preparing indium nitride thin film Download PDFInfo
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- CN102268650B CN102268650B CN 201110188062 CN201110188062A CN102268650B CN 102268650 B CN102268650 B CN 102268650B CN 201110188062 CN201110188062 CN 201110188062 CN 201110188062 A CN201110188062 A CN 201110188062A CN 102268650 B CN102268650 B CN 102268650B
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Abstract
The invention relates to a magnetron sputtering method for preparing an indium nitride thin film. The method comprises the following sequential steps of: 1, taking silicon (111) as a substrate, washing the substrate clearly at room temperature and normal pressure and then placing the substrate in a nitrogen environment to dry; 2, placing the substrate treated in the step 1 in a sputtering chamber, taking aluminum as a target material, and growing a first buffer layer of aluminum nitride on the substrate by using the magnetron sputtering method under a vacuum condition; 3, replacing the target material with an aluminum-indium alloy of which the atomic ratio of aluminum to indium is 1:3 after finishing the growth of the first buffer layer of aluminum nitride, and completing growth of a second buffer layer of Al0.24In0.76N on the first buffer layer of aluminum nitride by using the magnetron sputtering method under the vacuum condition; and 4, replacing the target material with indium after finishing the growth of the second buffer layer of Al0.24In0.76N, and completing the growth of the indium nitride thin films on the second buffer layer of Al0.24In0.76N by using the magnetron sputtering method under the vacuum condition.
Description
Technical field
The invention belongs to nitride optoelectronic thin film material preparation field, particularly a kind of method that adopts the double-buffering layer technology to prepare the InN film by sputtering method.
Background technology
The group iii nitride semiconductor material is considered to the most potential photoelectric material, and InN is because its novel physical character and potential using value have been subjected to extensive concern in the recent period.Studies show that: the energy gap of InN is (Appl. Phys. Lett. 80 about 0.6-0.7eV, 3967 (2002)), rather than previous generally accepted 1. 9eV (Appl. Phys. Lett. 83,251 (2003)), so can obtain continuous adjustable direct band gap from 0.7eV (InN) to 6.2eV (AlN) by regulating alloy compositions, thereby utilize the material of unitary system just can prepare the photoelectric device of covering near infrared to the deep UV (ultraviolet light) spectral limit.The InN material has the highest mobility in the group iii nitride semiconductor material (maximum mobility is 14000cm under the room temperature
2V
-1s
-1), peak rate, electronic drifting rate and spike speed (4.3 * 10
7Cm/ s) and have a minimum effective electron mass m*=0. 05m
0(J. Appl. Phys. 94,2779-2808 (2003)).These characteristics make the InN material at high performance solar batteries, diode, laser apparatus, and optical fiber has very special advantages in the transistorized application of high frequency and two-forty.
Yet preparation InN film faces two big difficulties: the dissociation temperature of the one, InN material is lower, has just decomposed (Jpn. J. Appl. Phys. 42: 2549-2599, (2003)) about 600 ℃, and this just requires the InN that grows at low temperatures; The 2nd, be difficult to find the substrate of lattice and matched coefficients of thermal expansion.Sapphire is growth InN film substrate commonly used, but its lattice mismatch rate is up to 25% (Thin Solid Films, 515,4619 – 4623 (2007)).Silicon also is the epitaxial growth substrate material of using always, but InN and Si (111) substrate also has 8% lattice mismatch rate.Moreover in process of growth, surface of silicon is formed SiN by nitrogenize easily
x, this can cause the decline (Nanotechnology 20,345203 (2009)) of InN film quality.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of magnetically controlled sputter method of the InN of preparation film is provided, to reduce the lattice mismatch rate, improve the quality of InN film.
The magnetically controlled sputter method of preparation InN film of the present invention adopts the double-buffering layer technology, and processing step is as follows successively:
(1) processing of substrate
Be substrate with Si (111), under room temperature, normal pressure, substrate cleaned up to be placed in the nitrogen environment and dry up;
The growth of (2) first buffer layer AlN
To put into sputtering chamber through the substrate that handled step (1), and adopt magnetron sputtering method at the substrate growth first buffer layer AlN under vacuum condition, target is Al, with N
2Be reactant gases, Ar is working gas, N
2With the throughput ratio of Ar be 9:1, sputtering power 50W ~ 60W, sputtering time 20 minutes ~ 30 minutes, substrate temperature control is at 450 ℃～550 ℃ in the sputter procedure;
(3) second buffer layer Al
0.24In
0.76The growth of N
Behind the growth ending of the first buffer layer AlN, the atomic ratio of target being replaced by Al and In is the Al-In alloy of 1:3, adopts magnetron sputtering method to finish the second buffer layer Al under vacuum condition
0.24In
0.76The growth of N on the first buffer layer AlN is with N
2Be reactant gases, Ar is working gas, N
2With the throughput ratio of Ar be 3:1, sputtering power 80W～150W, sputtering time 10 minutes～30 minutes, substrate temperature control is at 250 ℃～350 ℃ in the sputter procedure;
(4) InN growth for Thin Film
The second buffer layer Al
0.24In
0.76After the end of N growth, target is replaced by In, under vacuum condition, adopts magnetron sputtering method to finish the InN film at the second buffer layer Al
0.24In
0.76Growth on the N is with N
2Be reactant gases, Ar is working gas, N
2With the throughput ratio of Ar be 3:1, sputtering power 60W ~ 120W, sputtering time 10 minutes ~ 30 minutes, substrate temperature control is at 250 ℃ ~ 350 ℃ in the sputter procedure.
In the aforesaid method, the growth step of the described first buffer layer AlN, the second buffer layer Al
0.24In
0.76In the growth step of N and the InN growth for Thin Film step, base vacuum degree≤5 * 10
-5Pa, operating air pressure are 0.35Pa ~ 0.45Pa.
In the aforesaid method, the cleaning step of substrate is: under room temperature, normal pressure successively in trieline ultrasonic cleaning at least 20 minutes, in acetone ultrasonic cleaning at least 30 minutes, in HF, soaked at least 10 minutes, then with deionized water rinsing at least 10 minutes.
The present invention has following beneficial effect:
(1) the present invention adopts vacuum magnetic-control sputtering method low-temperature epitaxy InN film, as long as maintenance operating air pressure and sputtering power are constant, can obtain stable deposition rate, and therefore the film that makes is even.
(2) preparation method of the present invention adopts AlN to do first for buffer layer, has significantly reduced Al
0.24In
0.76Lattice mismatch between N and substrate, temperature is 500 ± 50 ℃ during growing AIN, is conducive to nitrogen and aluminium atom and fully is reacted into the AlN synthetics and is deposited on substrate surface.
(3) preparation method of the present invention is because at first at substrate grown AlN buffer layer thereby the second buffer layer Al
0.24In
0.76The quality of N improves, because the InN film growth is at the second buffer layer Al
0.24In
0.76On the N, thereby further reduce the lattice mismatch of InN film and substrate, be conducive to the raising of InN film quality.
(4) the InN film crystal preferred orientation excellence of the method for the invention preparation only has the X-ray diffraction peak (see figure 1) of InN (0002) in its XRD figure.
(5) the InN film buffer layer thickness of the method for the invention preparation is less, the first buffer layer AlN and the second buffer layer Al
0.24In
0.76The total thickness of N only is about 150 nm, can the power and energy saving.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram of the InN film of the method for the invention (embodiment 1) preparation, and substrate is Si (111);
Fig. 2 is scanning electron microscope (SEM) picture of the InN film of the method for the invention (embodiment 1) preparation, and wherein, Fig. 2 (a) is the face shape appearance figure, and Fig. 2 (b) is sectional view;
Fig. 3 is high-resolution-ration transmission electric-lens (TEM) figure ((b), (c), (d) among the figure) that the transmission electron microscope (TEM) in the InN film cross section of the method for the invention (embodiment 1) preparation is schemed (among the figure (a)) and each subgrade;
Fig. 4 is x-ray photoelectron power spectrum (XPS) figure of the InN film of the method for the invention (embodiment 1) preparation;
Fig. 5 is X-ray diffraction (XRD) spectrogram of the InN film of Comparative Examples 1 preparation, and substrate is Si (111);
Fig. 6 is scanning electron microscope (SEM) picture of the InN film of Comparative Examples 1 preparation, and wherein, Fig. 6 (a) is the face shape appearance figure, and Fig. 6 (b) is sectional view.
Embodiment
Below by embodiment the magnetically controlled sputter method of preparation InN film of the present invention is described further.
Embodiment 1
The processing step of present embodiment is as follows successively:
(1) processing of substrate
Be substrate with Si (111), at first with substrate ultrasonic cleaning 20 minutes in trieline successively, ultrasonic cleaning is 30 minutes in acetone, soaks 10 minutes in hydrofluoric acid under room temperature, normal pressure, used deionized water rinsing then 10 minutes, and dried up with nitrogen at last that to put into sputtering chamber stand-by;
The growth of (2) first buffer layer AlN
(model: JGP560, manufacturing enterprise: finish Shenyang Scientific Instrument Research ﹠ Mfg. Center Co., Ltd., C.A.S), base vacuum is 4.0 * 10 to the ultra-high vacuum multifunctional magnetron sputtering equipment that is grown in of the first buffer layer AlN
-5Pa; To put into sputtering chamber through Si (111) substrate that handled step (1), and adopt magnetron sputtering method growing AIN buffer layer on substrate under vacuum condition, operating air pressure is controlled at 0.4Pa, and target is Al(purity 99.8%), N
2Be reactant gases, Ar is working gas, N
2Be respectively 5.4 Sccm and 0.6 Sccm with Ar, sputtering power 56W, sputtering time 30 minutes, substrate temperature control is at 500 ℃ in the sputter procedure; Ionization takes place and forms Ar in Ar
+, Ar
+Under electromagnetic field effect, collide target, Ar
+With the target atom exchange energy, the energy that target atom obtains will leave target material surface, with reactant gases N during greater than metal escape merit
2Reactive deposition forms the AlN buffer layer at substrate surface;
(3) second buffer layer Al
0.24In
0.76The growth of N
Behind the first buffer layer AlN growth ending, the atomic ratio of target being replaced by Al and In is the Al-In alloy of 1:3, and operating air pressure is controlled at 0.4Pa, N
2Be respectively 9.0 Sccm and 3.0 Sccm with Ar, sputtering power 100W, sputtering time 20 minutes, substrate temperature control is at 300 ℃ in the sputter procedure; Ionization takes place and forms Ar in Ar
+, Ar
+Under electromagnetic field effect, collide target, Ar
+With the target atom exchange energy, the energy that target atom obtains will leave target material surface, with reactant gases N during greater than metal escape merit
2Reactive deposition forms the second buffer layer Al on first buffer layer AlN surface
0.24In
0.76N;
(4) InN growth for Thin Film
The second buffer layer Al
0.24In
0.76Behind the N growth ending, target is replaced by In(purity 99.99%), operating air pressure is controlled at 0.4Pa, N
2Be respectively 9.0 Sccm and 3.0 Sccm with Ar, sputtering power is 80W, and sputtering time is 20 minutes, and substrate temperature control is at 300 ℃ in the sputter procedure; Ionization takes place and forms Ar in Ar
+, Ar
+Under electromagnetic field effect, collide target, Ar
+With the target atom exchange energy, the energy that target atom obtains will leave target material surface, with reactant gases N during greater than metal escape merit
2Reactive deposition is at the second buffer layer Al
0.24In
0.76The last formation of N InN film.
The InN film of this examples preparation X-ray diffraction (XRD) spectrogram see Fig. 1 (diffraction peak having only InN (0002)), scanning electron microscope (SEM) photo is seen Fig. 2, transmission electron microscope (TEM) photo is seen Fig. 3, x-ray photoelectron power spectrum (XPS) figure sees Fig. 4, analytical results shows, the prepared InN film of present embodiment is the fine zinc of six sides (wurtzite) structure, crystal growth preferred orientation excellence, (0002) diffraction peak is in 31.31 °, 0.219 ° of peak width at half height, grain size is 37.25 nm, buffer layer AlN and buffer layer Al
0.24In
0.76About 150 nm of the total thickness of N.
Comparative Examples 1
The processing step of this Comparative Examples is as follows successively:
(1) processing of substrate
Be substrate with Si (111), the treatment process of substrate is identical with embodiment 1;
(2) InN growth for Thin Film
(model: JGP560, manufacturing enterprise: finish Shenyang Scientific Instrument Research ﹠ Mfg. Center Co., Ltd., C.A.S), base vacuum is 4.0 * 10 to the InN growth for Thin Film at the ultra-high vacuum multifunctional magnetron sputtering equipment
-5Pa; To put into sputtering chamber through Si (111) substrate that handled step (1), and adopt magnetron sputtering method at substrate growth InN film under vacuum condition, operating air pressure is controlled at 0.4Pa, and target is In(purity 99.99%), N
2Be reactant gases, Ar is working gas, N
2Be respectively 9.0 Sccm and 3.0 Sccm with Ar, sputtering power 80W, sputtering time 20 minutes, substrate temperature control is at 300 ℃ in the sputter procedure; Ionization takes place and forms Ar in Ar
+, Ar
+Under electromagnetic field effect, collide target, Ar
+With the target atom exchange energy, the energy that target atom obtains will leave target material surface, with reactant gases N during greater than metal escape merit
2Reactive deposition forms the InN film at substrate surface.
The InN film of this Comparative Examples preparation X-ray diffraction (XRD) spectrogram see Fig. 5, scanning electron microscope (SEM) photo is seen Fig. 6, analytical results shows, the prepared InN film of this Comparative Examples is the fine zinc of six sides (wurtzite) structure, there are (0002), (102) and (103) diffraction peak of InN to occur in X-ray diffraction (XRD) spectrogram, wherein (0002) diffraction peak is in 31.63 °, and its peak width at half height is about 0.298 °.In addition, also have metal In cluster peak In(101) occur, illustrate that prepared InN film crystal preferred orientation is poor, second-rate.
Claims (2)
1. magnetically controlled sputter method for preparing the InN film is characterized in that processing step is as follows successively:
(1) processing of substrate
Be substrate with Si (111), under room temperature, normal pressure, substrate cleaned up to be placed in the nitrogen environment and dry up;
The growth of (2) first buffer layer AlN
To put into sputtering chamber through the substrate that handled step (1), and adopt magnetron sputtering method at the substrate growth first buffer layer AlN under vacuum condition, target is Al, with N
2Be reactant gases, Ar is working gas, N
2With the throughput ratio of Ar be 9:1, sputtering power 50W ~ 60W, sputtering time 20 minutes ~ 30 minutes, substrate temperature control is at 450 ℃～550 ℃ in the sputter procedure;
(3) second buffer layer Al
0.24In
0.76The growth of N
Behind the growth ending of the first buffer layer AlN, the atomic ratio of target being replaced by Al and In is the Al-In alloy of 1:3, adopts magnetron sputtering method to finish the second buffer layer Al under vacuum condition
0.24In
0.76The growth of N on the first buffer layer AlN is with N
2Be reactant gases, Ar is working gas, N
2With the throughput ratio of Ar be 3:1, sputtering power 80W～150W, sputtering time 10 minutes～30 minutes, substrate temperature control is at 250 ℃～350 ℃ in the sputter procedure;
(4) InN growth for Thin Film
The second buffer layer Al
0.24In
0.76After the end of N growth, target is replaced by In, under vacuum condition, adopts magnetron sputtering method to finish the InN film at the second buffer layer Al
0.24In
0.76Growth on the N is with N
2Be reactant gases, Ar is working gas, N
2With the throughput ratio of Ar be 3:1, sputtering power 60W ~ 120W, sputtering time 10 minutes ~ 30 minutes, substrate temperature control is at 250 ℃ ~ 350 ℃ in the sputter procedure.
2. according to the magnetically controlled sputter method of the described preparation of claim 1 InN film, it is characterized in that growth step, the second buffer layer Al of the described first buffer layer AlN
0.24In
0.76In the growth step of N and the InN growth for Thin Film step, base vacuum degree≤5 * 10
-5Pa, operating air pressure are 0.35Pa ~ 0.45Pa.
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| CN104694884A (en) * | 2015-03-03 | 2015-06-10 | 安阳工学院 | Polarity control method for indium nitride (InN) thin films |
| CN106024583B (en) * | 2016-05-13 | 2018-08-14 | 西北大学 | A method of preparing different crystalline phase preferential growth InN on Si (100) substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101197409A (en) * | 2006-11-07 | 2008-06-11 | 斯尔瑞恩公司 | Compound semiconductor substrate grown on metal layer, method for manufacturing the same, and compund semiconductor device using the same |
| CN101423927A (en) * | 2008-12-11 | 2009-05-06 | 四川师范大学 | Method for preparing AlxIn1-xN film |
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| CN101197409A (en) * | 2006-11-07 | 2008-06-11 | 斯尔瑞恩公司 | Compound semiconductor substrate grown on metal layer, method for manufacturing the same, and compund semiconductor device using the same |
| CN101423927A (en) * | 2008-12-11 | 2009-05-06 | 四川师范大学 | Method for preparing AlxIn1-xN film |
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