CN113279063A - IV-VI family infrared semiconductor film and preparation method thereof - Google Patents

IV-VI family infrared semiconductor film and preparation method thereof Download PDF

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CN113279063A
CN113279063A CN202110441818.7A CN202110441818A CN113279063A CN 113279063 A CN113279063 A CN 113279063A CN 202110441818 A CN202110441818 A CN 202110441818A CN 113279063 A CN113279063 A CN 113279063A
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infrared semiconductor
group
semiconductor film
substrate
family
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王启胜
王立
吴识腾
王震东
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Nanchang University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention discloses a method for preparing an IV-VI group infrared semiconductor film, which adopts a gas phase epitaxy method for preparation, and takes a compound containing IV-VI group elements as a reaction source, wherein the reaction source can also contain VI group simple substance materials, a crystal substrate which is matched with the IV-VI group infrared semiconductor crystal in lattice symmetry is taken as a substrate, argon is taken as carrier gas, the temperature of the VI group simple substance reaction source is 500-plus-materials, the temperature range of the IV-VI group compound reaction source is 600-plus-materials 1000 ℃, the temperature range of the substrate is 600-plus-materials 600 ℃, and the growth time is not less than 6 minutes. The invention also discloses the IV-VI group infrared semiconductor film prepared by the method, which comprises PbS, PbSe, PbTe and Pb1‑ xSnxS、Pb1‑xSnxSe、Pb1‑xSnxTe thin film, wherein x represents atomic percent, the substrate of the IV-VI group infrared semiconductor thin film is matched with the IV-VI group infrared semiconductor crystal lattice symmetryA crystalline substrate. The preparation method has the advantages of low cost, simplicity, convenience, practicability and high efficiency, and the prepared IV-VI family infrared semiconductor film has high crystallization quality, low defect density and uniform surface.

Description

IV-VI family infrared semiconductor film and preparation method thereof
Technical Field
The invention belongs to the technical field of photoelectron semiconductor materials, and particularly relates to an IV-VI family infrared semiconductor film and a preparation method thereof.
Background
Group IV-VI semiconductors are an important class of semiconductor materials, including PbS, PbSe, PbTe, Pb1-xSnxS、Pb1- xSnxSe、Pb1-x SnxTe (x represents atomic percent), etc., which are used as windows of infrared detectors in the form of single crystals or polycrystals. The application of the infrared semiconductor still has the problems of complex preparation process, low crystal quality and the like. This severely limits the applications of such infrared semiconductors. It is well known that defects, impurities, etc. are major factors affecting the photoelectric properties of semiconductor materials. A large number of defects are detrimental to the transport of carriers and reduce the performance of the device. Particularly, the IV-VI family infrared semiconductor has a narrow direct band gap, so that the thermal energy and the transition energy of charge carriers are comparable at the temperature close to room temperature, thereby enabling thermal transition, and the thermal transition is used as a semiconductor material of an infrared photon detector, so that the noise is heavy and the noise ratio is low. Therefore, the preparation method of the high-quality IV-VI family infrared semiconductor is particularly important for the application thereof.
Common IV-VI infrared semiconductor preparing processes include chemical bath deposition, electrochemical deposition, continuous ion layer adsorption reaction, sol-gel process, molecular beam epitaxy, etc. As a standard process for preparing the lead salt film, the technology for preparing the IV-VI semiconductor by a chemical bath deposition method (CBD) is mature, and the high-sensitivity IV-VI semiconductor infrared detector can be obtained by assisting a sensitization process, so that the severe requirements of the military field on the device performance are met. However, the IV-VI semiconductor film prepared by the method has the problems of complex process, rough film surface, poor uniformity, high manufacturing cost, poor repeatability controllability, difficulty in realizing large-area preparation and the like.
Electrochemical deposition, namely, metal ions or metal simple substances are formed by discharging metal ions in the solution near the cathode, the metal simple substances can be directly deposited on the cathode through electric crystallization, and the lower-valence metal ions are deposited on the cathode through combining with cations in the solution to form precipitates. The method has low cost and does not generate toxic gas, but the discharge rate is slow due to the principle of the primary battery, so that the growth rate of the film is slow, the film is greatly influenced by temperature, and the crystal quality is not high.
The continuous ion layer adsorption method is a chemical film-forming technology developed on the basis of a chemical bath deposition method and atomic layer epitaxial growth, and adopts an independent ion precursor to ensure that a cluster of precipitates cannot be formed in a solution, so that the influence of a homogeneous deposition mechanism is avoided, and a film with good uniformity and high density is obtained under the control of a heterogeneous deposition mechanism. Although this method can deposit a film over a large area, the growth rate is slow and the yield is difficult to control.
The sol-gel method is to dissolve metal alkoxide or other salts in an organic solvent such as alcohol or ether to form a uniform solution, the solution is hydrolyzed and polycondensed to form a sol, further polymerization is carried out to form a gel through a sol-gel reaction, and the gel is heat-treated to remove the remaining organic substances and water, thereby finally forming a desired thin film. The method is expensive and requires a long time for the sol-gel process.
The molecular beam epitaxy is realized by epitaxially growing a crystal film on a crystal substrate under ultrahigh vacuum by accurately controlling molecular beams and atomic beam flows, and has the advantages of low growth temperature, capability of avoiding impurity diffusion caused by high-temperature growth and capability of obtaining abrupt interface impurity distribution; the thickness of the epitaxial film can be accurately controlled; since the substrate can be rotated, uniformity of the epitaxial thin film can be ensured. Its disadvantages are high maintenance and equipment cost, slow growth rate, and not good for mass production. For the preparation of group IV-VI semiconductor thin films, PbSe, PbTe and BaF with lattice constant similar to that of PbTe are commonly used2As a substrate, however, PbTe single crystals themselves have problems of non-uniform composition, high defect density, etc. due to PbSe, and the crystal quality of the resulting thin films is not satisfactory. For using BaF2As a substrate, although the crystallization quality can be further improved, a plurality of V-shaped defects are distributed on the surface of the film, and the performance of the film is seriously influenced.
In view of the above consideration, it is of great significance to develop a preparation method of IV-VI infrared semiconductor film with low cost, simplicity, convenience, high crystallization quality and low defect density.
Disclosure of Invention
Aiming at the defects and problems in the prior art, the invention aims to provide an IV-VI family infrared semiconductor film and a preparation method thereof.
The invention is realized by the following technical scheme:
the invention also provides a preparation method of the IV-VI family infrared semiconductor film, which adopts a gas phase epitaxy method for preparation, and the method takes a compound containing IV-VI family elements as a reaction source, takes a crystal substrate which is matched with the IV-VI family infrared semiconductor crystal in lattice symmetry as a substrate, takes argon as a carrier gas, and has the temperature range of 600-600 ℃ and 600 ℃ as the reaction source of the IV-VI family compound, and the growth time of not less than 6 minutes as the substrate temperature range of 300-600 ℃.
Further, the reaction source includes a pharmaceutical product containing group IV elements of Pb and Sn and group VI elements of S, Se and Te.
Furthermore, the reaction source can also be a combination of a VI group simple substance material and a compound containing IV-VI group elements, namely the reaction source can be any combination of S powder + Pb powder, Se powder + Pb powder and Te powder + Pb powder, or only PbS powder, PbSe powder and PbTe powder are used; when the reaction source comprises a VI group elementary substance material, the reaction temperature range of the VI group elementary substance reaction source is 100-500 ℃.
Further, substrates include, but are not limited to, SrTiO3, KTaO3、MgAl2O4、(La,Sr)(Al,Ta)O3、Bi4Ge3O12、Y3Al5O12、Cd3Ga5O12、CdTe、ZnTe、Cd1-xZnxTe、ZnS、ZnSe、InAs、NaCl、LiF、CaF2、BaF2、MgO、ZrO2、Fe3O4。
Further, the purity of the reaction source is 99% or more, preferably 99.9% or more, and more preferably 99.99% or more.
The invention provides IV-VI prepared by the methodGroup infrared semiconductor film, IV-VI group infrared semiconductor film including PbS, PbSe, PbTe, Pb1-xSnxS、Pb1-xSnxSe、Pb1-x SnxAnd the Te thin film, wherein x represents the atomic percentage, and the base of the IV-VI infrared semiconductor thin film is a crystal substrate which is matched with the IV-VI infrared semiconductor crystal in lattice symmetry.
Furthermore, the thickness of the IV-VI family infrared semiconductor film is 10nm to 1.5 μm, and the width and the length are not less than 5 mm.
Furthermore, the thickness and the size of the IV-VI family infrared semiconductor film can be adjusted along with the change of the substrate temperature, the thickness of the film can be adjusted along with the substrate temperature within the range of 10nm to 1.5 mu m, and the width and the length of the film can be adjusted within the range of 1mm to 10 cm.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method has low cost, is simple and easy to implement and has high efficiency.
(2) The IV-VI family infrared semiconductor film has high crystallization quality, low defect density and uniform surface.
Drawings
FIG. 1 is a macroscopic structural view of a group IV-VI infrared semiconductor film of the present invention.
FIG. 2 is a diagram of a test apparatus for preparing a group IV-VI infrared semiconductor film according to the present invention.
FIG. 3 is a Scanning Electron Microscope (SEM) image of a group IV-VI infrared semiconductor film of an embodiment of the invention.
FIG. 4 is an X-ray diffraction pattern (XRD) of a group IV-VI infrared semiconductor thin film of example of the present invention.
Illustration of the drawings: 1-film, 2-substrate; 3-tube furnace, 4-heater, 5-heating ring, 6-S powder, 7-PbS powder, 8-SrTiO3 substrate and 9-mechanical pump.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Embodiments of the invention generally include the use of a reaction source containing a group IV-VI element to produce a semiconductor thin film (e.g., PbS, PbSe, PbTe, Pb) as shown in FIG. 11-xSnxS、Pb1-xSnxSe、Pb1-x SnxTe, where x represents atomic percent), a thin film 2 having high crystal quality, low defect density, and uniform surface is formed on a substrate 1, and is prepared by a vapor phase epitaxy method including, but not limited to, chemical vapor deposition, molecular beam epitaxy, metal organic vapor deposition, and the like, preferably using chemical vapor deposition.
The preparation method takes a compound medicine containing IV group elements Pb and Sn and VI group elements S, Se and Te as a reaction source, the reaction source can also comprise VI group element simple substances, a crystal substrate which is matched with the IV-VI group infrared semiconductor crystal in lattice symmetry is taken as a substrate, argon is taken as carrier gas, the flow rate of the argon is 150sccm, the temperature range of the VI group element simple substance reaction source is 100-1000-.
For example, the reaction source can adopt any combination of S powder + PbS powder, Se powder + PbSe powder, Te powder + PbTe powder, or only adopts PbS powder, PbSe powder, PbTe powder; substrates include, but are not limited to, SrTiO3, KTaO3、MgAl2O4、(La,Sr)(Al,Ta)O3、Bi4Ge3O12、Y3Al5O12、Cd3Ga5O12、CdTe、ZnTe、Cd1-xZnxTe、ZnS、ZnSe、InAs、NaCl、LiF、CaF2、BaF2、MgO、ZrO2、Fe3O4And the like. In specific implementation, S powder and PbS powder are preferably used as reaction sources, and SrTiO3 is used as a substrate; and the purity of the reaction source is 99% or more, preferably 99.9% or more, more preferably 99.99% or more.
The thickness of the IV-VI family infrared semiconductor film formed according to the embodiment of the invention is 98nm to 1.5 mu m, and the size is not less than 5 mm; in addition, the thickness and the size of the IV-VI family infrared semiconductor film can be adjusted along with the change of the substrate temperature, the thickness of the film can be adjusted along with the change of the substrate temperature within the range of 10nm to 1.5 mu m, and the size of the film can be adjusted along with the change of the substrate temperature within the range of 1mm to 10 cm.
Examples
This example is represented by Chemical Vapor Deposition (CVD) for preparing lead sulfide (PbS) thin film, SrTiO3The substrate takes sulfur powder and high-purity PbS powder as reaction sources, and the test device is shown in figure 2 and comprises the following specific steps:
(1) before preparation, performing decontamination treatment on a SrTiO3 substrate to keep the surface clean, putting the SrTiO3 substrate into absolute ethyl alcohol for ultrasonic cleaning, and then putting the SrTiO3 substrate into deionized water for ultrasonic cleaning; cleaning the CVD system and keeping the quartz tube furnace 3 free of other impurities;
(2) 0.1g of high-purity PbS powder and 0.3g of sulfur powder are prepared and respectively put into a quartz boat for standby.
(3) A heating ring 5 is arranged at the upstream of the tubular furnace 3 and is arranged at 190 ℃, a heater 4 sleeved outside the tubular furnace 3 is arranged in the tubular furnace 3, the temperature in the tubular furnace 3 is 800 ℃, the temperature of the center of the furnace is 800 ℃ at the moment, and the temperature is gradually reduced from the downstream to the position close to a pipe orifice;
(4) pushing the quartz boat filled with the medicine into a corresponding area after the temperature reaches a set temperature, placing sulfur powder 6 at a position close to a heating ring 5, placing PbS powder 7 at the center of the furnace, and placing SrTiO3 substrate 8 at a relatively low-temperature area close to the downstream of a pipe orifice;
(5) after the placement of the medicines is finished, closing the system, vacuumizing by using a mechanical pump 9, introducing high-purity argon at 150sccm, and reacting for 6 minutes;
(6) after the reaction is finished, the heating device is closed, after cooling to room temperature after about 30 minutes, the argon introduction is stopped, the mechanical pump 9 is closed, and the device is opened to take out the sample.
As shown in FIG. 3, the microscopic morphology of the IV-VI infrared semiconductor film was observed by using a scanning electron microscope, which indicated that the film had high crystallinity and a flat surface.
As shown in fig. 4, the monocrystallinity of the prepared group iv-vi infrared semiconductor thin film was characterized using X-ray diffraction, showing that the peak at 30.3 ° is the PbS (200) orientation peak and the peak at 62.8 ° is the PbS (400) orientation peak, indicating that the thin film has good monocrystallinity.
The test result shows that the lead sulfide (PbS) film prepared by the method has high crystallinity, flat surface, adjustable thickness along with temperature, and thickness up to tens of nanometers.
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (8)

1. A method for preparing an IV-VI family infrared semiconductor film is characterized by comprising the following steps: the preparation method adopts a gas phase epitaxy method, takes a compound containing IV-VI group elements as a reaction source, takes a crystal substrate which is matched with the IV-VI group infrared semiconductor crystal in lattice symmetry as a substrate, takes argon as a carrier gas, and takes the temperature range of the IV-VI group compound reaction source as 1000 ℃, the temperature range of the substrate as 300-600 ℃ and the growth time as less than or equal to 6 minutes.
2. The method for preparing a group IV-VI infrared semiconductor film as claimed in claim 1, wherein: the reaction source comprises medicines containing IV group elements Pb and Sn and VI group elements S, Se and Te.
3. The method for preparing a group IV-VI infrared semiconductor film as claimed in claim 2, wherein: the reaction source can also be a combined form of a VI family simple substance material and a compound containing IV-VI family elements; the temperature of the VI group simple substance reaction source is 100-500 ℃.
4. The method for preparing a group IV-VI infrared semiconductor film as claimed in claim 1, wherein: the substrate comprises SrTiO3、KTaO3、MgAl2O4、(La,Sr)(Al,Ta)O3、Bi4Ge3O12、Y3Al5O12、Cd3Ga5O12、CdTe、ZnTe、Cd1-xZnxTe、ZnS、ZnSe、InAs、NaCl、LiF、CaF2、BaF2、MgO、ZrO2、Fe3O4。
5. The method for preparing a group IV-VI infrared semiconductor film as claimed in claim 1, wherein: the purity of the reaction source is more than 99%.
6. A group IV-VI infrared semiconductor film prepared according to any of the methods of claims 1 to 5, wherein: the IV-VI family infrared semiconductor film comprises PbS, PbSe, PbTe and Pb1-xSnxS、Pb1-xSnxSe、Pb1-x SnxAnd the substrate of the IV-VI family infrared semiconductor film is a crystal substrate which is matched with the IV-VI family infrared semiconductor crystal in lattice symmetry.
7. The group iv-vi infrared semiconductor film according to claim 6, wherein: the thickness of the IV-VI family infrared semiconductor film is 10nm to 1.5 mu m, and the length and the width of the IV-VI family infrared semiconductor film are not less than 5 mm.
8. The group iv-vi infrared semiconductor film according to claim 6, wherein: the thickness and the size of the IV-VI family infrared semiconductor film can be adjusted along with the change of the temperature of the substrate, the thickness of the film can be adjusted along with the temperature of the substrate within the range of 10nm to 1.5 mu m, and the length and the width of the film can be adjusted within the range of 1mm to 10 cm.
CN202110441818.7A 2021-04-23 2021-04-23 IV-VI family infrared semiconductor film and preparation method thereof Pending CN113279063A (en)

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Publication number Priority date Publication date Assignee Title
CN114361275A (en) * 2021-12-17 2022-04-15 南昌大学 Room-temperature ultrafast infrared detector based on lead salt semiconductor film with crystal boundary and detection method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114361275A (en) * 2021-12-17 2022-04-15 南昌大学 Room-temperature ultrafast infrared detector based on lead salt semiconductor film with crystal boundary and detection method thereof

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