CN116024659A - Preparation method of hexagonal phase tantalum pentoxide single crystal film - Google Patents
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Abstract
The invention discloses a preparation method of a hexagonal phase tantalum pentoxide monocrystalline film, and belongs to the technical field of photoelectronic information functional materials. Tantalum ethoxide is used as an organic metal compound material, high-purity oxygen is used as oxidizing gas, and a hexagonal phase tantalum pentoxide single crystal film without twin crystals is prepared on a hexagonal structured lanthanum fluoride single crystal substrate by adopting metal organic chemical vapor deposition equipment. The hexagonal phase tantalum pentoxide single crystal film material prepared by the method has high single crystal quality and good stability, and therefore has good application prospect in the field of semiconductor devices.
Description
Technical Field
The invention relates to a preparation method of a high-quality hexagonal phase tantalum pentoxide single crystal film based on a lanthanum fluoride substrate, and belongs to the technical field of wide-bandgap oxide semiconductor photoelectric materials.
Background
In recent years, with the rapid development of semiconductor technology, conductor materials are being developed toward a wide band gap, higher breakdown voltage, and low loss. Corresponding semiconductor devices are being developed towards high power, high integration and low power consumption, and wide band gap oxide materials are one of the hot spots of current research. Tantalum pentoxide (Ta) 2 O 5 ) The material mainly has tetragonal, orthorhombic and hexagonal phase structures, has the characteristics of wide band gap, high breakdown voltage, high dielectric constant, stable physical and chemical properties and the like, and is a potential multifunctional material. Ta 2 O 5 Is not equal to the band gap width of (a)About 3.9-4.5eV, its dielectric constant: 20-22, thus being applicable to semiconductor devices such as thin film transistors, high electron mobility transistors, supercapacitors and the like as insulating dielectric materials. In particular Ta with hexagonal phase 2 O 5 The lattice structure of the material is similar to gallium nitride, and the material is a promising wide-bandgap oxide semiconductor material.
Ta 2 O 5 Powder materials (CN 105197996B) and film materials (Optical Materials,97 (2019) 109404) have been reported. Ta prepared by traditional methods such as sol-gel and radio frequency magnetron sputtering 2 O 5 Films that are often amorphous or polycrystalline in structure. Thin film Ta using heteroepitaxial growth 2 O 5 Materials have all been reported [ orthorhombic Ta ] 2 O 5 Epitaxial thin film: ceramics International,48 (2022) 26800-26805; hexagonal phase Ta 2 O 5 Epitaxial thin film: materials Science in Semiconductor Processing 135 (2021) 106065]。
The hexagonal phase tantalum pentoxide material prepared at present still has the following problems:
(1) For the currently growing hexagonal phase Ta 2 O 5 The single crystal substrate used for the thin film generally has a hexagonal phase Ta obtained at present due to a difference in lattice structure or a poor lattice match with the single crystal substrate 2 O 5 The epitaxial thin film generally contains a twin crystal structure, and has the problems of incomplete lattice structure, many lattice defects and poor crystallization quality. At present, ta with hexagonal phase is not adopted 2 O 5 Monocrystalline material with same lattice structure and good lattice matching as substrate for growing hexagonal phase Ta 2 O 5 Report of single crystal thin film.
(2) Ta of currently amorphous or polycrystalline structure 2 O 5 Thin film materials are commonly used as insulating dielectric layers in semiconductor devices. If a high quality hexagonal phase Ta is used 2 O 5 The monocrystalline film is used as an insulating medium layer, which is beneficial to reducing leakage current of the device and improving the integration level of the device, thereby improving the performance of the device.
(3) At present, ta is not available in hexagonal phase 2 O 5 Good lattice matchingA monocrystalline substrate material. In this case, it is difficult to obtain high-quality hexagonal phase Ta even with special equipment for producing single crystal thin films by Metal Organic Chemical Vapor Deposition (MOCVD), molecular Beam Epitaxy (MBE), or the like 2 O 5 Single crystal thin film material. This is hexagonal phase Ta without twinning and with complete structure which is not obtained at present 2 O 5 The reason for the importance of single crystal thin films.
(4) At present, the improvement of hexagonal phase Ta is not yet known 2 O 5 The research on the electrical properties of materials limits the application range of the materials in semiconductor devices. Thus, there is no twinning hexagonal phase Ta 2 O 5 The acquisition of high-quality monocrystalline film material is favorable for developing Ta 2 O 5 And the doping research of the film improves the electrical property of the film.
To sum up, find the hexagonal phase Ta 2 O 5 Lattice matched monocrystalline substrate material, research and preparation of hexagonal phase Ta with complete lattice structure 2 O 5 The monocrystalline film has important value for expanding the application of the monocrystalline film in the field of semiconductor devices. For this reason, the invention provides a high-quality hexagonal phase Ta based on lanthanum fluoride substrate 2 O 5 Method for preparing monocrystalline film, hexagonal phase Ta prepared by method 2 O 5 The monocrystalline film has complete lattice structure and no twin crystal.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a high-quality hexagonal phase tantalum pentoxide single crystal film based on a lanthanum fluoride substrate.
MOCVD: metalorganic chemical vapor deposition is a conventional technique in the art for preparing epitaxial monocrystalline films.
The invention adopts hexagonal phase lanthanum fluoride (LaF) 3 ) A single crystal wafer (lattice constant a=0.719 nm, c=0.737 nm) was used as an epitaxial substrate. Compared with hexagonal phase Ta 2 O 5 (lattice constant a=0.724nm, c= 1.161 nm), both of which are identical in lattice structure, and the lattice mismatch rate of the (0001) plane thereof is only 0.7%. Thus, laF 3 Is hexagonal phase Ta 2 O 5 Ideal heteroepitaxial substrate of monocrystalline film on which hexagonal phase Ta is epitaxially grown 2 O 5 The film not only has good lattice matching, but also does not generate twin crystal, and is obtained by high-quality hexagonal phase Ta 2 O 5 The key of the single crystal film. Preparation of hexagonal phase Ta by MOCVD technology 2 O 5 The film, the technology is suitable for the growth of epitaxial monocrystalline film, is one of the important conditions for preparing monocrystalline film. Tantalum ethoxide (C) 10 H 25 O 5 Ta) as a metal organic compound raw material, ultra-high purity nitrogen as a metal organic source carrier gas, high purity oxygen as an oxidizing gas, and a process for preparing the same in LaF 3 (0001) High temperature growth of Ta on monocrystalline substrates 2 O 5 A film. Under the proper growth temperature and deposition rate, the hexagonal phase Ta without twin crystal is successfully obtained 2 O 5 A single crystal thin film. The growth temperature of the thin film directly affects the crystallization quality of the thin film. Thin films cannot crystallize when the growth temperature is too low, while too high a growth temperature reduces the crystallization quality of the thin film.
The technical scheme of the invention is as follows:
a preparation method of a high-quality hexagonal phase tantalum pentoxide single crystal film based on a lanthanum fluoride substrate comprises the following steps of 2 O 5 The single crystal film is a single phase single crystal with a hexagonal structure; the specific preparation method adopts the conventional MOCVD preparation process of the oxide film.
The preparation method comprises the following steps:
according to the present invention, preferably, the hexagonal phase Ta 2 O 5 The growth substrate of the monocrystalline film is hexagonal phase lanthanum fluoride (LaF) 3 ) Single crystal plate with crystal face (0001).
According to the present invention, preferably, the MOCVD method grows hexagonal phase Ta 2 O 5 The temperature of the film is 760-860 ℃;
according to the present invention, preferably, the hexagonal phase Ta 2 O 5 The crystal growth surface of the monocrystalline film is hexagonal phase Ta 2 O 5 (0001)。
According to the invention, it is preferred that hexagonal phase Ta 2 O 5 Film and LaF 3 Out-of-plane and in-plane of the substrateThe epitaxy relationship is hexagonal phase Ta respectively 2 O 5 (0001)‖LaF 3 (0001) And hexagonal phase Ta 2 O 5 
‖LaF 3 />
According to the invention, the hexagonal phase Ta 2 O 5 A method for preparing a single crystal film by MOCVD method and TaC method 10 H 25 O 5 As a raw material of the metal organic compound, nitrogen is used as a carrier gas, oxygen is used as an oxidizing gas, and LaF 3 (0001) Growth of hexagonal phase Ta on monocrystalline substrates 2 O 5 Thin film, hexagonal phase Ta is obtained at a suitable growth temperature 2 O 5 A single crystal thin film.
According to the present invention, preferably, the MOCVD method prepares hexagonal phase Ta 2 O 5 The single crystal film has the following process conditions:
the pressure of the reaction chamber is 15-45 Torr;
the growth temperature is 760-860 ℃;
according to the invention, it is further preferred that the process conditions are as follows:
the pressure of the reaction chamber is 25Torr;
the growth temperature is 810 ℃;
according to the invention, preferably, the metal-organic tantalum source is tantalum ethoxide (TaC 10 H 25 O 5 ) The oxidizing gas is oxygen.
According to the invention, the substrate is preferably a hexagonal phase lanthanum fluoride single crystal plate with a crystal face of LaF 3 (0001)。
According to the invention, ta obtained by the preparation method 2 O 5 Is a monocrystal film with hexagonal structure, hexagonal phase Ta 2 O 5 The growth surface of (a) is hexagonal phase Ta 2 O 5 0001) plane of (b).
Hexagonal phase Ta prepared by the invention 2 O 5 The single crystal film has a plurality of unionsThe film has the advantages of high crystallization quality, complete lattice structure, no twin crystal existence, few defects and wide application prospect.
The invention is not described in detail and is carried out according to the state of the art.
Hexagonal phase Ta prepared by the invention 2 O 5 Film and existing Ta 2 O 5 The film has the following excellent effects:
1. hexagonal phase Ta of the invention 2 O 5 The film is a single crystal film having a hexagonal structure. Hexagonal phase Ta 2 O 5 The growth surface of the film is (0001), and the out-of-plane epitaxial relationship between the film and the substrate is Ta 2 O 5 (0001)‖LaF 3 (0001) The in-plane and in-plane retardation relationship is Ta 2 O 5 
‖LaF 3 />
2. Hexagonal phase Ta of the invention 2 O 5 The single crystal film has higher insulativity, is suitable for being used as an insulating medium material for manufacturing high-performance semiconductor devices, and is beneficial to reducing leakage current of the devices.
3. Hexagonal phase Ta of the invention 2 O 5 The film has a complete monocrystalline structure, no twin crystal structure exists, the film has few lattice defects, the improvement of doping efficiency is facilitated, and the hexagonal phase Ta is improved by doping in the later period 2 O 5 The study of electrical properties provides high quality single crystal thin films. Is hexagonal phase Ta 2 O 5 Single crystal thin films provide a strong support for the application of semiconductor devices.
Drawings
FIG. 1 shows the preparation of hexagonal phase Ta according to the invention 2 O 5 X-ray theta-2 theta scanning diffraction pattern of single crystal film. Wherein, the abscissa: 2θ (degrees), ordinate: intensity (arbitrary units).
FIG. 2 shows the preparation of hexagonal phase Ta according to the invention 2 O 5 Single crystal thinRocking curve of film (0001) plane X-ray diffraction peak. Wherein, the abscissa: omega (degree), ordinate: intensity (arbitrary units).
FIG. 3 shows the preparation of hexagonal phase Ta according to the invention 2 O 5 X-ray in situ phi scanning typical patterns of a monocrystalline film and a substrate, wherein (a) is LaF 3 Substrate and method for manufacturing the same
Diffraction spectrum of plane, (b) is hexagonal phase Ta 2 O 5 Film->
Diffraction spectrum of the facets. Wherein, the abscissa: Φ (degree), ordinate: intensity (arbitrary units).
FIG. 4 shows the preparation of hexagonal phase Ta according to the invention 2 O 5 High Resolution Transmission Electron Microscope (HRTEM) patterns of single crystal thin films.
Detailed Description
The present invention will be further described with reference to examples and comparative examples, but is not limited thereto.
A preparation method of a hexagonal phase tantalum pentoxide single crystal film comprises the following steps:
step (1) starting high-vacuum MOCVD equipment, pumping the reaction chamber into a high-vacuum state, and cleaning LaF 3 The monocrystalline substrate is placed on a reaction chamber base and heated to a growth temperature;
step (2) opening a nitrogen cylinder valve, and introducing N into the reaction chamber 2 The pressure of the reaction chamber is 10 to 40Torr;
opening an oxygen bottle valve and adjusting the oxygen flow;
opening a valve of the tantalum ethoxide source bottle, and adjusting the flow of the tantalum ethoxide source;
step (5), the gases in the steps (3) and (4) are simultaneously introduced into a reaction chamber to start growing a film, and the growing time is determined according to the thickness of the film;
step (6), closing valves of the tantalum ethoxide source bottle and the oxygen bottle, and ending the reaction; and naturally cooling after flushing the pipeline with nitrogen. Thereby preparing hexagonal phase Ta 2 O 5 Single crystal thinAnd (3) a film.
Example 1:
LaF with hexagonal phase 3 (0001) The single-chip is used as a substrate, tantalum ethoxide is used as a metal organic source, ultra-high purity nitrogen is used as carrier gas, high purity oxygen is used as oxidizing gas, and MOCVD technology is adopted to prepare hexagonal phase Ta 2 O 5 A film material.
The method comprises the following steps:
(1) The MOCVD reaction chamber is pumped into a high vacuum state, and the vacuum degree is 2 multiplied by 10 -4 Pa, laF 3 Placing a single crystal substrate in a reaction chamber and heating to 810 ℃;
(2) Opening a nitrogen cylinder valve, and introducing a background N into the reaction chamber 2 The pressure of the reaction chamber is 25Torr;
(3) Opening an oxygen bottle valve, and adjusting the oxygen flow to 55sccm;
(4) Opening a valve of a metal organic source bottle, and regulating the flow of tantalum ethoxide to be 3.0x10 -6 mol/min；
(5) Simultaneously introducing the oxygen in the step (3) and the tantalum ethoxide in the step (4) into a reaction chamber, wherein the holding time is 180 minutes; in LaF 3 (0001) Growth of hexagonal phase Ta on a substrate 2 O 5 A film;
(6) And after the reaction is finished, closing valves of the metal organic source bottle and the oxygen bottle, flushing a pipeline with nitrogen, and naturally cooling.
The film prepared in this example 1 is hexagonal phase Ta 2 O 5 Monocrystalline film, growth surface of the film is Ta 2 O 5 (0001). The out-of-plane epitaxial relationship between the film and the substrate is Ta 2 O 5 (0001)‖LaF 3 (0001) The in-plane and in-plane retardation relationship is Ta 2 O 5 
‖LaF 3 
Hexagonal phase Ta prepared 2 O 5 The lattice structure of the epitaxial monocrystalline film is complete, and no twin crystal structure exists.
Ta prepared by the invention 2 O 5 The X-ray theta-2 theta scanning diffraction pattern of the single crystal film is shown in figure 1. The 2 diffraction peaks of the film are located at 22.92 DEG and 46.95 DEG, respectively, corresponding to hexagonal phase Ta 2 O 5 (0001) And (0002) diffraction peaks (JCPSDSNO.19-1299), indicating that the film was prepared as hexagonal phase Ta 2 O 5 The structure, the growth surface is (0001).
Hexagonal phase Ta prepared by the invention 2 O 5 The rocking curve of the single crystal film (0001) plane X-ray diffraction peak is shown in fig. 2. The half width of the diffraction peak was only 0.7 °, and the symmetry was good, indicating that the film was a high quality single crystal film.
The monocrystalline film Ta prepared by the invention 2 O 5 
Surface and substrate LaF 3 />
A typical map of an in situ Φ scan of the face X-rays is shown in fig. 3. Ta 2 O 5 />
Surface and substrate LaF 3 />
The positions of the surface diffraction peaks are the same and correspond one to one, so that the determination can be made: the out-of-plane epitaxial relationship between the film and the substrate is hexagonal phase Ta 2 O 5 (0001)‖LaF 3 (0001) The in-plane and in-plane retardation relationship is Ta 2 O 5 />
LaF 3 />
And no twinning structure exists in the film.
Preparation of hexagonal phase Ta according to the invention 2 O 5 High Resolution Transmission Electron Microscope (HRTEM) pattern of single crystal thin film as shown in FIG. 4Shown. Ta is shown in the figure 2 O 5 The lattice arrangement of the monocrystalline film is neat, the relevant crystal face and included angle of the film are marked in the figure, and the Ta with hexagonal structure obtained by the invention is further proved 2 O 5 A single crystal thin film.
Example 2:
preparation of hexagonal phase Ta by MOCVD technology 2 O 5 A film. The substrate material and film preparation procedure used was the same as in example 1, except that the preparation temperature was 860 ℃. The prepared film is hexagonal phase Ta 2 O 5 The growth surface and lattice structure of the prepared film were the same as in example 1. However, the film crystallization quality was slightly lowered and the film roughness of the film was significantly increased as compared with example 1.
Example 3:
preparation of hexagonal phase Ta by MOCVD technology 2 O 5 A film. The substrate material and film preparation procedure used was the same as in example 1, except that the growth temperature was 760 ℃. The prepared film is hexagonal phase Ta 2 O 5 The growth surface and lattice structure of the prepared film were the same as in example 1. However, the crystallization quality of the prepared film is remarkably reduced compared with example 1 due to the lower substrate temperature.
Example 4:
ta is prepared by MOCVD technology 2 O 5 A film. The substrate material and film preparation procedure used was the same as in example 1, except that the growth temperature was 660 ℃. Since the temperature required for crystallization of the film was not reached, the prepared film did not measure a significant X-ray diffraction peak, indicating that the film did not form a significant crystalline structure.
Comparative example 1:
the substrate materials and film preparation process conditions used were as described in example 1, except that: a yttrium-doped zirconia (YSZ, cubic structure) single crystal plate is adopted as a substrate, the crystal face is (111), and the film growth temperature is 800 ℃. Ta produced 2 O 5 The film is hexagonal phase Ta 2 O 5 Epitaxial film with hexagonal Ta epitaxial growth surface 2 O 5 (0001) II cube YSZ (111), in-planeEpitaxial relationship is Ta 2 O 5 
‖YSZ/>
Due to the cubic structure of the YSZ substrate and the hexagonal structure of Ta 2 O 5 The lattice structures of the films are different, so that the prepared hexagonal Ta 2 O 5 The film has a double twin structure.
Comparative example 2:
the film preparation process conditions were as described in example 1, except that: by using sapphire with C-plane (alpha-Al) 2 O 3 ) (0001) the single-crystal wafer is the substrate material, and the growth temperature is 750 ℃. Ta produced 2 O 5 The film is hexagonal phase Ta 2 O 5 Epitaxial film with epitaxial growth surface of Ta 2 O 5 
The in-plane and in-plane retardation relationship is Ta 2 O 5 />
‖Al 2 O 3 />
The thin film has a triple domain structure, and twin crystals exist in the thin film.
Comparative example 3:
the film preparation process conditions used were as described in comparative example 2, except that: the substrate adopts gallium nitride epitaxial wafer (epi-GaN/alpha-Al 2 O 3 ) The epitaxial crystal face of GaN is (0001), ta 2 O 5 The growth temperature of the film was 850 ℃. Ta produced 2 O 5 The film is orthorhombic Ta 2 O 5 Epitaxial film with film growth surface of orthorhombic phase Ta 2 O 5 (001) The thin film has a triple twin structure in which twin crystals exist.
Comparative example 4:
the film preparation process conditions were as described in example 1, except that: yttrium Vanadate (YVO) having tetragonal structure 4 ) The single-chip wafer (100) is used as a substrate, and the growth temperature is 850 ℃. Ta produced 2 O 5 The film is of hexagonal structure Ta 2 O 5 Film with growth surface of Ta 2 O 5 (0001) But the film contains a triple twin structure.
Claims (8)
1. A preparation method of a hexagonal phase tantalum pentoxide single crystal film is characterized by comprising the following steps: adopts an organic metal chemical vapor deposition process to prepare tantalum TaC ethanol 10 H 25 O 5 Using nitrogen as carrier gas, oxygen as oxidizing gas, and MOCVD equipment to grow hexagonal phase tantalum pentoxide monocrystal film on lanthanum fluoride substrate wafer;
the preparation method comprises the following specific steps:
starting high-vacuum MOCVD equipment, and pumping the reaction chamber into a high-vacuum state; placing an ultrasonic-cleaned lanthanum fluoride LaF3 (0001) surface single-crystal wafer substrate on a substrate base station in a reaction chamber and heating to a growth temperature;
setting the pressure of the reaction chamber, opening a nitrogen cylinder valve, and introducing a background N into the reaction chamber 2 And keep the flow stable;
opening an oxygen bottle valve, adjusting the oxygen flow and keeping the flow stable;
opening a valve of the tantalum ethoxide source bottle, adjusting the flow of tantalum ethoxide steam and keeping the flow stable;
step (5) oxygen in the step (3) and tantalum ethoxide steam in the step (4) are simultaneously introduced into a reaction chamber; ta on epitaxial substrate 2 O 5 The growth rate of the film is 0.2-1.2 nm/min;
closing valves of the tantalum ethoxide source bottle and the oxygen bottle after the reaction in the step (6) is finished, flushing a pipeline with nitrogen, closing the nitrogen bottle valve and naturally cooling; preparing hexagonal phase Ta 2 O 5 A single crystal thin film.
2. A hexagonal phase pentoxide according to claim 1The preparation method of the tantalum monocrystal film is characterized by comprising the following steps of: the hexagonal phase Ta 2 O 5 The single crystal film is Ta with hexagonal structure and single phase 2 O 5 A single crystal thin film.
3. The method for preparing the hexagonal phase tantalum pentoxide single crystal film according to claim 1, wherein the method comprises the following steps: the hexagonal phase Ta 2 O 5 The growth substrate of the monocrystalline film is lanthanum fluoride (LaF) 3 ) (0001) planar substrate single crystal wafer.
4. The method for preparing the hexagonal phase tantalum pentoxide single crystal film according to claim 1, wherein the method comprises the following steps: hexagonal phase Ta 2 O 5 Film and LaF 3 The epitaxial relationship between the out-of-plane and in-plane of the substrate is hexagonal phase Ta respectively 2 O 5 (0001)‖LaF 3 (0001) And hexagonal phase
5. The method for preparing the hexagonal phase tantalum pentoxide single crystal film according to claim 1, wherein the method comprises the following steps: the MOCVD method prepares hexagonal phase Ta 2 O 5 The single crystal film has the following process conditions:
the pressure of the reaction chamber is 10-40 Torr;
the growth temperature is 800-900 ℃;
background N 2 The flow is 80-160 sccm;
the oxygen flow is 30-70 sccm;
tantalum ethoxide TaC 10 H 25 O 5 Flow 1.0X10 -6 ～6.0×10 -6 Mole/min;
Ta 2 O 5 the growth rate of the film is 0.2-1.2 nm/min.
6. The method for preparing the hexagonal phase tantalum pentoxide single crystal film according to claim 1, wherein the method comprises the following steps: the process conditions are as follows:
the pressure of the reaction chamber is 20Torr;
the growth temperature is 850 ℃;
background N 2 The flow rate is 120sccm;
oxygen flow rate 50sccm;
tantalum ethoxide flow rate 3.1X10 -6 mol/min。
7. The method for preparing the hexagonal phase tantalum pentoxide single crystal film according to claim 1, wherein the method comprises the following steps: the metal organic tantalum source is tantalum ethoxide TaC 10 H 25 O 5 The oxidizing gas is oxygen; the substrate is lanthanum fluoride (LaF) 3 ) (0001) planar substrate single crystal wafer.
8. The method for preparing the hexagonal phase tantalum pentoxide single crystal film according to claim 1, wherein the method comprises the following steps: ta obtained by the preparation method 2 O 5 Is a monocrystal film with hexagonal structure, hexagonal phase Ta 2 O 5 The growth surface of (a) is hexagonal phase Ta 2 O 5 0001) plane of (b).
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