CN114540944A - Method for preparing exol semimetal crystal by vertical CVT seed crystal method - Google Patents
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Abstract
The invention relates to a method for preparing a peril semimetal crystal by a vertical CVT seed crystal method, which comprises the steps of mixing massive metal niobium foil or tantalum foil fine powder with powdery arsenic and iodine to obtain a first mixture; adding the exol semi-metal crystal grains serving as seed crystals into the first mixture to obtain a second mixture; adding the second mixture as a reaction raw material into a quartz tube, vacuumizing the quartz tube and sealing the quartz tube; vertically placing the sealed quartz tube in a vertical growth furnace, heating to the temperature of 450-550 ℃, and then preserving heat for 20-40 min; continuously heating to 1000 ℃ and 1100 ℃, and then preserving the heat for 20-40 days; after the heat preservation is finished, the reaction is stopped after the temperature is slowly cooled to 450-550 ℃, and the reaction is cooled to room temperature. The invention adopts a vertical growth process, does not need a large transmission path when the crystal grows at the bottom and can keep the continuity of crystal growth; the axial and radial temperature gradients in the quartz tube are reduced, so that the reaction process is more stable, and large-size single crystals can be obtained.
Description
Technical Field
The invention belongs to the field of new material preparation, and particularly relates to a preparation method of a large-size peril semimetal single crystal.
Background
In 2014, professor of wuhong Ming et al found for the first time that solid materials such as TaAs, TaP, NbAs and NbP are still semimetal materials by theoretical calculation. Different from the prior theoretical scheme, the series of materials can be naturally synthesized, and careful and complicated regulation and control such as doping and the like are not needed. More importantly, the material has no central inversion but keeps time inversion symmetry, so that the material has no complexity of magnetic domains and the like caused by magnetic materials, and can be directly observed by angle-resolved photoelectron spectroscopy (ARPES) experiments. Since the discovery of these materials, they have attracted much attention from domestic and foreign scientists because they exhibit a series of peculiar phenomena such as fermi arc, ultra-high mobility, giant magnetoresistance due to chiral anomalies. And scientists predict that these materials will have potential applications in future spintronics and even quantum computing.
However, there are difficulties in obtaining single crystal materials of the exotic semimetals. The method for preparing the peril semimetal crystal which is disclosed at present is mainly a chemical vapor transport process, but in the growth process of the crystal, not only an axial temperature gradient but also a radial temperature gradient exist, and the larger radial temperature gradient can cause crystal growth defects and generate excessive nucleation sites, thereby reducing the quality and the yield of the crystal. On the other hand, the transport path of the raw material atmosphere is short during the growth process, and as a result, the product is mostly small-sized crystal grains, and it is difficult to obtain large-sized and high-quality single crystals.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing a peril semimetal crystal by a vertical CVT seed crystal method, which can improve the growth condition of the crystal, thereby obtaining a large-size and high-quality peril semimetal single crystal material.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing exol semimetal crystals by a vertical CVT seed crystal method comprises the following steps:
mixing massive niobium foil or tantalum foil fine powder with powdery arsenic and iodine to obtain a first mixture;
adding the exol semimetal crystal grains serving as seed crystals into the first mixture to obtain a second mixture;
step three, adding the second mixture as a reaction raw material into a quartz tube, vacuumizing the quartz tube and sealing the quartz tube;
step four, vertically placing the sealed quartz tube in a vertical growth furnace, heating to 450-550 ℃, and then preserving heat for 20-40 min; continuously heating to 1000 ℃ and 1100 ℃, and then preserving the heat for 20-40 days; after the heat preservation is finished, the reaction is stopped after the temperature is slowly cooled to 450-550 ℃, and the reaction is cooled to room temperature.
Further, in the first step, in terms of molar ratio, the ratio of niobium foil or tantalum foil: arsenic powder: iodine powder = 1.00: (1.02-1.05): (0.02-0.05).
Further, in the first step, the bulk tantalum foil or niobium foil is finely crushed small-sized pieces with a thickness of 0.015-0.025 mm and a size of (1.5-2.5) × (1.5-2.5) mm2。
Further, in the first step, the thickness of the bulk tantalum foil or niobium foil is 0.02 mm and the size is 2X 2 mm2。
Further, in step three, during the sealing process, the quartz tube is placed in acetone solution added with dry ice all the way.
Further, in the third step, the quartz tube is vacuumized to 10 deg.C-5-10-4pa and then sealing the film.
Further, in the fourth step, the temperature is raised to 450-550 ℃ at a rate of 2 ℃/min.
Further, in the fourth step, the temperature is raised to 1000-1100 ℃ at a rate of 5 ℃/min.
Further, in the fourth step, the temperature is raised to 500 ℃ at a rate of 2 ℃/min.
Further, in the fourth step, the temperature is raised to 1050 ℃ at a rate of 5 ℃/min.
The invention provides a vertical CVT seed crystal growth process aiming at the problems that the existing preparation process has incomplete raw material reaction, more nucleation points in crystal growth, difficulty in obtaining large-size single crystals and the like. The process is characterized in that the traditional chemical vapor transport process is improved, the transport path of the raw material atmosphere is firstly reduced in a vertical growth mode, and the axial and radial temperature gradients are reduced, so that the concentration of the raw material at the bottom of the quartz tube is always higher than that at the top of the quartz tube in the growth process to form a concentration difference, and further, the atmosphere beneficial to crystal growth is manufactured at the bottom. On the other hand, a smaller temperature gradient environment prolongs the continuity and stability of crystal growth. In addition, the addition of a seed crystal provides a nucleation site for crystal growth. These create conditions for obtaining large-sized exotic semimetallic materials.
The invention selects niobium (Nb) foil or tantalum (Ta) foil and arsenic (As) powder which are subjected to fine crushing treatment As raw materials, the crushed niobium foil and tantalum foil generate fewer defects and larger specific surface area in the growth process of crystals, and in addition, a small amount of elemental iodine (I) is added2) As a transport agent.
The invention adopts a vertical growth process, does not need a large transmission path when the crystal grows at the bottom and can keep the continuity of crystal growth; the axial and radial temperature gradients in the quartz tube are reduced, and the reaction process is more stable, thereby being beneficial to obtaining large-size single crystals.
Different from the CVT process of the two-step method, namely the CVT process of the invention only needs one-step method, namely the process of the invention firstly obtains small-size crystal grains and then takes out the small-size crystal grains to carry out secondary growth to obtain larger-size crystals.
The invention has simple process, strong repeatability and certain universality, and the prepared seoul semimetal single crystal has larger size which can reach 4 multiplied by 5 multiplied by 4 mm3。
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing exol semimetal crystals by a vertical CVT seed crystal method.
FIG. 2 is an optical image of a single-crystal material of niobium arsenide (NbAs) obtained in example 1.
FIG. 3 is an XRD diffraction pattern of the niobium arsenide single crystal material obtained in example 1.
FIG. 4 is a Raman spectrum of the niobium arsenide single crystal material obtained in example 1.
Detailed Description
Aiming at the problems of incomplete reaction of raw materials, large axial and radial temperature gradients, more crystal nucleation points and small crystal size in the growth process of crystals, the typical embodiment of the invention provides a method for preparing exol semimetal crystals by a vertical CVT seed crystal method, which comprises the following steps.
Firstly, mixing the massive niobium foil or tantalum foil fine powder with powdered arsenic and iodine to obtain a first mixture.
Wherein, in terms of mole ratio, niobium or tantalum foil: arsenic powder: iodine powder = 1.00: (1.02-1.05): (0.02-0.05), preferably, niobium or tantalum foil: arsenic powder: iodine powder = 1.00: 1.05: 0.05.
wherein the bulk tantalum foil or niobium foil is finely crushed small-sized pieces having a thickness of 0.015-0.025 mm and a size of (1.5-2.5) × (1.5-2.5) mm2. Preferably, the bulk tantalum or niobium foil has a thickness of 0.02 mm and a size of 2X 2 mm2. The use of the finely crushed niobium and tantalum foils results in fewer defects and a larger specific surface area in the process of preparing the peril-semi-metallic single crystal material, thereby contributing to an increase in reaction efficiency and obtaining a larger-sized single crystal material.
The raw material weighing process in the step one needs to be completed in the glove box in the whole process.
And step two, adding the exol semimetal crystal grains serving as seed crystals into the first mixture to obtain a second mixture.
In the second step, 1 small-size crystal grain with good crystallinity is selected as seed crystal to provide nucleation sites for crystal growth. The selected seed crystal is tantalum arsenide or niobium arsenide crystal grain with main exposed surface being (004) crystal face, and the size of single crystal grain is about 1 mm3. More nucleation points appear in the growth process of the crystal, and the obtainment of large-size crystals is limited. The addition of the seed crystal reduces the nucleation energy of the crystal, reduces the appearance of nucleation points and finally obtains the large-size peril semimetal single crystal on the basis of the existing seed crystal.
Preferably, the seed crystal is a semimetal single crystal obtained by a horizontal CVT method or a vertical CVT method.
And step three, adding the second mixture serving as a reaction raw material into a quartz tube, vacuumizing the quartz tube and sealing the quartz tube. Preferably, the quartz tube is evacuated to 10 deg.C-5-10-4pa and then sealing the film.
During the sealing process, the quartz tube was placed in an acetone solution with dry ice added throughout. The sealing process needs to be performed in a low temperature solution to prevent volatilization of iodine. The sum of the gas pressures generated by the arsenic powder and the iodine powder must not exceed the pressure which can be borne by the sealed quartz tube.
Step four, vertically placing the sealed quartz tube in a vertical growth furnace, heating to 450-550 ℃, and then preserving heat for 20-40 min; continuously heating to 1000 ℃ and 1100 ℃, and then preserving the heat for 20-40 days; after the heat preservation is finished, the reaction is stopped after the temperature is slowly cooled to 450-550 ℃, and the reaction is cooled to room temperature.
Wherein the temperature is raised to 450-550 ℃ at 2 ℃/min, preferably to 500 ℃ at 2 ℃/min.
Wherein the temperature is raised to 1000-1100 ℃ at 5 ℃/min, preferably to 1050 ℃ at 5 ℃/min.
The implementation mode adopts a vertical growth process and is characterized in that the traditional horizontal transportation mode is changed into a vertical transportation mode. This causes a large difference in the concentration of the raw material in the quartz tube, with the concentration in the bottom of the tube being much higher than in the top. As a result, the crystal does not need a large transmission path when growing at the bottom, and the continuity of the crystal growth can be maintained; the vertical growth process can reduce the axial and radial temperature gradients in the quartz tube, so that the reaction process is more stable, thereby being beneficial to obtaining large-size single crystals.
The claimed solution is further illustrated by the following examples. However, the examples are intended to illustrate embodiments of the invention without departing from the scope of the subject matter of the invention, and the scope of the invention is not limited by the examples. Unless otherwise specifically indicated, the materials and reagents used in the present invention are available from commercial products in the art.
In the following examples, the preparation of the exol semimetal crystals was carried out in an apparatus as shown in FIG. 1. The quartz tube 1 is vertically placed in the vertical growth furnace 2.
Example 1
Selecting a material with a molar ratio of 1: 1.05: 0.05 niobium foil, arsenic powder and iodine powder. And finely crushing the niobium foil to a thickness of 0.02 mm and a size of 2X 2 mm2. Specifically, 0.279 g of niobium foil, 0.236 g of arsenic powder and 0.038 g of iodine powder are uniformly mixed and added into a quartz tube, and the process needs to be carried out in a glove box.
The exposed surface obtained is selected as (004) crystal surface with a size of about 1 mm3The niobium arsenide single crystal is added into the quartz tube as a seed crystal. The quartz tube was evacuated to 4X 10-4Pa, then immediately sealed, and the process required placing the quartz tube in a dry ice bath (minus 78 ℃) of dry ice mixed with acetone.
Vertically placing a quartz tube in a vertical growth furnace, and setting the program to be 2 ℃/min to 500 ℃ and then preserving the temperature for 30 min; then heating to 1050 ℃ at the speed of 5 ℃/min, and then preserving heat for 30 days; after the heat preservation is finished, the reaction is stopped and cooled to the room temperature after the reaction is cooled to 500 ℃ at the speed of 5 ℃/min.
Through the experimental steps, the large-size peril semimetal niobium arsenide single crystal material is successfully prepared.
An optical image of the niobium arsenide single crystal material prepared in this example is shown in FIG. 2, and the single crystal size is about 4X 5X 4 mm3。
The XRD pattern of the niobium arsenide single crystal material prepared in the example is shown in figure 3, the diffraction peak position of the crushed crystal is consistent with that of a PDF card, and the diffraction peak position of the crystal proves that the (001) crystal face orientation of the exposed face position.
The Raman spectrum of the niobium arsenide single crystal material prepared in the example is shown in fig. 4, and the Raman shifts at three positions in the graph are consistent with those reported in the literature.
Example 2
Selecting a material with a molar ratio of 1: 1.02: 0.05 niobium foil, arsenic powder and iodine powder. And finely crushing the niobium foil to a thickness of 0.02 mm and a size of 2X 2 mm2. Specifically, 0.279 g of niobium foil, 0.229 g of arsenic powder and 0.038 g of iodine powder are selected, uniformly mixed and added into a quartz tube, andthis process needs to be performed in a glove box.
Selecting the exposed surface as (004) crystal surface with size of about 1 mm3The niobium arsenide single crystal is added into the quartz tube as a seed crystal. The quartz tube was evacuated to 4X 10-4Pa, then immediately sealed, and the process required placing the quartz tube in a dry ice bath (minus 78 ℃) of dry ice mixed with acetone.
Vertically placing a quartz tube in a vertical growth furnace, and setting the program to be 2 ℃/min to 500 ℃ and then preserving the temperature for 30 min; then heating to 1050 ℃ at the speed of 5 ℃/min, and then preserving heat for 30 days; after the heat preservation is finished, the reaction is stopped and cooled to the room temperature after the reaction is cooled to 500 ℃ at the speed of 5 ℃/min.
By the above experimental procedure, a size of about 3X 5X 4 mm was successfully prepared3The semimetal niobium arsenide monocrystal material.
Example 3
Selecting a material with a molar ratio of 1: 1.05: 0.05 tantalum foil, arsenic powder and iodine powder. And finely crushing the tantalum foil to a thickness of 0.02 mm and a size of 2X 2 mm2. Specifically, 0.543 g of tantalum foil, 0.229 g of arsenic powder and 0.038 g of iodine powder are selected, uniformly mixed and added into a quartz tube, and the process needs to be carried out in a glove box.
Selecting the exposed surface as (004) crystal surface with size of about 1 mm3The tantalum arsenide single crystal is added into the quartz tube as a seed crystal. The quartz tube was evacuated to 4X 10-4Pa, then immediately sealed, and the process required placing the quartz tube in a dry ice bath (minus 78 ℃) of dry ice mixed with acetone.
Vertically placing a quartz tube in a vertical growth furnace, and setting the program to be 2 ℃/min to 500 ℃ and then preserving the temperature for 30 min; then raising the temperature to 1030 ℃ at a speed of 5 ℃/min, and then preserving the heat for 30 days; after the heat preservation is finished, the reaction is stopped and cooled to the room temperature after the temperature is cooled to 500 ℃ at the speed of 5 ℃/min.
By the above experimental procedure, a size of about 4X 5 mm was successfully prepared3The semimetal niobium arsenide monocrystal material.
Example 4
Selecting a material with a molar ratio of 1: 1.05: 0.02 tantalum foil, arsenic powder and iodine powder. And finely crushing the tantalum foil to a thickness of 0.015 mm and a size of 1.5X 1.5 mm2. Specifically, 0.543 g of tantalum foil, 0.092 g of arsenic powder and 0.038 g of iodine powder are selected, uniformly mixed and added into a quartz tube, and the process needs to be carried out in a glove box.
Selecting the exposed surface as (004) crystal surface with size of about 1 mm3The tantalum arsenide single crystal is added into the quartz tube as a seed crystal. The quartz tube was evacuated to 10 deg.C-4Pa, then immediately sealed, and the process required placing the quartz tube in a dry ice bath (minus 78 ℃) of dry ice mixed with acetone.
Vertically placing a quartz tube in a vertical growth furnace, and setting the program to heat up to 450 ℃ at a speed of 2 ℃/min and then preserving the heat for 40 min; then raising the temperature to 1000 ℃ at a speed of 5 ℃/min and then preserving the heat for 40 days; after the heat preservation is finished, the reaction is stopped and the temperature is cooled to 450 ℃ at the speed of 5 ℃/min, and then the reaction is cooled to room temperature.
By the above experimental procedure, a size of about 4X 5 mm was successfully prepared3The semimetal tantalum arsenide single crystal material is exol.
Example 5
Selecting a material with a molar ratio of 1: 1.05: 0.05 tantalum foil, arsenic powder and iodine powder. And finely crushing the tantalum foil to a thickness of 0.02 mm and a size of 2X 2 mm2. Specifically, 0.543 g of tantalum foil, 0.229 g of arsenic powder and 0.038 g of iodine powder are selected and uniformly mixed and added into a quartz tube, and the process needs to be carried out in a glove box.
Selecting the exposed surface as (004) crystal surface with size of about 1 mm3The niobium arsenide single crystal is added into the quartz tube as a seed crystal. The quartz tube was evacuated to 10 deg.C-5The tube was sealed immediately after Pa and the process required placing the tube in a dry ice bath (minus 78 ℃) of dry ice mixed with acetone.
Vertically placing a quartz tube in a vertical growth furnace, and setting the program to be 2 ℃/min to 550 ℃ and then preserving the temperature for 20 min; then heating to 1100 ℃ at a speed of 5 ℃/min, and then preserving heat for 20 days; after the heat preservation is finished, the reaction is stopped and cooled to the room temperature after the reaction is cooled to 550 ℃ at the speed of 5 ℃/min.
Through the above experimental procedures, a size of about4×5×5 mm3The semimetal niobium arsenide monocrystal material.
The above examples are intended to illustrate embodiments of the invention without going beyond the scope of the subject matter of the invention, the scope of protection of which is not limited by the examples. Unless otherwise specifically indicated, the materials and reagents used in the present invention are available from commercial products in the art.
Claims (10)
1. A method for preparing a exol semimetal crystal by a vertical CVT seed crystal method is characterized by comprising the following steps:
mixing massive niobium foil or tantalum foil fine powder with powdery arsenic and iodine to obtain a first mixture;
adding the exol semimetal crystal grains serving as seed crystals into the first mixture to obtain a second mixture;
step three, adding the second mixture as a reaction raw material into a quartz tube, vacuumizing the quartz tube and sealing the quartz tube;
step four, vertically placing the sealed quartz tube in a vertical growth furnace, heating to 450-550 ℃, and then preserving heat for 20-40 min; continuously heating to 1000 ℃ and 1100 ℃, and then preserving the heat for 20-40 days; after the heat preservation is finished, the reaction is stopped after the temperature is slowly cooled to 450-550 ℃, and the reaction is cooled to room temperature.
2. The method of claim 1, wherein: in the first step, in terms of molar ratio, niobium foil or tantalum foil: arsenic powder: iodine powder = 1.00: (1.02-1.05): (0.02-0.05).
3. The method according to claim 1 or 2, characterized in that: in the first step, the massive tantalum foil or niobium foil is a finely crushed small-sized fragment, the thickness of the massive tantalum foil or niobium foil is 0.015-0.025 mm, and the size of the massive tantalum foil or niobium foil is (1.5-2.5) × (1.5-2.5) mm2。
4. The method of claim 3, wherein: in the first step, the thickness of the massive tantalum foil or niobium foil is 0.02 mm, and the size is 2 multiplied by 2 mm2。
5. The method according to claim 1 or 4, characterized in that: in the third step, in the sealing process, the quartz tube is placed in the acetone solution added with the dry ice in the whole process.
6. The method of claim 5, wherein: in the third step, the quartz tube is vacuumized to 10 degrees-5-10-4pa and then sealing the film.
7. The method according to claim 1 or 6, characterized in that: in the fourth step, the temperature is raised to 450-550 ℃ at a speed of 2 ℃/min.
8. The method of claim 7, wherein: in the fourth step, the temperature is raised to 1000-1100 ℃ at a speed of 5 ℃/min.
9. The method of claim 7, wherein: in the fourth step, the temperature is raised to 500 ℃ at a rate of 2 ℃/min.
10. The method of claim 8, wherein: in the fourth step, the temperature is raised to 1050 ℃ at a rate of 5 ℃/min.
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