CN117702276A - Magnesium telluride alloy and preparation method thereof - Google Patents
Magnesium telluride alloy and preparation method thereof Download PDFInfo
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- CN117702276A CN117702276A CN202311720795.9A CN202311720795A CN117702276A CN 117702276 A CN117702276 A CN 117702276A CN 202311720795 A CN202311720795 A CN 202311720795A CN 117702276 A CN117702276 A CN 117702276A
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 61
- 239000000956 alloy Substances 0.000 title claims abstract description 61
- ZTBJFXYWWZPTFM-UHFFFAOYSA-N tellanylidenemagnesium Chemical compound [Te]=[Mg] ZTBJFXYWWZPTFM-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000011777 magnesium Substances 0.000 claims abstract description 96
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 92
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 92
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 73
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 73
- 238000010438 heat treatment Methods 0.000 claims abstract description 63
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000013078 crystal Substances 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims 7
- 239000012535 impurity Substances 0.000 abstract description 9
- 238000004321 preservation Methods 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 22
- 229910002804 graphite Inorganic materials 0.000 description 22
- 239000010439 graphite Substances 0.000 description 22
- 229910017680 MgTe Inorganic materials 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910002058 ternary alloy Inorganic materials 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical group [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a magnesium telluride alloy and a preparation method thereof, which belong to the technical field of semiconductors and comprise the following steps: the molar ratio is 1: (1-1.25) preparing magnesium blocks and tellurium blocks; uniformly dividing a magnesium block into n blocks, uniformly dividing a tellurium block into n-1 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method; placing the stacked materials into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 3-5 times, heating to 680-800 ℃, preserving heat for 2-3 h, heating to 850-1200 ℃, preserving heat for 4-6 h, and cooling to obtain magnesium telluride alloy; n is 3 or 4. According to the invention, magnesium blocks and tellurium blocks are uniformly divided into n blocks and n-1 blocks according to a specific molar ratio, the blocks are stacked by adopting an alternating block stacking method, and then two-stage heating and heat preservation are carried out under the protection of argon gas, so that the magnesium telluride alloy with high purity, no impurity phase and uniform components is obtained.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a magnesium telluride alloy and a preparation method thereof.
Background
The magnesium tellurium compound is a potential photoelectric material and can be used in the field of polycrystalline thin film solar cells. The MgTe has a hexagonal zinc blende structure, the tellurium content in the MgTe is fixed, so that a single MgTe phase can be kept in the synthesized substance as much as possible, and other impurity phases are avoided. The band gap of MgTe under the AM1.5 spectrum is in the range of 1.6-1.8eV, and the purity of the MgTe influences the photoelectric conversion effect of the MgTe serving as a solar material. The ternary alloy CdMgTe (CMT) formed by serially connecting MgTe and CdTe devices can effectively expand the spectrum utilization range of sunlight, and therefore, the ternary alloy CdMgTe (CMT) also becomes a material with great photoelectric application potential.
At present, the research on developing and researching MgTe related materials and physicochemical properties is relatively few, so that the industrialized method for preparing the MgTe alloy has important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a magnesium telluride alloy and a preparation method thereof, wherein the magnesium telluride alloy has high purity and no impurity phase.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the magnesium telluride alloy comprises the following steps:
the molar ratio is 1: (1-1.25) preparing magnesium blocks and tellurium blocks;
uniformly dividing a magnesium block into n blocks, uniformly dividing a tellurium block into n-1 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method;
placing the stacked materials into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 3-5 times, heating to 680-800 ℃, preserving heat for 2-3 hours, heating to 850-1200 ℃, preserving heat for 4-6 hours, cooling, taking out the materials, and cutting off free matters at the top and bottom to obtain magnesium telluride alloy;
n is 3 or 4.
As a preferred embodiment of the present invention, the molar ratio of the magnesium block to the tellurium block is 1: (1-1.08).
As a preferred embodiment of the present invention, the purity of the magnesium block is not lower than 4N.
As a preferred embodiment of the present invention, the purity of the tellurium block is not lower than 5N.
As a preferred embodiment of the present invention, said n=3.
As a preferred embodiment of the invention, when alternating stacks of magnesium and tellurium blocks are used, the lowermost and uppermost layers are both magnesium blocks.
As a preferred embodiment of the invention, argon is filled into the single crystal furnace until the pressure in the furnace is 1.5-2.5 MPa.
As a preferred embodiment of the present invention, the heating rate is 10 to 20 ℃/min when the temperature is raised to 680 to 800 ℃.
As a preferred embodiment of the present invention, the temperature is raised to 850-1200 ℃ at a rate of 5-10 ℃/min.
The invention also provides a magnesium telluride alloy which is prepared by adopting the preparation method.
The invention has the beneficial effects that: according to the invention, magnesium blocks and tellurium blocks are uniformly divided into n blocks and n-1 blocks according to a specific molar ratio, the blocks are stacked by adopting an alternating block stacking method, and then two-stage heating and heat preservation are carried out under the protection of argon gas, so that the magnesium telluride alloy with high purity, no impurity phase and uniform components is obtained.
Drawings
FIG. 1 is an X-ray diffraction pattern of the magnesium telluride alloy prepared in example 1.
Fig. 2 is an X-ray diffraction pattern of the magnesium telluride alloy prepared in example 2.
FIG. 3 is an X-ray diffraction pattern of the magnesium telluride alloy prepared in comparative example 1.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
In the present application, the technical features described in an open manner include a closed technical scheme composed of the listed features, and also include an open technical scheme including the listed features.
In the present application, reference is made to numerical intervals, where the numerical intervals are considered to be continuous unless specifically stated, and include the minimum and maximum values of the range, and each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
In the present application, the specific mixing manner is not particularly limited as long as the desired mixture materials are uniformly mixed.
The raw materials or instruments for the components used in each example and comparative example of the present invention were all commercially available raw materials or instruments unless otherwise specified, and the raw materials for the components used in each parallel experiment were all the same.
The embodiment of the application provides a preparation method of magnesium telluride alloy, which comprises the following steps:
the molar ratio is 1: (1-1.25) preparing magnesium blocks and tellurium blocks;
uniformly dividing a magnesium block into n blocks, uniformly dividing a tellurium block into n-1 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method;
placing the stacked materials into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 3-5 times, heating to 680-800 ℃, preserving heat for 2-3 h, heating to 850-1200 ℃, preserving heat for 4-6 h, and cooling to obtain magnesium telluride alloy;
n is 3 or 4.
According to the invention, magnesium blocks and tellurium blocks are uniformly divided into n blocks and n-1 blocks according to a specific molar ratio, the blocks are stacked by adopting an alternating block stacking method, and then two-stage heating and heat preservation are carried out under the protection of argon, so that the magnesium telluride alloy with high purity, no impurity phase and uniformity is obtained.
The inventor of the invention researches and discovers that the stacking method and the secondary heating and heat preservation temperature have obvious influence on the effect, and the magnesium telluride alloy with high purity, no impurity phase and uniform components is obtained by adopting the specific stacking method and controlling the two-stage heating and heat preservation temperature.
By adopting the stacking method, the total interface area between tellurium and magnesium is increased, the interface reaction between tellurium and magnesium is enhanced, and the reaction can be more fully and thoroughly carried out when heating and heat preservation are carried out, so that the obtained magnesium telluride alloy has single and uniform components, high purity and no impurity phase.
According to the invention, the volatilization of tellurium is effectively avoided by controlling the two-stage heating and heat preserving temperature, and meanwhile, the segregation of components is avoided, so that the magnesium telluride alloy with single and uniform components and high purity and no impurity phase is obtained.
In one embodiment, the molar ratio of the magnesium block to the tellurium block is 1: (1 to 1.08), for example, may be 1:1. 1:1.02, 1:1.05, 1:1.06, 1:1.08 or any two values therein.
In one embodiment, the magnesium block has a purity of not less than 4N (i.e., a purity of not less than 99.99%).
In one embodiment, the tellurium blocks have a purity of not less than 5N (i.e., a purity of not less than 99.999%).
In one embodiment, n=3.
In one embodiment, when alternating stacks of magnesium and tellurium blocks are used, the lowermost and uppermost layers are both magnesium blocks.
In one embodiment, argon is introduced into the single crystal furnace until the pressure in the furnace is 1.5 to 2.5MPa, and for example, the pressure may be 1.5MPa, 1.6MPa, 1.8MPa, 2MPa, 2.2MPa, 2.4MPa, 2.5MPa, or a range of any two values thereof.
In one embodiment, the heating rate is 10 to 20 ℃ per minute when the temperature is raised to 680 to 800 ℃, and may be, for example, 10 ℃ per minute, 12 ℃ per minute, 14 ℃ per minute, 15 ℃ per minute, 16 ℃ per minute, 18 ℃ per minute, 20 ℃ per minute, or a range of any two values thereof.
In one embodiment, the heating rate is 5 to 10 ℃ per minute when the temperature is raised to 850 to 1200 ℃, and for example, the heating rate may be 5 ℃ per minute, 6 ℃ per minute, 7 ℃ per minute, 8 ℃ per minute, 9 ℃ per minute, 10 ℃ per minute, or a range composed of any two values thereof.
The invention also provides a magnesium telluride alloy which is prepared by adopting the preparation method.
The following examples are provided to facilitate an understanding of the present invention. These examples are not provided to limit the scope of the claims.
Example 1
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 680 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
The X-ray diffraction diagram of the magnesium telluride alloy prepared in example 1 is shown in fig. 1.
Example 2
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1.08 preparation of magnesium block (4N purity), tellurium block (5N purity);
(2) Uniformly dividing a magnesium block into 4 blocks, uniformly dividing a tellurium block into 3 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block magnesium block+tellurium block+magnesium block);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 800 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 1000 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
The X-ray diffraction diagram of the magnesium telluride alloy prepared in example 2 is shown in fig. 2.
Example 3
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1.25 preparation of magnesium block (4N purity), tellurium block (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 680 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Example 4
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 700 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 1100 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Example 5
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 1200 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Comparative example 1
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Stacking tellurium blocks above magnesium blocks;
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 680 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, and taking out the material to obtain the magnesium telluride alloy.
Wherein, the X-ray diffraction diagram of the magnesium telluride alloy prepared in comparative example 1 is shown in fig. 3.
Comparative example 2
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Comparative example 3
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 600 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 800 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Comparative example 4
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 1300 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Comparative example 5
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:1 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And (3) placing the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, heating to 680 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out the materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Comparative example 6
The preparation method of the magnesium telluride alloy comprises the following steps:
(1) The molar ratio is 1:2 preparing magnesium blocks (4N purity) and tellurium blocks (5N purity);
(2) Uniformly dividing a magnesium block into 3 blocks, uniformly dividing a tellurium block into 2 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method, wherein the lowest layer and the uppermost layer are both magnesium blocks (namely, a stacking mode of magnesium block+tellurium block+magnesium block is adopted);
(3) And loading the stacked materials into a graphite crucible, placing the graphite crucible into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 4 times, and filling the argon for the last time until the air pressure is 2.0MPa. Heating to 680 ℃ at a heating rate of 10 ℃/min, preserving heat for 2 hours, heating to 850 ℃ at a heating rate of 10 ℃/min, preserving heat for 4 hours, cooling, taking out materials, and cutting off free matters at the top and the bottom to obtain the magnesium telluride alloy.
Test data
Tellurium content in the magnesium telluride alloys of examples and comparative examples was detected by the ICP-OES method.
The phases were detected by XRD method.
TABLE 1
| Tellurium content/% | Phase (3) | |
| Example 1 | 83.56 | MgTe+Te |
| Example 2 | 83.84 | MgTe+Te |
| Example 3 | 84.35 | MgTe+Te |
| Example 4 | 83.66 | MgTe+Te |
| Example 5 | 84.33 | MgTe+Te |
| Comparative example 1 | 81.14 | MgTe+Te+TeO 2 |
| Comparative example 2 | 82.08 | MgTe+Te+Mg |
| Comparative example 3 | 81.00 | MgTe+Te+Mg |
| Comparative example 4 | 82.33 | MgTe+Mg |
| Comparative example 5 | 78.54 | MgTe+Mg |
| Comparative example 6 | 88.60 | MgTe2+TeO 2 |
As can be seen from Table 1, the magnesium telluride alloy of the present invention has high purity, no impurity phase, and single and uniform components.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the magnesium telluride alloy is characterized by comprising the following steps of:
the molar ratio is 1: (1-1.25) preparing magnesium blocks and tellurium blocks;
uniformly dividing a magnesium block into n blocks, uniformly dividing a tellurium block into n-1 blocks, and stacking the magnesium block and the tellurium block by adopting an alternating stacking method;
placing the stacked materials into a single crystal furnace, vacuumizing the single crystal furnace, filling argon, repeating for 3-5 times, heating to 680-800 ℃, preserving heat for 2-3 h, heating to 850-1200 ℃, preserving heat for 4-6 h, and cooling to obtain magnesium telluride alloy;
n is 3 or 4.
2. The method for preparing the magnesium telluride alloy according to claim 1, wherein the molar ratio of the magnesium block to the tellurium block is 1: (1-1.08).
3. The method for producing a magnesium telluride alloy as set forth in claim 1, wherein the purity of said magnesium block is not lower than 4N.
4. The method for producing a magnesium telluride alloy as set forth in claim 1, wherein the purity of said tellurium block is not lower than 5N.
5. The method for producing a magnesium telluride alloy as set forth in claim 1, wherein n = 3.
6. The method for producing a magnesium telluride alloy according to claim 1, wherein when the magnesium blocks and tellurium blocks are alternately stacked, the lowermost layer and the uppermost layer are both magnesium blocks.
7. The method for producing a magnesium telluride alloy according to claim 1, wherein argon is introduced into the single crystal furnace until the gas pressure in the furnace is 1.5 to 2.5MPa.
8. The method for producing a magnesium telluride alloy as set forth in claim 1, wherein the heating rate is 10 to 20 ℃/min when the temperature is raised to 680 to 800 ℃.
9. The method for producing a magnesium telluride alloy as claimed in claim 1, wherein the heating rate is 5 to 10 ℃/min when the temperature is raised to 850 to 1200 ℃.
10. A magnesium telluride alloy, characterized in that it is prepared by the preparation method according to any one of claims 1 to 9.
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