CN113716531B - Solid-phase synthesis method of narrow-bandgap semiconductor MTeI - Google Patents
Solid-phase synthesis method of narrow-bandgap semiconductor MTeI Download PDFInfo
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- CN113716531B CN113716531B CN202111021676.5A CN202111021676A CN113716531B CN 113716531 B CN113716531 B CN 113716531B CN 202111021676 A CN202111021676 A CN 202111021676A CN 113716531 B CN113716531 B CN 113716531B
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000010532 solid phase synthesis reaction Methods 0.000 title claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 31
- 239000010453 quartz Substances 0.000 claims description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000000376 reactant Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910002916 BiTeI Inorganic materials 0.000 abstract description 40
- 239000013078 crystal Substances 0.000 abstract description 13
- 238000003746 solid phase reaction Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 239000002243 precursor Substances 0.000 abstract description 3
- 238000002441 X-ray diffraction Methods 0.000 description 29
- 238000001878 scanning electron micrograph Methods 0.000 description 25
- 239000000843 powder Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 229910052740 iodine Inorganic materials 0.000 description 8
- 229910052797 bismuth Inorganic materials 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 6
- 239000011630 iodine Substances 0.000 description 6
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000007039 two-step reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000000731 high angular annular dark-field scanning transmission electron microscopy Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
Abstract
The invention provides a solid phase synthesis method of a narrow bandgap semiconductor MTeI, which comprises the following steps: adding M, te and excessive I 2 The simple substance is subjected to solid phase reaction under the vacuum condition to obtain a narrow band gap semiconductor MTeI; m is Bi and/or Sb. The invention uses metal Bi simple substance and/or Sb simple substance for the first time, te simple substance and I 2 Simple substance is used as a precursor, and the novel narrow band gap semiconductor BiTeI and/or SbTeI crystal is prepared by a simple one-step solid phase reaction method, so that the synthesis path is simple and the operation is convenient. The narrow bandgap semiconductor BiTeI and/or SbTeI prepared by the method has high crystallinity, high purity and good stability, greatly shortens the synthesis time, and has good practical prospect.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a solid-phase synthesis method of a narrow bandgap semiconductor MTeI.
Background
The BiTeI compound is a compound composed of heavy elements, and electrons thereof have strong association effects, thereby bringing a number of interesting properties to be intensively studied by physicists. However, the synthesis of this compound has been one of the difficulties impeding its development. Therefore, development of a synthetic method with lower cost, convenience and rapidness is urgently needed for the materials.
Disclosure of Invention
The invention aims to provide a solid-phase synthesis method of a narrow bandgap semiconductor MTeI, and the narrow bandgap semiconductor MTeI prepared by the method has high crystallinity, good stability and good practical prospect.
The invention provides a solid phase synthesis method of a narrow bandgap semiconductor MTeI, which comprises the following steps:
adding M, te and excessive I 2 The simple substance is subjected to solid phase reaction under the vacuum condition to obtain a narrow band gap semiconductor MTeI;
m is Bi and/or Sb.
Preferably, the metal M simple substance, te simple substance and excessive I 2 The simple substance is put into a closed vacuum container, heated to a temperature T, kept for 20 hours, and the reaction is finished.
Preferably, the temperature is raised to a temperature T at a rate of 5 to 20 ℃/min.
Preferably, M is Bi; t is more than or equal to 500 ℃ and less than or equal to 650 ℃.
Preferably, M is Sb; t is more than or equal to 350 ℃ and less than or equal to 450 ℃.
The invention provides a solid phase synthesis method of a narrow bandgap semiconductor MTeI, which comprises the following steps: metal M simple substance and TeSimple substance and excessive I 2 The simple substance is subjected to solid phase reaction under the vacuum condition to obtain a narrow band gap semiconductor MTeI; m is Bi and/or Sb. The invention uses metal Bi simple substance and/or Sb simple substance for the first time, te simple substance and I 2 Simple substance is used as a precursor, and the novel narrow band gap semiconductor BiTeI and/or SbTeI crystal is prepared by a simple one-step solid phase reaction method, so that the synthesis path is simple and the operation is convenient. The narrow bandgap semiconductor BiTeI and/or SbTeI prepared by the method has high crystallinity, high purity and good stability, greatly shortens the synthesis time, and has good practical prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is an X-ray diffraction pattern (XRD) of a narrow bandgap semiconductor BiTeI prepared in example 1 and a Scanning Electron Micrograph (SEM) of the dispersion in ethanol (a-b);
FIG. 2 is a high-resolution transmission electron micrograph (HRTEM) (a) of the narrow bandgap semiconductor BiTeI prepared in example 1, and a high-angle annular dark field image (HAADF-STEM) of the contained element, and a Mapping photograph (b);
FIG. 3 is the X-ray photoelectron spectrum (XPS) of the element Te3d (c), bi4f (b), te3d (c) and Bi4f (b) of the narrow bandgap semiconductor BiTeI prepared in example 1;
FIG. 4 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the narrow bandgap semiconductor BiTeI prepared in comparative example 1;
FIG. 5 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the narrow bandgap semiconductor BiTeI prepared in example 2;
FIG. 6 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the narrow bandgap semiconductor BiTeI prepared in example 3;
FIG. 7 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the narrow bandgap semiconductor BiTeI prepared in comparative example 2;
FIG. 8 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the narrow bandgap semiconductor SbTeI prepared in example 4;
FIG. 9 is an X-ray diffraction pattern (XRD) of the narrow bandgap semiconductor SbTeI prepared in comparative example 3.
Detailed Description
The invention provides a solid phase synthesis method of a narrow bandgap semiconductor MTeI, which comprises the following steps:
adding M, te and excessive I 2 The simple substance is subjected to solid phase reaction under the vacuum condition to obtain a narrow band gap semiconductor MTeI;
m is Bi and/or Sb.
In the present invention, the excess I 2 Simple substance means a slight excess but not more than 1.2 times I calculated in stoichiometric ratio 2 Simple substance.
The invention preferably comprises the steps of adding a metal M simple substance, a Te simple substance and an excess amount of I 2 The simple substance is placed in the quartz tube, the quartz tube is sealed under the vacuum state in the holding tube, the sealed quartz tube is obliquely placed in the muffle furnace, and reactants are held at the bottom of the quartz tube.
Then, the muffle furnace was heated to a temperature T, and then kept at that temperature for 20 hours, thereby ending the reaction.
In the present invention, it is preferable to raise the temperature to the temperature T at a rate of 5 to 20 ℃/min, more preferably 6 to 15 ℃/min, such as 5 ℃/min,6 ℃/min,7 ℃/min,8 ℃/min,9 ℃/min,10 ℃/min,11 ℃/min,12 ℃/min,13 ℃/min,14 ℃/min,15 ℃/min, preferably a range value in which any of the above values is an upper limit or a lower limit;
in the present invention, M is Bi; t is more than or equal to 500 ℃ and less than or equal to 650 ℃;
m is Sb; t is more than or equal to 350 ℃ and less than or equal to 450 ℃.
After the reaction is finished, naturally cooling to room temperature to obtain a bulk solid MTeI product with metallic luster.
Such control I in the present invention 2 The excessive one-step synthesis method is simple to operateThe method has novel thought, greatly shortens the reaction time compared with the prior method, and can be widely applied to the control preparation of other M-VIA-VIIA compounds.
The invention provides a solid phase synthesis method of a narrow bandgap semiconductor MTeI, which comprises the following steps: adding M, te and excessive I 2 The simple substance is subjected to solid phase reaction under the vacuum condition to obtain a narrow band gap semiconductor MTeI; m is Bi and/or Sb. The invention uses metal Bi simple substance and/or Sb simple substance for the first time, te simple substance and I 2 Simple substance is used as a precursor, and the novel narrow band gap semiconductor BiTeI and/or SbTeI crystal is prepared by a simple one-step solid phase reaction method, so that the synthesis path is simple and the operation is convenient. The narrow bandgap semiconductor BiTeI and/or SbTeI prepared by the method has high crystallinity, high purity and good stability, greatly shortens the synthesis time, and has good practical prospect.
In order to further illustrate the present invention, the following examples are provided to describe in detail a solid phase synthesis method of narrow bandgap semiconductor MTeI according to the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
0.5mmol bismuth [ Bi ] was taken]Elemental powder, 0.5mmol Te]Elemental powder and slightly more than 0.25mmol elemental iodine [ I ] 2 ]The tube was placed in a quartz tube having an inner diameter of 8mm, and the quartz tube was sealed while maintaining the inside of the tube under vacuum. The sealed quartz tube was placed obliquely in the muffle furnace, keeping the reactants at the bottom of the quartz tube. The muffle furnace is heated to about 500 ℃ for a certain time, and the temperature is kept for 20 hours. And naturally cooling the muffle furnace to room temperature after the reaction is finished to obtain a bulk solid BiTeI product with metallic luster.
The morphology, structure, phase, composition and the like of the BiTeI product are characterized as follows:
BiTeI belongs to the P3m1 space group, and the X-ray diffraction pattern (XRD) is shown in figure 1a, wherein 2 theta peaks at 12.932 degrees, 23.675 degrees, 26.033 degrees, 27.067 degrees, 35.474 degrees, 39.492 degrees, 41.624 degrees, 43.768 degrees, 46.563 degrees, 50.358 degrees, 53.547 degrees, 55.813 degrees, 58.719 degrees, 59.336 degrees, 64.210 degrees, 67.325 degrees and 68.539 degrees can precisely correspond to (001), (100), (002), (011), (102), (003), (110), (11-1), (103), (201), (004), (022), (11-3), (014), (023), (21-1) and (005) diffraction crystal faces (JCCDS 01-082-0484) of the material respectively. No peaks other than the target product were observed in the figure, indicating that the BiTeI prepared by the simple one-step method presented in this experiment was pure phase and highly crystalline. FIG. 1b is an SEM photograph of a BiTeI sample dispersed in ethanol, the morphology of the sample exhibiting a uniform coiled flake shape.
The BiTeI is calibrated in a High Resolution Transmission Electron Micrograph (HRTEM) (fig. 2 a), where lattice fringes at 0.227nm and 0.329nm can exactly correspond to the (003) and (011) crystal planes of the BiTeI. FIG. 2b is a Mapping photograph of a high angle annular dark field image (HAADF-STEM) and three basic elements Bi, te and I, respectively, constituting a sample, showing that the three elements are uniformly distributed inside the material, demonstrating successful preparation of the BiTeI material.
X-ray photoelectron spectroscopy (XPS) reflects information such as the composition of elements in a material and the chemical states of the elements. For the BiTeI material (FIGS. 3 a-d), there are only electron-corresponding peaks of Bi, te, I elements and unavoidable C1s and O1s peaks in XPS full spectrum, which indicates that the synthesized BiTeI sample is a pure phase. In the fine spectrum of Bi4f (FIG. 3 b), characteristic peaks at 164.0 and 158.8eV binding energies can be observed, respectively, and in FIG. 3c, the fine XPS spectrum of Te3d is composed of Te3d at 583.2 and 587.2eV 3/2 Peak, te3d at 572.8 and 576.8eV 5/2 Peak composition. FIG. 3d is a diagram of I3 d at 630.8 3/2 Peak and I3 d at 619.3eV 5/2 Peak composition.
Through the analysis discussed above, it is demonstrated that the narrow bandgap semiconductor BiTeI material can be successfully obtained by the one-step method provided by the present invention. The preparation method is simple to operate, novel in thought, greatly shortened in reaction time, and capable of synthesizing the high-crystallinity narrow-bandgap semiconductor BiTeI material.
Comparative example 1
Adopts a traditional two-step reaction method, and melts first and then slowly cools to the reaction temperature. The same amount of 0.5mmol bismuth [ Bi ] as in example 1 was taken]Elemental powder, 0.5mmol Te]Elemental powder and slightly more than 0.25mmol elemental iodine [ I ] 2 ]The tube was placed in a quartz tube having an inner diameter of 8mm, and the quartz tube was sealed while maintaining the inside of the tube under vacuum. The sealed quartz tube was placed obliquely in the muffle furnace, keeping the reactants at the bottom of the quartz tube. The muffle furnace is heated to 600 ℃ after 90min, then cooled to 500 ℃ slowly within 8 hours, and naturally cooled to room temperature after the temperature is kept for 24 hours. FIG. 4 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the sample prepared in comparative example 1, showing that Bi in the binary phase is present in the synthesized sample in addition to the target product BiTeI 4 Te 3 And TeI 0.44 And (5) impurities. It was demonstrated that the product obtained contained other impurities when the same reaction temperature of 500℃as in the process shown in this patent was chosen. From the scanning electron micrograph, the particles are mainly in a large lamellar shape which is agglomerated, and even in ethanol solution, the particles cannot be effectively reduced in size and have poor solubility. In summary, compared with the traditional two-step reaction method, the method can shorten the reaction time by at least 12 hours under the same reaction temperature condition to obtain the narrow band gap semiconductor BiTeI with higher purity and better crystallinity; in addition, the BiTeI crystal obtained by the method has good solubility in ethanol solution, so that the BiTeI crystal can be conveniently used as a junction type and photoconductive photoelectric detector by well contacting a BiTeI film with a silicon wafer and a graphene electrode through spin coating, and further, the BiTeI crystal can be applied to the aspects of communication, imaging, military detection and the like.
Example 2
The same amount of 0.5mmol bismuth [ Bi ] as in example 1 was taken]Elemental powder, 0.5mmol Te]Elemental powder and slightly more than 0.25mmol elemental iodine [ I ] 2 ]The tube was placed in a quartz tube having an inner diameter of 8mm, and the quartz tube was sealed while maintaining the inside of the tube under vacuum. The sealed quartz tube was placed obliquely in the muffle furnace, keeping the reactants at the bottom of the quartz tube. After a certain time of heating the muffle furnace to 550 ℃, the muffle furnace is kept at the temperature for 20 hours. And naturally cooling the muffle furnace to room temperature after the reaction is finished to obtain a bulk solid BiTeI product with metallic luster. FIG. 5 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of BiTeI prepared in example 2, in which all diffraction peak positions match the crystal planes of BiTeIThe preparation shows that the pure narrow band gap semiconductor BiTeI product with good crystallinity can be still synthesized at the temperature of 550 ℃.
Example 3
The same amount of 0.5mmol bismuth [ Bi ] as in example 1 was taken]Elemental powder, 0.5mmol Te]Elemental powder and slightly more than 0.25mmol elemental iodine [ I ] 2 ]The tube was placed in a quartz tube having an inner diameter of 8mm, and the quartz tube was sealed while maintaining the inside of the tube under vacuum. The sealed quartz tube was placed obliquely in the muffle furnace, keeping the reactants at the bottom of the quartz tube. After the muffle furnace is heated to 600 ℃ for a certain time, the temperature is directly kept for 20 hours. And naturally cooling the muffle furnace to room temperature after the reaction is finished to obtain a massive solid product with metallic luster. FIG. 6 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of BiTeI prepared in example 3, showing that pure narrow bandgap semiconductor BiTeI blocks can be synthesized at this temperature as well, and that each peak in the XRD pattern is sharper than in example 2, with smaller half-width, demonstrating that higher temperatures are favorable for producing better crystalline BiTeI.
Comparative example 2
The same amount of 0.5mmol bismuth [ Bi ] as in example 1 was taken]Elemental powder, 0.5mmol Te]Elemental powder and slightly more than 0.25mmol elemental iodine [ I ] 2 ]The tube was placed in a quartz tube having an inner diameter of 8mm, and the quartz tube was sealed while maintaining the inside of the tube under vacuum. The sealed quartz tube was placed obliquely in the muffle furnace, keeping the reactants at the bottom of the quartz tube. The muffle furnace is heated to 700 ℃ for a certain time, and the temperature is kept for 20 hours. And naturally cooling the muffle furnace to room temperature after the reaction is finished. FIG. 7 is an X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of the sample prepared in comparative example 2, showing that the sample synthesized at this time is mainly the target product BiTeI and Bi in binary phase 2 Te 3 And TeI 4 And (5) impurities. The temperature is too high, the obtained product contains more impurities, and the temperature condition is not suitable for synthesizing a narrow band gap semiconductor BiTeI.
Example 4
0.5mmol of antimony [ Sb ] is taken]Elemental powder, 0.5mmol Te]Elemental powder and slightly more than 0.25mmol elemental iodine [ I ] 2 ]Is arranged in a quartz tube with the inner diameter of 8mm,the quartz tube was sealed while maintaining the vacuum state in the tube. The sealed quartz tube was placed obliquely in the muffle furnace, keeping the reactants at the bottom of the quartz tube. The muffle furnace is heated to about 350 ℃ for a certain time, and the temperature is kept for 20 hours. And after the reaction is finished, naturally cooling the muffle furnace to room temperature, finding that a rod-shaped product adheres to the wall of the quartz tube, and collecting for later use. FIG. 8 shows the X-ray diffraction pattern (XRD) and Scanning Electron Micrograph (SEM) of SbTeI prepared in example 4, in which no excessive impurity peaks were present. In addition, from SEM pictures, the product has clear rod-shaped structure, which is consistent with the C2/m space group of SbTeI crystals. This demonstrates this control I 2 The solid phase method is very versatile in preparing such materials. In addition, the SbTeI crystal prepared has a rod-shaped structure, and a photoelectric detector with a metal-semiconductor-metal structure is easy to prepare.
Comparative example 3
The same amount of elemental powder as in example 4 was filled into a quartz tube using a conventional two-step reaction method, and the quartz tube was sealed while maintaining the vacuum state in the tube. The sealed quartz tube was placed obliquely in a muffle furnace. The muffle furnace is heated to 400 ℃ after 90min, then is slowly cooled to 350 ℃ after 8 hours, is kept at the temperature for 24 hours, and is naturally cooled to room temperature after the reaction is finished. The amount of crystals obtained in comparative example 3 was small compared with SbTeI prepared by the method of example 4, and it can be concluded from the X-ray diffraction pattern (XRD) of SbTeI shown in fig. 9 that the crystallinity of crystals prepared by the method was poor.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (2)
1. A solid phase synthesis method of a narrow bandgap semiconductor MTeI comprises the following steps:
adding M, te and excessive I 2 The simple substance is placed in a quartz tube, and the quartz is kept in a vacuum state in the tubeSealing the tube, placing the sealed quartz tube in a muffle furnace in an inclined manner, keeping reactants at the bottom of the quartz tube, then heating the muffle furnace to a temperature T, then preserving heat for 20 hours, and ending the reaction to obtain the narrow bandgap semiconductor MTeI;
the excess I 2 Simple substance means a slight excess but not more than 1.2 times I calculated in stoichiometric ratio 2 Simple substance;
m is Bi, and T is more than or equal to 500 ℃ and less than or equal to 650 ℃.
2. The method for solid phase synthesis of narrow bandgap semiconductor MTeI according to claim 1, wherein the temperature is raised to temperature T at a rate of 5-20 ℃/min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6222242B1 (en) * | 1998-07-27 | 2001-04-24 | Komatsu Ltd. | Thermoelectric semiconductor material and method of manufacturing same |
| CN101486449A (en) * | 2008-01-18 | 2009-07-22 | 北京化工大学 | Solid phase synthesis method for quaternary selenide K2CdSnSe4 |
| CN106571422A (en) * | 2016-11-09 | 2017-04-19 | 苏州科技大学 | Bismuth telluride based N type thermoelectric material and preparation method thereof |
| CN109797430A (en) * | 2018-12-28 | 2019-05-24 | 中山大学 | A kind of novel codope chalcogen superconductor and preparation method thereof |
| CN112064116A (en) * | 2020-09-14 | 2020-12-11 | 中国科学院上海硅酸盐研究所 | Method for preparing InSeI single crystal |
-
2021
- 2021-09-01 CN CN202111021676.5A patent/CN113716531B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6222242B1 (en) * | 1998-07-27 | 2001-04-24 | Komatsu Ltd. | Thermoelectric semiconductor material and method of manufacturing same |
| CN101486449A (en) * | 2008-01-18 | 2009-07-22 | 北京化工大学 | Solid phase synthesis method for quaternary selenide K2CdSnSe4 |
| CN106571422A (en) * | 2016-11-09 | 2017-04-19 | 苏州科技大学 | Bismuth telluride based N type thermoelectric material and preparation method thereof |
| CN109797430A (en) * | 2018-12-28 | 2019-05-24 | 中山大学 | A kind of novel codope chalcogen superconductor and preparation method thereof |
| CN112064116A (en) * | 2020-09-14 | 2020-12-11 | 中国科学院上海硅酸盐研究所 | Method for preparing InSeI single crystal |
Non-Patent Citations (2)
| Title |
|---|
| Giant Rashba-type spin splitting in bulk BiTeI;K. Ishizaka et al.;NATURE MATERIALS;第10卷;第521-526页 * |
| Synthesis and Study of Electrical Properties of SbTeI;Harish K. Dubey et al.;Advances in Physical Chemistry;第2014卷;第1页第2.1节 * |
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