CN113957531B - High-quality ilmenite structure zinc metatitanate single crystal film and preparation method and application thereof - Google Patents

High-quality ilmenite structure zinc metatitanate single crystal film and preparation method and application thereof Download PDF

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CN113957531B
CN113957531B CN202111219940.6A CN202111219940A CN113957531B CN 113957531 B CN113957531 B CN 113957531B CN 202111219940 A CN202111219940 A CN 202111219940A CN 113957531 B CN113957531 B CN 113957531B
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metatitanate
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CN113957531A (en
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栾彩娜
马瑾
张彪
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Shandong University
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Abstract

The invention relates to a high-quality ilmenite structure zinc metatitanate single crystal film, a preparation method and application thereof. The zinc metatitanate target is used as a raw material and is prepared in a substrate by adopting a pulse laser deposition mode. The zinc metatitanate single crystal film has complete internal lattice arrangement, few defects, no twin crystal structure, relative average transmittance in a visible light region of over 95 percent, and wide application prospect in the field of transparent optoelectronic devices.

Description

High-quality ilmenite structure zinc metatitanate single crystal film and preparation method and application thereof
Technical Field
The invention relates to a high-quality ilmenite structure zinc metatitanate single crystal film and a preparation method thereof, belonging to the technical field of semiconductor photoelectric materials.
Background
In recent years, with the development of semiconductor technology, wide band gap oxide semiconductor materials have become one of the hot spots of research. Ternary oxide zinc metatitanate (ZnTiO)3) The oxide semiconductor material is a functional material with wide application, has the advantages of zinc oxide and titanium oxide, and has excellent photoelectric properties, so the oxide semiconductor material is a potential oxide semiconductor material. The zinc metatitanate has two structures of cubic ilmenite and hexagonal ilmenite, the band gap width of the zinc metatitanate is about 3.2-3.7eV at room temperature, and the zinc metatitanate is a wide-bandgap semiconductor material. ZnTiO 2 3Due to the excellent photoelectric property and high specific surface area, the nano-composite material has potential application value in the aspects of photocatalysis, gas sensors, dye-sensitized solar cells, pigment coatings, microwave dielectrics, nonlinear optics and the like.
The preparation method of the zinc metatitanate material reported at present mostly adopts chemical methods such as solution, sol-gel and the like, and the prepared zinc metatitanate is mostly in the form of powder and nanocrystalline structure, for example, the publication number is CN 104498033A. Only a few reports have been made on the production of a metatitanic acid film by magnetron sputtering and laser pulse deposition (PLD) [ Journal of applied physics,2009,106(3): 033520-4; thin Solid Films,2010,518: 7366-7371; superlatices and microstuctures, 2016,92: 308-315-]. However, ZnTiO reported in the literature3The film is of a polycrystalline structure. At present, no reports on the zinc metatitanate single crystal thin film exist.
The currently prepared zinc metatitanate material still has the following problems:
(1) the zinc metatitanate prepared at present is mostly in three forms of powder, a nano structure and a polycrystalline film, the crystalline phase of the material is usually a mixed-phase polycrystalline structure and a single-phase polycrystalline structure, and the problems of poor crystalline quality, more defects and the like exist. At present, the report of the zinc metatitanate single crystal thin film material is not seen.
(2) The research on zinc metatitanate mostly improves the photocatalytic performance, dielectric performance and the like of the material, and the research on the photoelectric properties of semiconductors is lacked. The lack of high-quality zinc metatitanate film restricts the application of the zinc metatitanate film in the field of semiconductor photoelectric devices.
(3) The preparation of the zinc metatitanate single crystal film requires a proper single crystal film preparation technology process and a single crystal substrate material matched with the single crystal film preparation technology process. The substrate material for growing the zinc metatitanate film reported at present is SiO2the/Si and ITO substrates, little consideration is given to the lattice mismatch between the film and the substrate. Therefore, a suitable substrate material for growing the zinc metatitanate single crystal thin film is needed to be found.
(4) In the manufacture of zinc metatitanate-based semiconductor devices, there is a need for zinc metatitanate thin film materials that achieve superior electrical properties by doping on the basis of high quality zinc metatitanate single crystal thin films.
To sum up the limitation in the research field of zinc metatitanate film materials, the high-quality ZnTiO is developed and prepared3The single crystal film has important significance in expanding the application of the single crystal film in the field of semiconductor photoelectric devices. The invention is therefore proposed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-quality ilmenite zinc metatitanate single crystal film and a preparation method thereof.
Interpretation of terms:
PLD: pulsed laser deposition, as is conventional in the art.
Summary of the invention:
the invention adopts the Pulsed Laser Deposition (PLD) technology to prepare the zinc metatitanate film. The raw material is a high-purity zinc metatitanate ceramic target which is a conventional commercial product and is sold by Taizhou Senno material science and technology company Limited. The target material is ZnTiO with the purity of 99.99 percent3The powder is formed by pressing and sintering at high temperature, and the diameter of the target material is 5.5 cm. The substrate material is single crystal lithium niobate (LiNbO)3) The (006) crystal plane of (c). The preparation method is that the high-purity zinc metatitanate target material is bombarded by pulse laser to form zinc metatitanate plasma, and the plasma is directionally and locally expanded and emitted in a reaction chamberAnd depositing and growing a zinc metatitanate film on the substrate. When the substrate temperature reaches the temperature suitable for the growth of the zinc metatitanate, the high-quality ilmenite zinc metatitanate single crystal film is obtained. The invention successfully prepares the high-quality ilmenite zinc metatitanate single crystal film by optimizing raw materials, a substrate and PLD process conditions.
The technical scheme of the invention is as follows:
a zinc metatitanate single crystal film has a chemical composition of zinc metatitanate, a hexagonal ilmenite structure single crystal material.
According to the invention, the crystal growth surface of the zinc metatitanate monocrystal film is ZnTiO 3(003) The crystal lattice structure in the film is complete and twin crystals are not generated.
According to the invention, the ilmenite zinc metatitanate film has a complete structure and regular lattice arrangement, and the average transmittance of the ilmenite zinc metatitanate film relative to a substrate in a visible light region exceeds 95%, so that a perfect single crystal film is provided for the effective doping of a zinc metatitanate material, and the research of the zinc metatitanate material in the field of semiconductor photoelectric devices is laid.
According to the invention, preferably, the zinc metatitanate single crystal film is prepared in a substrate by adopting a pulsed laser deposition mode and taking a zinc metatitanate target as a raw material;
preferably, the substrate is made of lithium niobate, and the in-plane and out-of-plane epitaxial relationship 110 between the zinc metatitanate thin film and the lithium niobate substrate]//LiNbO3[2110]And ZnTiO3(003)//LiNbO3(006)。
According to the present invention, the method for producing the zinc metatitanate single crystal thin film comprises the steps of:
the zinc metatitanate single crystal film is prepared on a substrate by taking a zinc metatitanate target material as a raw material and adopting a pulse laser deposition mode.
According to the present invention, preferably, the substrate is a lithium niobate substrate having a hexagonal structure; further preferably, the (006) crystal plane of lithium niobate having a hexagonal structure. The lattice mismatch ratio of the crystal faces of the zinc metatitanate and the lithium niobate (006) is the smallest and is 1.367 percent. The substrate plays a very important role in the epitaxial growth of the thin film, and the selection of a proper substrate for growing the single crystal thin film is very important.
According to the present invention, preferably, the laser parameter conditions during the pulsed laser deposition process are:
laser single pulse energy is 150-400 mJ
Laser burst length of 20ns
The pulse frequency is 1 to 20 Hz.
According to the present invention, preferably, the parameter conditions of the reaction chamber during the pulsed laser deposition process are:
the pressure of the reaction chamber is 1-20 Pa
The substrate temperature is 500-900 DEG C
The flow rate of the oxygen is 10-20 sccm.
According to the invention, the technological parameters of preparing the zinc metatitanate single crystal film by pulsed laser deposition are as follows:
Figure BDA0003312193100000031
under the preparation process conditions, the deposition time is 120 minutes, and the growth rate of the zinc metatitanate film is 1-2.5 nm/minute.
According to the invention, most preferably, the process parameters for preparing the zinc metatitanate single crystal film by pulsed laser deposition are as follows:
Figure BDA0003312193100000032
under the above preparation conditions, the deposition time was 120 minutes, and the growth rate of the zinc metatitanate film was 1.75 nm/min.
According to the present invention, a method for producing a zinc metatitanate single crystal thin film, a preferred embodiment, comprises the steps of:
(1) firstly, putting a lithium niobate substrate into a water bath container at 80 ℃, and cleaning for 10 minutes by using an ultrasonic cleaner; then, drying the surface of the substrate by using a high-purity nitrogen gun;
(2) LiNbO is reacted with 3(006) The substrate and the zinc metatitanate target are respectively arranged at the position of the base and the target in the reaction chamberThe reaction chamber is closed. The molecular pump is turned on, the reaction chamber is pumped to high vacuum with the vacuum degree of 1X 10-4Pa～8×10-5Pa, heating the substrate base to 650-750 ℃;
(3) opening a high-purity oxygen bottle, introducing oxygen into the reaction cavity, controlling the flow of the oxygen to be 15-25 sccm by using a gas flow meter, adjusting a valve of the reaction cavity, stabilizing the pressure of the reaction cavity at 2-10 Pa, and keeping the pressure for 20-30 minutes;
(4) and starting the laser, adjusting the laser to be in an energy stable mode, wherein the single pulse energy is 200-300 mJ, the burst length is 20ns, and the laser pulse frequency is 2-10 Hz. Starting a laser to perform pre-deposition for 10 minutes, and removing the attachments on the surface of the target;
(5) after the pre-deposition is finished, formal deposition is carried out for 120 minutes in LiNbO3(006) Epitaxial growth of ZnTiO on substrate3The epitaxial growth rate of the film is 1-2.5 nm/min;
(6) and after the deposition reaction is finished, closing the high-purity oxygen cylinder valve, closing the laser, closing the molecular pump, opening the reaction chamber and taking out the sample.
According to the invention, the zinc metatitanate single-crystal film is prepared by the process method.
According to the invention, the application of the zinc metatitanate single crystal thin film in the preparation of a transparent oxide semiconductor photoelectric device is also provided.
The invention has not been described in detail, but is in accordance with the state of the art.
The zinc metatitanate single crystal film prepared by the invention has unique advantages in structure, the crystal lattice structure of the film is complete, and twin crystals do not exist in the film. At present, no zinc metatitanate single crystal film is reported.
The zinc metatitanate single crystal film prepared by the technical method has good uniformity and repeatability, and is an advantageous film epitaxial growth technical method.
ZnTiO prepared by the invention3Film and ZnTiO of the prior art3Compared with the thin film, the film has the following advantages in structural and optical properties:
1. ZnTiO of the invention3The film is a monocrystal film with ilmenite hexagonal structure, and a crystal face growsIs ZnTiO3(003). Preferred substrates are LiNbO3(006) The substrate can obtain a single crystal film, and the ZnTiO is successfully prepared at the preferable substrate temperature of 700 DEG C3A single crystal thin film. The full width at half maximum of the rocking curve of the (003) plane of the film was as low as 0.047 °, indicating that the film had a high crystalline quality. ZnTiO 23Thin film and LiNbO3The out-of-plane epitaxial relationship of the substrate is ZnTiO3(003)//LiNbO3(006)。
2. ZnTiO of the invention3Film {119} plane and LiNbO3As can be seen from the results of the X-ray in-situ phi scan of the {116} plane of the substrate, 110]//LiNbO3[2110]。
3. The film structure representation result shows that the internal crystal lattice arrangement of the film is complete, the defects are few, and a twin crystal structure is avoided, so that a solid foundation is laid for manufacturing the zinc metatitanate based photoelectric device.
4. ZnTiO prepared by the invention3The relative average transmittance of the single crystal film in a visible light region can reach more than 95 percent, which shows that the film material has wide application prospect in the field of transparent optoelectronic devices.
Drawings
FIG. 1 shows ZnTiO compound of example 13X-ray theta-2 theta scanning diffraction pattern of the film.
FIG. 2 shows ZnTiO compound of example 13Rocking curve of diffraction peak of film (003).
FIG. 3 shows ZnTiO compound in example 13Film {119} and LiNbO3X-ray in-situ phi scan pattern of the {116} plane of the substrate.
FIG. 4 shows ZnSnO in example 13The transmission spectrum of the film sample has the abscissa (wavelet/nm) as Wavelength/nm and the ordinate (transmittince/%) as Transmittance/%.
Detailed Description
The invention is further described below by reference to the drawings, examples and comparative examples, but is not limited thereto.
The raw material used in the examples was a high purity zinc metatitanate ceramic target material, which is a conventional commercially available product available from texas knono materials technologies ltd.
Example 1:
with LiNbO3(006) Is taken as a substrate, 99.99 percent of ceramic target is taken as a target material, and the PLD technology is adopted to prepare the zinc metatitanate film.
The method comprises the following steps:
(1) mixing clean LiNbO3(006) The substrate and the zinc metatitanate target are respectively placed at the position of the base and the target in the reaction chamber, and the reaction chamber is closed. The molecular pump is turned on, the reaction chamber is pumped to high vacuum with the vacuum degree of 8.5X 10 -5Pa, heating the substrate base to 700 ℃;
(2) opening a high-purity oxygen bottle, introducing oxygen into the reaction cavity, controlling the oxygen flow to be 20sccm by using a gas flow meter, adjusting a valve of the reaction cavity, stabilizing the pressure of the reaction cavity at 5Pa, and keeping the pressure for 30 minutes;
(3) and (3) starting the laser, adjusting the laser to be in an energy stable mode, wherein the single pulse energy is 200mJ, the burst length is 20ns, and the laser pulse frequency is 4 Hz. Starting a laser to carry out pre-deposition for 10 minutes, and removing attachments on the surface of the target;
(4) after the pre-deposition is finished, formal deposition is carried out for 120 minutes in LiNbO3(006) Epitaxial growth of ZnTiO on substrate3A film having an epitaxial growth rate of 1.75 nm/min;
(5) and after the deposition reaction is finished, closing the high-purity oxygen cylinder valve, closing the laser, closing the molecular pump, opening the reaction chamber after the sample is naturally cooled to room temperature, and taking out the sample.
ZnTiO prepared in example 13The film is a single crystal film, the X-ray theta-2 theta scanning diffraction pattern is shown in figure 1, and as can be seen from figure 1, only ZnTiO appears except the diffraction peak of the lithium niobate substrate3(003) diffraction Peak of film, indicating that film is along [003 ]]The single orientation growth, the out-of-plane epitaxial relationship between the film and the substrate is ZnTiO3(003)// LiNbO3 (006).
ZnTiO prepared in example 13The rocking curve of the diffraction peak of the thin film (003) is shown in FIG. 2. from FIG. 2, it can be seen that the X-ray rocking curve has very good symmetry and the full width at half maximum of the curve is as low as 0.047, indicating that the thin film has excellent crystalline quality.
ZnTiO produced in this example3Film {119} and LiNbO3The X-ray in-situ phi scan pattern of the {116} plane of the substrate is shown in FIG. 3. For a complete hexagonal crystal, the family of crystal planes of thin film ZnTiO3{119} is hexagonally symmetric with respect to the (001) crystal plane, as is the family of crystal planes of substrate LiNbO3{116 }. As can be seen from fig. 3, of the film and the substrate
Figure BDA0003312193100000051
The diffraction peaks scanned correspond one-to-one, indicating a thinness of 110]//LiNbO3[2110]。
ZnTiO compound obtained in this example3The transmission spectrum of the film sample is shown in fig. 4, and as can be seen from fig. 4, the relative average transmittance of the film in the visible light region exceeds 95%, and the calculated optical band gap of the film is 3.72eV, which indicates that the zinc metatitanate film has great application prospects in the field of transparent wide-band-gap oxide semiconductors.
Example 2:
preparation of ZnTiO by PLD technology3The single crystal thin film, the target and the substrate used and the production process were the same as in example 1 except that the substrate temperature was 650 ℃. ZnTiO prepared in this example3The film had a single epitaxial orientation of the (003) plane, but in comparison with example 1, ZnTiO 3(003) The diffraction peak intensity of the crystal face is reduced, and the full width at half maximum is also increased, which shows that the quality of the film single crystal prepared at the substrate temperature is reduced.
Example 3:
preparation of ZnTiO by PLD technology3The single crystal thin film, the target and the substrate used and the production process were the same as in example 1 except that the substrate temperature was 750 ℃. ZnTiO prepared in this example3The film had a single epitaxial orientation of the (003) plane, and the variation in the peak width of the diffraction peak of the (003) plane of the film as compared with example 1 all indicated that the crystal quality of the film was degraded.
Example 4:
as described in example 1, except that:
the parameter conditions of the pulse laser are as follows: the single pulse energy was 200mJ, the pulse frequency was 2Hz, and the burst length was constant.
Example 5:
as described in example 1, except that:
the parameter conditions of the pulse laser are as follows: the single pulse energy was 200mJ, the pulse frequency was 10Hz, and the burst length was constant.
Comparative example 1:
preparation of ZnTiO by PLD technique3A film. The target material and preparation were as described in example 1, except that sapphire (001) was used as the substrate. ZnTiO prepared under the condition3The film was a polycrystalline film and had a relative average transmittance in the visible light region of about 75%.
Comparative example 2:
Preparation of ZnTiO by PLD technique3A film. The target material and preparation were as described in example 1, except that lithium tantalate (001) was used as the substrate. ZnTiO prepared under the condition3The film was a polycrystalline film and had a relative average transmittance in the visible light region of about 85%.
Comparative example 3:
preparation of ZnTiO by PLD technique3A film. The target materials used and the preparation were as described in example 1, except that quartz (001) was used as the substrate. ZnTiO prepared under the condition3The film was a polycrystalline film and had a relative average transmittance in the visible light region of about 75%.
Comparative example 4:
preparation of ZnTiO by PLD technique3A film. The target material used and the preparation were as described in example 1, except that the pulse laser had a single pulse energy of 300 mJ. The laser has large energy and the film growth speed is too fast, and the ZnTiO prepared under the condition3The film is a polycrystalline film, and has a relative average transmittance in the visible light region of about 90%.

Claims (6)

1. The zinc metatitanate single crystal film is characterized in that the chemical composition of the film is single crystal material with a zinc metatitanate and hexagonal ilmenite structure, and the crystal growth surface of the zinc metatitanate single crystal film is ZnTiO3（003）。
2. The zinc metatitanate single crystal film according to claim 1, wherein the zinc metatitanate single crystal film is prepared in a substrate by a pulsed laser deposition method using a zinc metatitanate target as a raw material.
3. The zinc metatitanate single crystal film according to claim 2, wherein the substrate is made of lithium niobate, and the epitaxial relationship of film growth is ZnTiO3 (003) // LiNbO3 (006)。
4. The method for producing a zinc metatitanate single crystal thin film according to claim 1, comprising the steps of:
preparing a zinc metatitanate single-crystal film on a (006) crystal face of lithium niobate with a hexagonal structure by taking a zinc metatitanate target as a raw material and adopting a pulse laser deposition mode;
the parameter conditions of the laser in the pulse laser deposition process are as follows:
laser single pulse energy is 150~200 mJ
Laser burst length 20 ns
The pulse frequency is 1-20 Hz;
the parameter conditions of the reaction chamber in the pulse laser deposition process are as follows:
the pressure of the reaction chamber is 1-20 Pa
The substrate temperature is 650-750 DEG C
The flow rate of the oxygen is 10-20 sccm.
5. The method for preparing a single-crystal zinc metatitanate film according to claim 4, wherein the pulsed laser deposition process for preparing the single-crystal zinc metatitanate film has the following parameters:
laser single pulse energy is 150~200 mJ
Laser burst length of 20 ns
The pulse frequency is 2-10 Hz
The pressure of the reaction chamber is 2-10 Pa
The substrate temperature is 650-750 DEG C
The oxygen flow is 15-20 sccm;
under the preparation process conditions, the deposition time is 120 minutes, and the growth rate of the zinc metatitanate film is 1-2.5 nm/minute.
6. Use of the zinc metatitanate single crystal thin film according to claim 1 for the production of a transparent oxide semiconductor optoelectronic device.
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JP2012140673A (en) * 2010-12-28 2012-07-26 Sumitomo Chemical Co Ltd Zinc oxide based transparent conductive film forming material, method for producing the material, target using the material, and method for forming zinc oxide based transparent conductive film
CN107287563A (en) * 2016-03-31 2017-10-24 中国科学院上海硅酸盐研究所 A kind of extension stronitum stannate cobalt thin film and preparation method thereof
CN110172733A (en) * 2019-06-20 2019-08-27 山东大学 A kind of high quality zinc stannate monocrystal thin films and preparation method thereof
CN112941631A (en) * 2021-01-18 2021-06-11 山东大学 Zinc orthotitanate single crystal film and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JP2012140673A (en) * 2010-12-28 2012-07-26 Sumitomo Chemical Co Ltd Zinc oxide based transparent conductive film forming material, method for producing the material, target using the material, and method for forming zinc oxide based transparent conductive film
CN107287563A (en) * 2016-03-31 2017-10-24 中国科学院上海硅酸盐研究所 A kind of extension stronitum stannate cobalt thin film and preparation method thereof
CN110172733A (en) * 2019-06-20 2019-08-27 山东大学 A kind of high quality zinc stannate monocrystal thin films and preparation method thereof
CN112941631A (en) * 2021-01-18 2021-06-11 山东大学 Zinc orthotitanate single crystal film and preparation method thereof

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