CN103014654A - Preparation method of AlN/ZnO/InGaN/diamond/Si multilayer-structure surface acoustic wave filter - Google Patents
Preparation method of AlN/ZnO/InGaN/diamond/Si multilayer-structure surface acoustic wave filter Download PDFInfo
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Abstract
The invention belongs to the field of piezoelectric film materials, and particularly relates to a preparation method of an AlN/ZnO/InGaN/diamond/Si multilayer-structure surface acoustic wave filter. The method comprises the following steps: cleaning an Si substrate, sending the Si substrate into a hot-wire chemical vapor deposition reaction chamber, depositing a diamond film with the thickness of 100-300nm on the Si substrate, sending the substrate into a metal organic compound chemical vapor deposition reaction chamber, introducing trimethyl indium, trimethyl gallium and nitrogen gas into the reaction chamber, depositing an InGaN film with the thickness of 20-100nm on the diamond/Si substrate, simultaneously introducing argon carrying diethyl zinc and oxygen into the reaction chamber, depositing a ZnO film with the thickness of 20-100nm on the InGaN/diamond/Si substrate, and finally, introducing trimethyl aluminum and nitrogen gas into the reaction chamber to obtain the AlN/ZnO/InGaN/diamond/Si multilayer-structure surface acoustic wave filter. In the method, the diamond film is firstly deposited on the Si substrate, and the smooth high-crystallization-degree high-quality AlN nano piezoelectric film with high C-axis preferred orientation is deposited by using nano ZnO and InGaN films with high C-axis preferred orientation as buffer layers.
Description
Technical field
The invention belongs to the piezoelectric film material field, be specifically related to the preparation method of a kind of AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device.
Background technology
Surface Acoustic Wave Filter be a kind of utilize the preparation of surface acoustic wave effect and resonance characteristic to the selectable device of frequency, a kind of SAW(surface acoustic wave of application quantity maximum) device, its effect is to allow the signal of a certain frequency band to pass through, and stop the signal of other frequency band to pass through, utilize the mid-frequency of the SAW wave filter of interdigital transducer (IDT) making
fBy the acoustic surface wave propagation speed of making material
VWith the cycle of IDT electrode
LDetermine, namely
f=
V/
L
As everyone knows, diamond is the fastest material of acoustic propagation velocity in all substances, be higher than 10000m/s, make the high frequency SAW wave filter of 2.5GHz with it, its IDT electrode can relax to 1 μ m, and the technical requirements that electrode is prepared reduces greatly, in addition, the Young's modulus that diamond is very high is conducive to the high-fidelity transmission of acoustic wave; High thermal conductivity and good thermotolerance also are suitable for the application such as high-power transmitting terminal high frequency filter.These characteristics are so that diamond SAW wave filter becomes at present one of important in the world research focus.But diamond is not piezoelectric, self does not have piezoelectricity, can't excite and the receiving surface ripple, need to deposit in its surface one deck piezoelectric membrane and make the film SAW wave filter of multilayer, therefore, how deposit the key issue that Multilayer system that high c-axis orientation, low surface roughness and high-resistance piezoelectric membrane can be applicable to high frequency SAW wave filter just becomes current research at the high-sound-velocity material diamond.
AlN is electrical insulator, dielectric properties are good, loud propagation rate, the low transmission loss, chemical stability is good, good and absorb little and excellent high-temperature oxidation resistance to long infrared band perviousness at short infrared band, it is emerging electric elements material, but because diamond film substrate base and AlN material have very high lattice fit, so large lattice is adaptive to have caused very high dislocation desity, to the non-radiative recombination center in the acoustic surface wave filter device be increased, limited the further lifting of its internal quantum efficiency, be unfavorable for the transmission of sound wave, therefore, how the high quality AlN piezoelectric membrane that satisfies the SAW requirement on devices is incorporated into and becomes a gordian technique difficult problem that needs to be resolved hurrily on the diamond film.
Summary of the invention
In order to solve problems of the prior art, the invention provides the preparation method of a kind of AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device, purpose is passed through organic chemical vapor deposition, on the diamond thin substrate, deposit successively the ZnO of high C axle preferrel orientation and InGaN film as buffer layer, the nanometer AlN film for preparing high C axle preferrel orientation obtains the AlN/ZnO/InGaN/ diamond of excellent performance/Si multilayered structure acoustic surface wave filter device.
The technical scheme of realization the object of the invention is carried out according to following steps:
(1) with the Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, dry up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, in reaction chamber, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 100-300nm;
(2) with the above-mentioned diamond of deionized water rinsing/Si substrate, send into after drying up in the organometallics chemical gaseous phase deposition reaction chamber, with diamond/Si substrate heating to 300-600 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 0.6-2.0sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 0.3-1.0sccm is the nitrogen of 100-150sccm, deposit thickness is the InGaN film of 20-100nm on diamond/Si substrate;
(3) then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 20-100nm, uses afterwards high pure nitrogen clean deposition chamber;
(4) finally passing into trimethyl aluminium and the flow that flow is 0.6-2.0sccm in the reaction chamber is the nitrogen of 100-150sccm, with ZnO/InGaN/ diamond/Si substrate heating to 200-800 ℃, the operating device microwave power is 650W, deposit thickness is the AlN film of 500-1000nm on ZnO/InGaN/ diamond/Si substrate, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device.
Trimethyl indium reaction source control temperature is 20 ℃ among the present invention, and trimethyl-gallium reaction source control temperature is-14.1 ℃.
Compared with prior art, characteristics of the present invention and beneficial effect are:
The inventive method is at first at Si base substrate deposition preparation diamond thin, then with nano-ZnO that high C axle preferrel orientation is arranged and InGaN film as buffer layer, the AlN nanometer piezoelectric membrane of the high-quality of the high C axle preferrel orientation of smooth smooth, the better crystallinity degree of deposition preparation;
Deposition process in the inventive method is easy to control, the AlN/ZnO/InGaN/ diamond that obtains/Si multilayered structure acoustic surface wave filter device piezoelectric membrane good uniformity, velocity of sound transmission performance is excellent, can satisfy the application demand in the fields such as high frequency, high electromechanical coupling factor, low-loss, high-power SAW device, can be for the manufacture of high-power, high-frequency acoustic surface wave filter device.
Description of drawings
Fig. 1 is the AlN/ZnO/InGaN/diamond/Si multi-layered film structure surface acoustic wave filtering device schematic diagram that the inventive method obtains;
Among the figure: 1 is the Si substrate, and 2 is diamond thin, and 3 is InGaN film buffer layer, and 4 is the ZnO film buffer layer, and 5 is the AlN film;
Fig. 2 is the cross section SEM figure of the AlN/ZnO/InGaN/diamond/Si multi-layered film structure surface acoustic wave filtering device in the embodiment of the invention 1;
Fig. 3 is the surperficial SEM figure of the AlN/ZnO/InGaN/diamond/Si multi-layered film structure surface acoustic wave filtering device in the embodiment of the invention 2;
The surperficial SEM figure of the AlN/ZnO/InGaN/diamond/Si multi-layered film structure surface acoustic wave filtering device in Fig. 4 embodiment of the invention 3;
The surperficial SEM figure of the AlN/ZnO/InGaN/diamond/Si multi-layered film structure surface acoustic wave filtering device in Fig. 5 embodiment of the invention 4;
Embodiment
Organometallics chemical gaseous phase deposition of the present invention is the part of ERC-PVMOCVD equipment, has been open in 2110902328.1 the patent at application number; Described hot-wire chemical gas-phase deposition chamber is on the conventional CVD equipment.
Below in conjunction with embodiment technical scheme of the present invention is described further.
Embodiment 1
The Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, is dried up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, in reaction chamber, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 100nm;
With the above-mentioned diamond of deionized water rinsing/Si substrate, send into organometallics chemical gaseous phase deposition reaction chamber, with diamond/Si substrate heating to 300 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 0.6sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 0.3sccm is the nitrogen of 100sccm, deposit thickness is the InGaN film of 20nm on diamond/Si substrate;
Then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 20nm, uses afterwards high pure nitrogen clean deposition chamber;
Finally passing into trimethyl aluminium and the flow that flow is 0.6sccm in the reaction chamber is the nitrogen of 100sccm, with ZnO/InGaN/ diamond/Si substrate heating to 200 ℃, the operating device microwave power is 650W, depositing grain size at ZnO/InGaN/ diamond/Si substrate is 60nm, thickness is the AlN film of 500nm, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device, its structure as shown in Figure 1, cross section SEM figure as shown in Figure 2, surface SEM schemes as shown in Figure 3, and as can be seen from the figure its surface and intermembranous good uniformity carry out the Hall test to it, analyze its electric property result and show that it presents high value character, satisfy device to the requirement of resistance.
The Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, is dried up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, in reaction chamber, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 200nm;
With the above-mentioned diamond of deionized water rinsing/Si substrate, send in the organometallics chemical gaseous phase deposition equipment, with diamond/Si substrate heating to 400 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 1.0sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 0.5sccm is the nitrogen of 100sccm, deposit thickness is the InGaN film of 30nm on diamond/Si substrate;
Then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 30nm, uses afterwards high pure nitrogen clean deposition chamber;
Finally passing into trimethyl aluminium and the flow that flow is 1.0sccm in the reaction chamber is the nitrogen of 120sccm, with ZnO/InGaN/ diamond/Si substrate heating to 300 ℃, the operating device microwave power is 650W, depositing grain size at ZnO/InGaN/ diamond/Si substrate is 60nm, thickness is the AlN film of 600nm, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device, its structure as shown in Figure 1, surface SEM figure as shown in Figure 4, as can be seen from the figure its surface and intermembranous good uniformity, it is carried out the Hall test, analyze its electric property result and show that it presents high value character, satisfy device to the requirement of resistance.
The Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, is dried up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 300nm;
With the above-mentioned diamond of deionized water rinsing/Si substrate, send in the organometallics chemical gaseous phase deposition equipment, with diamond/Si substrate heating to 600 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 2.0sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 1.0sccm is the nitrogen of 150sccm, deposit thickness is the InGaN film of 100nm on diamond/Si substrate;
Then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 100nm, uses afterwards high pure nitrogen clean deposition chamber;
Finally passing into trimethyl aluminium and the flow that flow is 2.0sccm in the reaction chamber is the nitrogen of 150sccm, with ZnO/InGaN/ diamond/Si substrate heating to 800 ℃, the operating device microwave power is 650W, depositing grain size at ZnO/InGaN/ diamond/Si substrate is 60nm, thickness is the AlN film of 1000nm, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device, its structure as shown in Figure 1, surface SEM figure as shown in Figure 5, as can be seen from the figure its surface and intermembranous good uniformity, it is carried out the Hall test, analyze its electric property result and show that it presents high value character, satisfy device to the requirement of resistance.
The Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, is dried up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 250nm;
With the above-mentioned diamond of deionized water rinsing/Si substrate, send in the organometallics chemical gaseous phase deposition equipment, with diamond/Si substrate heating to 500 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 1.5sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 0.5sccm is the nitrogen of 130sccm, deposit thickness is the InGaN film of 80nm on diamond/Si substrate;
Then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 80nm, uses afterwards high pure nitrogen clean deposition chamber;
Finally passing into trimethyl aluminium and the flow that flow is 1.5sccm in the reaction chamber is the nitrogen of 120sccm, with ZnO/InGaN/ diamond/Si substrate heating to 700 ℃, the operating device microwave power is 650W, depositing grain size at ZnO/InGaN/ diamond/Si substrate is 60nm, thickness is the AlN film of 800nm, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device, its structure as shown in Figure 1, it is carried out the Hall test, analyze its electric property result and show that it presents high value character, satisfy device to the requirement of resistance.
The Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, is dried up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 150nm;
With the above-mentioned diamond of deionized water rinsing/Si substrate, send in the organometallics chemical gaseous phase deposition equipment, with diamond/Si substrate heating to 400 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 1.0sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 0.8sccm is the nitrogen of 150sccm, deposit thickness is the InGaN film of 80nm on diamond/Si substrate;
Then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 60nm, uses afterwards high pure nitrogen clean deposition chamber;
Finally passing into trimethyl aluminium and the flow that flow is 1.8sccm in the reaction chamber is the nitrogen of 110sccm, with ZnO/InGaN/ diamond/Si substrate heating to 500 ℃, the operating device microwave power is 650W, depositing grain size at ZnO/InGaN/ diamond/Si substrate is 60nm, thickness is the AlN film of 700nm, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device, its structure as shown in Figure 1, it is carried out the Hall test, analyze its electric property result and show that it presents high value character, satisfy device to the requirement of resistance.
Claims (2)
1. the preparation method of AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device is characterized in that carrying out according to following steps:
(1) with the Si substrate with acetone, ethanol and deionized water ultrasonic cleaning, dry up with nitrogen and to send in the hot filament chemical vapor deposition reactor chamber, reaction chamber is evacuated to 9.0 * 10
-4Behind the Pa, with Si substrate heating to 500 ℃, in reaction chamber, pass into the CH that flow is 1.6sccm
4With flow be the H of 200sccm
2, the control microwave power is 650W, at the thick diamond film of Si substrate deposition 100-300nm;
(2) with the above-mentioned diamond of deionized water rinsing/Si substrate, send into after drying up in the organometallics chemical gaseous phase deposition reaction chamber, with diamond/Si substrate heating to 300-600 ℃, the operating device microwave power is 650W, pass into the trimethyl indium that flow is respectively 0.6-2.0sccm in the reaction chamber, trimethyl-gallium and the flow that flow is 0.3-1.0sccm is the nitrogen of 100-150sccm, deposit thickness is the InGaN film of 20-100nm on diamond/Si substrate;
(3) then pass into simultaneously argon gas and the oxygen that carries zinc ethyl in reaction chamber, the throughput ratio of control argon gas and oxygen is 1:100, at InGaN/ diamond/thick ZnO film of Si substrate deposition 20-100nm, uses afterwards high pure nitrogen clean deposition chamber;
(4) finally passing into trimethyl aluminium and the flow that flow is 0.6-2.0sccm in the reaction chamber is the nitrogen of 100-150sccm, with ZnO/InGaN/ diamond/Si substrate heating to 200-800 ℃, the operating device microwave power is 650W, deposit thickness is the AlN film of 500-1000nm on ZnO/InGaN/ diamond/Si substrate, when treating that depositing temperature is reduced to room temperature, open the sediment chamber, obtain AlN/ZnO/InGaN/ diamond/Si multilayered structure acoustic surface wave filter device.
2. the preparation method of a kind of AlN/ZnO/InGaN/ diamond according to claim 1/Si multilayered structure acoustic surface wave filter device is characterized in that trimethyl indium reaction source control temperature is 20 ℃, and trimethyl-gallium reaction source control temperature is-14.1 ℃.
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| CN103352203A (en) * | 2013-07-17 | 2013-10-16 | 沈阳工程学院 | Preparation method for InN film low temperature sedimentation on AIN buffer layer/diamond film/Si multilayer film structure substrate by adopting ECR-PEMOCVD |
| CN103352208A (en) * | 2013-07-17 | 2013-10-16 | 沈阳工程学院 | Preparation method for InN film low temperature sedimentation on diamond plated film by adopting ECR-PEMOCVD |
| CN103361629A (en) * | 2013-07-17 | 2013-10-23 | 沈阳工程学院 | Preparation method for depositing InN film on GaN buffer layer/diamond film/Si multilayer film structure substrate at low temperature by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) |
| CN103388130A (en) * | 2013-07-17 | 2013-11-13 | 沈阳工程学院 | Method for preparing InN films through low temperature deposition on ZnO buffer layers / diamond films / multilayer film-structured Si substrates by means of ECR-PEMOCVD |
| CN104980117A (en) * | 2015-06-15 | 2015-10-14 | 电子科技大学 | Flexible surface acoustic wave device resistant to high temperature and manufacturing method thereof |
| CN107171653A (en) * | 2017-04-13 | 2017-09-15 | 天津理工大学 | A kind of SAW device with high electromechanical coupling factor and high center frequency |
| CN107385394A (en) * | 2017-06-26 | 2017-11-24 | 深圳大学 | ZnO/AlN/Si multilayer films and preparation method and application |
| WO2021134606A1 (en) * | 2019-12-31 | 2021-07-08 | Applied Materials, Inc. | Method and apparatus for deposition of piezo-electric materials |
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| CN103361629A (en) * | 2013-07-17 | 2013-10-23 | 沈阳工程学院 | Preparation method for depositing InN film on GaN buffer layer/diamond film/Si multilayer film structure substrate at low temperature by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) |
| CN103388130A (en) * | 2013-07-17 | 2013-11-13 | 沈阳工程学院 | Method for preparing InN films through low temperature deposition on ZnO buffer layers / diamond films / multilayer film-structured Si substrates by means of ECR-PEMOCVD |
| CN103352208B (en) * | 2013-07-17 | 2015-08-12 | 沈阳工程学院 | The preparation method of ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film |
| CN103352203B (en) * | 2013-07-17 | 2015-08-19 | 沈阳工程学院 | The preparation method of ECR-PEMOCVD low temperature depositing InN film on AlN buffer layer/diamond thin/Si multi-layer film structure substrate |
| CN103352203A (en) * | 2013-07-17 | 2013-10-16 | 沈阳工程学院 | Preparation method for InN film low temperature sedimentation on AIN buffer layer/diamond film/Si multilayer film structure substrate by adopting ECR-PEMOCVD |
| CN103361629B (en) * | 2013-07-17 | 2016-06-01 | 沈阳工程学院 | The preparation method of ECR-PEMOCVD low temperature depositing InN film on GaN buffer layer/diamond thin/Si multi-layer film structure substrate |
| CN104980117A (en) * | 2015-06-15 | 2015-10-14 | 电子科技大学 | Flexible surface acoustic wave device resistant to high temperature and manufacturing method thereof |
| CN107171653A (en) * | 2017-04-13 | 2017-09-15 | 天津理工大学 | A kind of SAW device with high electromechanical coupling factor and high center frequency |
| CN107385394A (en) * | 2017-06-26 | 2017-11-24 | 深圳大学 | ZnO/AlN/Si multilayer films and preparation method and application |
| CN107385394B (en) * | 2017-06-26 | 2019-06-25 | 深圳大学 | ZnO/AlN/Si multilayer films and preparation method and application |
| WO2021134606A1 (en) * | 2019-12-31 | 2021-07-08 | Applied Materials, Inc. | Method and apparatus for deposition of piezo-electric materials |
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