CN111118605B - Ideal dirac semimetal Cu2HgSnSe4Crystal and growth method and application thereof - Google Patents

Ideal dirac semimetal Cu2HgSnSe4Crystal and growth method and application thereof Download PDF

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CN111118605B
CN111118605B CN201911151400.1A CN201911151400A CN111118605B CN 111118605 B CN111118605 B CN 111118605B CN 201911151400 A CN201911151400 A CN 201911151400A CN 111118605 B CN111118605 B CN 111118605B
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吕洋洋
曹琳
陈延彬
张海军
陈延峰
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Abstract

Ideal DidiRake semimetal Cu2HgSnSe4A crystal, wherein said crystal is tetragonal and the space group is
Figure DDA0002283633750000011
(No.121)，
Figure DDA0002283633750000012
The Cu2HgSnSe4The energy band structure diagram of the crystal is asymmetric between a conduction band and a valence band, only Dirac fermions exist in the conduction band, and Schrodinger fermions and Dirac fermions coexist in the valence band. If the fermi energy is in the conduction band, the transport properties are mainly derived from Dirac fermi. Such a system would help us to obtain relatively clean transport experimental data so that novel transport properties of topological quantum states can be explored. Meanwhile, the linear dispersion relation of electrons near the Dirac point is always maintained in an energy range of about 400mV, and the Dirac cone energy band structure of the linear dispersion has nonlinear response to light waves with a wide range of frequencies. The crystal has great academic value and potential application prospect.

Description

Ideal dirac semimetal Cu2HgSnSe4Crystal and growth method and application thereof
Technical Field
The invention belongs to the technical field of new materials and crystal growth, and particularly relates to ideal Dirac semimetal Cu2HgSnSe4Crystal and its growth method and application.
Background
In more than ten years, a major breakthrough in condensed state physics is to introduce the mathematical topological principle into the basic theory of physics to construct the topological phase change and matter topological phase theory. The research of the topological properties of substances becomes an important direction in condensed physical and material science research. A completely new concept, topological quantum material, is also derived from the method. Due to the unique topological properties of the electronic structure, topological quantum materials can exhibit various quantum effects on a macroscopic scale, and thus have received extensive attention and research from numerous researchers. Since the experimental discovery of two-dimensional graphene in 2004, a series of completely new quantum states, such as Topological insulators (Topological insulators), Topological Dirac semimetals (Topological Dirac semiconductors), Topological Weyl semimetals (Topological Weyl semiconductors), Topological node-Line semimetals (Topological node-Line semiconductors), and the like, were successively discovered. The rapid development of the research of the topological quantum material greatly expands the application range of the quantum field theory on the one hand, and the novel physical phenomenon greatly promotes the development of the basic theory of physics on the other hand; on the other hand, the emergence of topological quantum materials may dominate the development of new generation of electronic components, such as future memory and logic devices, low-loss microwave emission sources, high-precision test systems, quantum computers, and the like.
As an important branch of topological quantum materials, three-dimensional Dirac/Weyl semimetal materials are widely studied due to their unique physical properties. Theoretical prediction Na from 2012 to 20133Bi and Cd3As2Is Dirac semimetal [ z.j.wang, y.sun, x. — q.chen, et al.phys.rev.b 85,195320 (2012); z.j. Wang, h.m.weng, q.s.wu, x.dai, and z.fang, phys.rev.b 88,125427 (2013).]The theory is predicted soon that a series of novel physical properties such as negative magnetoresistance effect, ultrahigh mobility and transport relaxation time three orders of magnitude longer than quantum state life are observed in transport experiments. The theory predicts that the iridium oxide of the Weyl semimetal-magnetic pyrochlore structure and the ferromagnetic HgCr2Se4However, the material has not been proved by experiments due to the limitation of the magnetic material in the angle-resolved photoelectron spectroscopy experiment or the existence of the multi-domain structure in the magnetic material. Until 2015, non-magnetic non-centrosymmetric TaAs family materials were theoretically found to be natural Weyl semimetals [ [ h.weng, c.fang, z.fang, b.a.bernevig, and x.dai, phys.rev.x 5,011029 (2015);
s. -m.huang, s. -y.xu, i.belopolski, et al, nat. commun.6,7373(2015) ]. The compounds in the class are proved to be Weyl semimetals by angle-resolved photoelectron spectroscopy experiments and have negative magnetoresistance effects caused by chiral anomalies. From the current research situation, the novel topological quantum material is discovered through the energy band calculation of the first principle of quantum mechanics, and the aspect of the topological state is proved by utilizing the angle-resolved photoelectric spectrum experiment, so that a great result is achieved. Meanwhile, experimental research work on the aspect of topological state transport is relatively little. In order to realize a device from a topological quantum material, the physical properties of the topological quantum material must be studied in depth from the viewpoint of electric transport, because electronic devices still process electric signals at present. However, it is very difficult to study topological quantum materials from the perspective of electrical transport because most topological quantum materials also have a large amount of conventional schrodinger fermion [ m.n.ali, j.xiong, s.flynn, et al, Nature 514, 205-. This is because Dirac/Weyl fermi is only present in the brillouin zone near some points where symmetry is higher, and mediocre schrodinger fermi is necessarily quantitatively superior. Non-mediocre topological states are difficult to detect in transit, since mediocre body states dominate in transit. In addition, the research on the topological quantum materials from the aspect of transport in the existing reports is still in a very preliminary stage, and many transport phenomena are still greatly controversial. For example, whether the negative magnetoresistance phenomenon can be used as a criterion for observing the chiral anomalous effect in the Weyl semimetal, the quantitative relationship between the negative magnetoresistance effect and the Fermi energy position, the relationship between the high conductivity mobility and the Fermi energy position, and the like. Some of these problems are even lacking in semi-quantitative studies. From the development of future functional devices, the research on the transport properties of topological quantum materials is crucial. If the transport research of the topological quantum material is not further developed, the corresponding device research will not be mentioned.
Based on the above current research, the concept of Ideal Dirac/Weyl semimetal materials (Ideal Dirac/Weyl semi metals) was proposed [ j.ruan, s.k.jian, d.zhang, et al, phys.rev.lett.116, 226801 (2016); ruan, s.jian, h.yao, et al, nat.commun.7,11136(2016) ]. The band characteristics of these materials are that only the Dirac/Weyl fermi ion exists near the fermi energy, and no other mediocre body states exist, while the linear dispersion relation of electrons near the Dirac/Weyl point is maintained over a large energy range. In view of the advantages of the ideal Dirac/Weyl semimetal material, it is necessary to develop such materials.
Disclosure of Invention
In order to improve the problems, the invention provides an ideal Dirac semimetal material-Cu2HgSnSe4Crystal and preparation method and application thereof.
The technical scheme of the invention is as follows:
ideal dirac semimetal Cu2HgSnSe4A crystal which is tetragonal, the space group being
Figure GDA0002432144780000031
According to an embodiment of the present invention, the Cu2HgSnSe4The crystal has an XRD pattern substantially as shown in figure 3.
According to an embodiment of the present invention, the Cu2HgSnSe4The band structure of the crystal is shown in fig. 1, the conduction band and the valence band are asymmetric, only Dirac fermi exists in the conduction band, and Schrodinger fermi and Dirac fermi coexist in the valence band. If the fermi energy is in the conduction band, the transport properties are mainly derived from Dirac fermi. Such a system would help us to obtain relatively clean transport experimental data so that novel transport properties of topological quantum states can be explored. Meanwhile, the linear dispersion relation of electrons near the Dirac point is always maintained in an energy range of about 400mV, and the Dirac cone energy band structure of the linear dispersion has nonlinear response to light waves with a wide range of frequencies.
According to an embodiment of the present invention, the Cu2HgSnSe4The crystal size reaches millimeter level or even centimeter level.
According to an embodiment of the present invention, the Cu2HgSnSe4The crystal is flaky or columnar, has metallic luster and excellent single crystal quality.
The invention also provides a method for growing the crystal, which comprises the following steps: chemical vapor transport or gradient cooling;
the chemical vapor transport method comprises the following steps:
a1) preparing a growth raw material: using Cu2Se, HgSe, Sn and Se are used as initial raw materials, the raw materials are uniformly mixed in a grinding mode, the mixture is filled into a quartz tube, the quartz tube is sealed, and solid-phase sintering is carried out to synthesize the polycrystalline Cu2HgSnSe4As a raw material for growing crystals;
a2)Cu2HgSnSe4crystal growth: taking the polycrystalline Cu prepared in the step a1)2HgSnSe4Mixing the mixture with a transport agent, filling the mixture into a quartz tube, and sealing the quartz tube; placing the sealed quartz tube in a tube furnace with two temperature regions, setting a growth temperature program, and growing to obtain Cu2HgSnSe4A crystal; or
A gradient cooling method, the gradient cooling method comprising the steps of:
b1) preparing a growth raw material: using Cu2Se, HgSe, Sn and Se are used as initial raw materials, the raw materials are uniformly mixed in a grinding mode, the mixture is filled into a quartz tube and sealed, and then solid-phase sintering reaction is adopted to synthesize the polycrystalline Cu2HgSnSe4As a raw material for growing crystals;
b2)Cu2HgSnSe4crystal growth: taking the polycrystalline Cu prepared in the step b1)2HgSnSe4Putting into a quartz tube, and sealing; placing the sealed quartz tube in a tube furnace with two vertical temperature zones, setting a growth temperature program, and growing to obtain Cu2HgSnSe4And (4) crystals.
According to an embodiment of the present invention, in the steps a1, a2), b1 and b2), the quartz tubes have the same or different lengths, are independently 10 to 20cm from each other, and have diameters of 1 to 3 cm.
According to an embodiment of the present invention, in the steps a1, a2), b1, b2), the sealing means are the same or different, and a gas flame, or an acetylene flame, or a hydrogen flame is used independently of each other.
According to an embodiment of the invention, in the step a1) or b1), the temperature of the solid phase sintering reaction is the same or different and is 800-1100 ℃ independently; the reaction times are identical or different and, independently of one another, are from 3 to 10 days.
According to an embodiment of the invention, in step a2), the delivery agent is selected from I2、Br2Or mixtures thereof.
According to the embodiment of the invention, in the step a2), the amount of the transport agent is 0.8-1.5 g of polycrystalline Cu2HgSnSe4In the process, the concentration of the transport agent in the system is 2-30 mg/cm3Preferably 5 to 20mg/cm3。
According to an embodiment of the invention, in step a2), the growth temperature program is set up as: the raw material end is 700 ℃ and 500 ℃, the crystal growth end is 600 ℃ and 400 ℃, and the growth period is 5-15 days.
According to an embodiment of the present invention, in step b2), the head of the quartz tube is tapered.
According to the embodiment of the invention, in the step b2), the initial temperature of crystal growth is 800-1100 ℃, the temperature is kept for 10-30 h, then the temperature is reduced to 400-600 ℃ at the speed of 5-30 ℃/h, then the temperature is reduced to 200-400 ℃ at the speed of 0.2-10 ℃/h, and finally the temperature is naturally reduced; the growth period is 5-15 days.
Preferably, the single crystal is obtained by the following chemical vapor transport method:
a'1) preparing a growth raw material: using Cu2Se, HgSe, Sn and Se powder as initial raw materials, according to Cu2Mixing Se, HgSe, Sn, Se according to the molar ratio of 1:1:1:2, uniformly mixing by adopting a mortar grinding mode, filling into a quartz tube, and vacuumizing by adopting a mechanical pump and a molecular pump (10)-3～10-4Pa) sealing, and synthesizing the polycrystalline Cu by adopting a solid-phase sintering reaction2HgSnSe4As a raw material for growing crystals;
a'2)Cu2HgSnSe4crystal growth: taking the polycrystalline Cu prepared in the step a'1)2HgSnSe4Mixing with transport agent, filling into quartz tube prepared in advance, and vacuum-pumping (10)-3～10-4Pa) sealing; placing the sealed quartz tube in a tube furnace with two temperature regions, setting a growth temperature program, and growing for a certain period to obtain Cu2HgSnSe4And (4) crystals.
Preferably, the single crystal is obtained by a gradient cooling method as follows:
b'1) preparation of growth raw materials: using Cu2Se, HgSe, Sn and Se powder as initial raw materials, based on Cu2Mixing Se, HgSe, Sn, Se according to the molar ratio of 1:1:1:2, uniformly mixing by adopting a mortar grinding mode, filling into a quartz tube, and vacuumizing by adopting a mechanical pump and a molecular pump (10)-3～10-4Pa) sealing, and synthesizing the polycrystalline Cu by adopting a solid-phase sintering reaction2HgSnSe4As a raw material for growing crystals;
b'2)Cu2HgSnSe4crystal growth: weighing the polycrystalline Cu prepared in the step b'1)2HgSnSe4Put into a quartz tube under vacuum (10)-3～10-4Pa) sealing; placing the sealed quartz tube in a tube furnace with two vertical temperature zones, setting a growth temperature program, and growing for a certain period to obtain Cu2HgSnSe4And (4) crystals.
The invention also provides Cu prepared by the method2HgSnSe4And (4) crystals. The invention also provides Cu as described above2HgSnSe4Use of the crystal as a Dirac semimetal material.
According to the embodiment of the invention, the Dirac semimetal material is used in the fields of future memory and logic devices, novel spintronic devices, low-loss microwave emission sources, high-precision test systems, quantum computers and the like.
Compared with the prior art, the invention has the advantages that:
(1) cu provided by the invention2HgSnSe4The crystal vapor transport growth method has the advantages of high purity of the grown crystal, high quality, low cost, simple device, easy operation and the like. The gradient cooling growth method has the advantages of large crystal size, high purity, high quality, low cost, strong operability and the like. Both methods can be used for industrial production.
(2) Cu prepared by the invention2HgSnSe4The crystal material has high crystal quality, and the crystal can be used as an ideal system to research the novel transport performance of the Dirac semimetal material. This is to clarify the topological quantityThe inherent physical properties of the sub-materials are of great significance.
(3) Cu prepared by the invention2HgSnSe4The crystal as an ideal Dirac semimetal material has important application prospect in the fields of future storage and logic devices, novel spintronic devices, low-loss microwave emission sources, high-precision test systems, quantum computers and the like.
(4) Cu prepared by the invention2HgSnSe4Only Dirac fermions are present in the conduction band, while schrodinger and Dirac fermions coexist in the valence band. If the fermi energy is in the conduction band, the transport properties are mainly derived from Dirac fermi. Such a system would help us to obtain relatively clean transport experimental data so that novel transport properties of topological quantum states can be explored. Therefore, the crystal of the invention has great academic value and potential application prospect.
Drawings
FIG. 1 shows an ideal Dirac semi-metallic material Cu prepared according to examples 1 and 2 of the present invention2HgSnSe4Band structure of the crystal.
FIG. 2(a) shows Cu grown in example 1 of the present invention2HgSnSe4An optical photograph of the crystal; 2(b) (c) is Cu grown in example 2 of the present invention2HgSnSe4An optical photograph of the crystal; (c) XRD pattern.
FIG. 3 shows Cu grown in example 1 of the present invention2HgSnSe4XRD pattern of the crystal.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
High-purity (more than 3N) Cu is adopted in the experiment2Se, HgSe, Sn and Se powders as raw materials, transport agents I used therefor2And Br2Are all high-purity (more than 3N) reagents, and the quartz tube for growing the crystal is made of high-purity (more than 3N) quartz.
Example 1 delivery agent I2Under the condition of Cu2HgSnSe4Growing Cu by using powder as raw material2HgSnSe4Crystal
Weighing 0.02mol of Cu2Se powder (4.1212g), HgSe powder (5.591g) in an amount of 0.02mol, Sn powder (2.3742g) in an amount of 0.02mol, and Se powder (3.1584g) in an amount of 0.04mol were mixed and charged into a quartz tube prepared in advance. Sealing the copper alloy in a state of adopting a mechanical pump and a molecular pump to pump vacuum, and carrying out high-temperature solid-phase sintering reaction at 900 ℃ for 5 days to prepare the Cu2HgSnSe4The powder is used as a growth raw material. Then weighing about 1g of Cu2HgSnSe4Powder with 100mg of delivery agent I2(concentration 5 mg/cm)3) The two were ground and mixed uniformly, and then they were put into a quartz tube (length: 10cm, diameter: 2cm) prepared in advance. The quartz tube is sealed and then placed in a two-temperature-zone tube furnace, growth temperature programs of 400 ℃ (growth end) -500 ℃ (raw material end) are set, and through a growth cycle of 10 days, millimeter-scale high-quality Cu can be obtained by natural cooling2HgSnSe4Large single crystals, the largest dimension of which is around 2mm, are shown in fig. 2 (a).
As shown in fig. 3, analysis by X-ray diffraction test (XRD) revealed that the above-prepared crystal was tetragonal. All diffraction peaks were (00l) peaks, indicating that the sample grew along the ab-plane and no hetero-peaks were present.
Example 2 gradient Cooling with Cu2HgSnSe4Growing Cu by using powder as raw material2HgSnSe4Crystal
Weighing 0.02mol of Cu2Se powder (4.1212g), HgSe powder (5.591g) 0.02mol, Sn powder (2.3742g) 0.02mol and Se powder (3.1584g) 0.04mol are mixed uniformly and put into a quartz tube prepared in advance, the quartz tube is sealed in a state of vacuum by a mechanical pump and a molecular pump, and the high-temperature solid-phase sintering reaction is carried out at 900 ℃ for 5 days to prepare Cu2HgSnSe4The powder is used as a growth raw material. Then weighing about 10 g of Cu2HgSnSe4The powder was packed into a quartz tube (length 10cm, diameter 2cm, head conical) prepared in advance. Sealing the quartz tube, placing the sealed quartz tube in a vertical two-temperature-zone tube furnace, setting a temperature program as initial 950 ℃, keeping the temperature for 12 hours, cooling to 500 ℃ at a speed of 10 ℃/h, cooling to 300 ℃ at a speed of 2 ℃/h, and finally naturally cooling to obtain centimeter-grade Cu with high quality2HgSnSe4Large single crystals, with a maximum size of around 15mm, are shown in fig. 2 (b).
As shown in fig. 2(c), the crystals prepared above were revealed to be tetragonal phase by X-ray diffraction test (XRD) analysis. All diffraction peaks were (00l)) indicating that the sample grew along the ab-plane and no hetero-peaks were present.
Example 3, Cu2HgSnSe4Energy band calculation of crystalline Dirac semimetal properties
By first principles, we calculated the Cu prepared in examples 1 and 22HgSnSe4The band structure of the crystal is shown in figure 1, and as a result, the conduction band and the valence band are asymmetric, only Dirac fermi exists in the conduction band, and Schrodinger fermi and Dirac fermi coexist in the valence band. If the fermi energy is in the conduction band, the transport properties are mainly derived from Dirac fermi. Such a system would help us to obtain relatively clean transport experimental data so that novel transport properties of topological quantum states can be explored. Meanwhile, the linear dispersion relation of electrons near a Dirac point is always maintained in an energy range of about 400mV, and a Dirac cone energy band structure of linear dispersion has nonlinear response of a large range of frequencies to light waves, so that the method is expected to be applied to a low-loss microwave emission source and the like.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (11)

1.Cu2HgSnSe4Crystal as Dirac semimetal materialThe use of (a);
the crystal is tetragonal system, and the space group is
Figure DEST_PATH_IMAGE002
(No. 121)，a=5.8224(3) Å，c=11.4219(6) Å，V=387.21(3) Å3。
2. Use according to claim 1, wherein the Dirac semimetal material is used in the fields of future memory and logic devices, new spintronic devices, low-loss microwave emission sources, high-precision test systems, quantum computers.
3. Use according to claim 1, characterized in that the Cu2HgSnSe4The conduction band and the valence band of the crystal are asymmetric, only Dirac fermions exist in the conduction band, and Schrodinger fermions and Dirac fermions coexist in the valence band;
the linear dispersion relation of electrons near the Dirac point is always maintained in the energy range of 400mV, and the Dirac cone energy band structure of the linear dispersion has nonlinear response to the optical wave with wide range of frequencies.
4. Use according to claim 1, characterized in that the Cu2HgSnSe4The crystals are in the shape of a plate or a column.
5. Use according to claim 1, characterized in that the Cu2HgSnSe4The crystal is prepared by the following method: including chemical vapor transport or gradient cooling;
the chemical vapor transport method comprises the following steps:
a1) preparing a growth raw material: using Cu2Se, HgSe, Sn and Se are used as initial raw materials, the raw materials are uniformly mixed in a grinding mode, the mixture is filled into a quartz tube, the quartz tube is sealed, and solid-phase sintering is carried out to synthesize the polycrystalline Cu2HgSnSe4As a raw material for growing crystals;
a2）Cu2HgSnSe4crystalGrowing: taking the polycrystalline Cu prepared in the step a1)2HgSnSe4Mixing the mixture with a transport agent, filling the mixture into a quartz tube, and sealing the quartz tube; placing the sealed quartz tube in a tube furnace with two temperature regions, setting a growth temperature program, and growing to obtain Cu2HgSnSe4A crystal; or
A gradient cooling method, the gradient cooling method comprising the steps of:
b1) preparing a growth raw material: using Cu2Se, HgSe, Sn and Se are used as initial raw materials, the raw materials are uniformly mixed in a grinding mode, the mixture is filled into a quartz tube and sealed, and then solid-phase sintering reaction is adopted to synthesize the polycrystalline Cu2HgSnSe4As a raw material for growing crystals;
b2）Cu2HgSnSe4crystal growth: taking the polycrystalline Cu prepared in the step b1)2HgSnSe4Putting into a quartz tube, and sealing; placing the sealed quartz tube in a tube furnace with two vertical temperature zones, setting a growth temperature program, and growing to obtain Cu2HgSnSe4And (4) crystals.
6. Use according to claim 5, characterized in that in step a1) or b1), the temperature of the solid phase sintering reaction is the same or different and is 800 to 1100 ℃ independently of each other.
7. Use according to claim 5, wherein in step a2), the delivery agent is selected from I2、Br2Or mixtures thereof.
8. The use according to claim 7, wherein in the step a2), the amount of the transport agent is 0.8-1.5 g of polycrystalline Cu2HgSnSe4In the process, the concentration of the transport agent in the system is 2-30 mg/cm3。
9. Use according to claim 5, characterized in that in step a2), the growth temperature program is set up as: the raw material end is 700-500 ℃, and the crystal growth end is 600-400 ℃.
10. The use according to claim 5, wherein in step b2), the initial temperature of crystal growth is 800-1100 ℃, after heat preservation for 10-30 h, the temperature is reduced to 400-600 ℃ at a speed of 5-30 ℃/h, and then the temperature is reduced to 200-400 ℃ at a speed of 0.2-10 ℃/h.
11. Use according to any one of claims 5 to 10, characterized in that the Cu is2HgSnSe4The crystal is prepared by the following method:
b'1) preparation of growth raw materials: using Cu2Se, HgSe, Sn and Se powder as initial raw materials, based on Cu2Mixing materials according to the molar ratio of Se to HgSe to Se =1:1:1:2, uniformly mixing the materials by adopting a mortar grinding mode, filling the mixture into a quartz tube, and vacuumizing the quartz tube by adopting a mechanical pump and a molecular pump by 10-3~10-4Pa sealing, and synthesizing polycrystal Cu by solid phase sintering reaction2HgSnSe4As a raw material for growing crystals;
b'2）Cu2HgSnSe4crystal growth: weighing the polycrystalline Cu prepared in the step b'1)2HgSnSe4Filling into a quartz tube under vacuum 10-3~10-4Sealing with Pa; placing the sealed quartz tube in a tube furnace with two vertical temperature zones, setting a growth temperature program, and growing for a certain period to obtain Cu2HgSnSe4And (4) crystals.
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