CN113564706B - RhO of trigonal system 2 Crystal, preparation method and application thereof - Google Patents
RhO of trigonal system 2 Crystal, preparation method and application thereof Download PDFInfo
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- CN113564706B CN113564706B CN202110753154.8A CN202110753154A CN113564706B CN 113564706 B CN113564706 B CN 113564706B CN 202110753154 A CN202110753154 A CN 202110753154A CN 113564706 B CN113564706 B CN 113564706B
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- 239000013078 crystal Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000012212 insulator Substances 0.000 claims abstract description 23
- 230000007704 transition Effects 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 230000008878 coupling Effects 0.000 claims abstract description 5
- 238000010168 coupling process Methods 0.000 claims abstract description 5
- 238000005859 coupling reaction Methods 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- 239000002243 precursor Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910000314 transition metal oxide Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000002547 anomalous effect Effects 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Abstract
The invention discloses a RhO 2 Crystals of RhO 2 The crystal belongs to a trigonal system, and the space group isHaving a lattice constant ofThe crystals exhibit novel transport properties, i.e. behave as a metal at high temperatures, with metal insulator transitions at 100-150K, and insulator behavior at temperatures below this. Analysis shows that the metal insulator transition is a Mott transition resulting from both electron association and spin-orbit coupling, i.e., rhO of the structure 2 Is a mote insulator.
Description
Technical Field
The invention belongs to the technical field of new materials and crystal growth, and in particular relates to a trigonal RhO 2 Crystals, and methods of making and using the same.
Background
4d and 5d transition metal oxide materials have been the focus of research in basic science and application science due to unique electronic properties. For example, moO 2 Exhibit a large magnetoresistive effect (q.chen, z.f.lou, et al, phys.rev.b 102,165133 (2020).); reO (Reo) 2 Is a novel topology material (s.s. wang, y.liu, et al, nat.commun.8,1844 (2017)); ruO (Ruo) 2 Not only is a node line topology semi-metallic material with a flat band characteristic surface state, it also exhibits anomalous antiferromagnetic properties (V.Jovic, R.J.Koch, S.K.Panda, et al, phys. Rev. B98,241101 (R) (2018); Z.H.Zhu, J.Strempfer, et al, phys. Rev. Lett.122,017202 (2019)); irO (IrO) 2 Has a strong spin orbit coupling (J.N.Nelson, J.P.Ruf, et al, phys. Rev. Materials.3,064205 (2019)); hfO (HfO) 2 Flat polar phonon bands in the film induce a robust, independently reversible dipole, thus giving it ferroelectricity (h.j.lee, m.lee, et al, science.369,1343-1347 (2020)). These properties are of great significance for the development of research fields such as topological physics, associative electronics, spintronics, etc. Due to the special electronic properties, the 4d and 5d transition metal oxides have great application potential in the aspects of catalysts, energy storage and the like. In addition, its unique physical properties provide more possibilities for developing new generation of functional devices.
The structure of the material is closely related to the performance of the material, and determines the function and application of the material. Studies have reported that 4d and 5d transition metal oxides having the same chemical formula but different structures also show a great difference in properties. By PtO 2 For example, experimental studies have shown that PtO 2 Has three phases, namely an alpha phase, a beta phase and a beta' phase; wherein PtO of alpha phase and beta phase 2 Exhibit high catalytic performance, and respectively have hexagonal CdI 2 Structure and orthogonalization CaCl 2 Structure (R.Kim, B.J.Yang, et al, phys.chem.Phys.8, 1566-1574 (2006)); ptO of beta' phase 2 Has a tetragonal rutile structure, but is a dirac half metal (r.kim, b.j. Yang, et al, phys. Rev. B99,045130 (2019).).
RhO 2 Is a 4d transition metal oxide having a rutile structure (tetragonal system) and having a space group of P4 2 /mn, is mainly used as an electrocatalyst (V.Schu nemann, B.Adelman, et al Catalysis Letters, 259-265 (1994)).
The invention discovers a new structural RhO 2 Single crystals of this new structureRhO 2 The discovery of the crystal has important research and application values in the aspects of associated physics, spintronics, high-temperature superconducting exploration and the like, can promote the development of basic disciplines, and on the other hand, the material can be also used for developing new-generation functional devices, such as temperature-sensitive sensors or switches, low-energy-consumption electronic elements, novel electronic logic elements and the like.
Disclosure of Invention
The invention aims to provide a trigonal RhO 2 Crystal and RhO based on trigonal system prepared by high-temperature aqueous solution method 2 Method for preparing RhO by adjusting solution temperature and preparation time 2 And (5) a crystal.
The technical scheme of the invention is as follows:
RhO (RhO) 2 Crystals of RhO 2 The crystal belongs to a trigonal system, and the space group is(No. 164) having a lattice constant +.>
According to the invention, the crystal exhibits metallic behavior at high temperatures, with metallic insulator transitions occurring at 100-150K, below which the insulator behavior is exhibited.
According to the Mott jump conductance theory, the formula is as follows: ρ (T) =aexp (1/T 1/4 ) Wherein ρ (T) is the resistivity at temperature T, a being a constant; t is the temperature (in K);
according to Mott jump conductance theory, it is shown by resistance temperature dependent test analysis that the metal insulator transition of the crystal is a Mott transition caused by electron association and spin-orbit coupling, namely the RhO 2 The crystal is a type of mote insulator.
According to the invention, the RhO 2 The crystal is single crystal, the RhO 2 The single crystal has at least one dimension of the order of millimeters.
In accordance with the present invention,the RhO is 2 The single crystal has at least one dimension of a size of 1mm or more, preferably 1 to 4mm, for example, 1.0mm, 1.5mm, 1.8mm, 2.0mm, 2.5mm, 3.0mm, 3.5mm, 4.0mm.
According to the invention, the monocrystal is flaky, light yellow, sharp in XRD diffraction peak, narrow in half-peak width and good in monocrystal quality.
According to the invention, the RhO 2 The crystals have an EDS pattern substantially as shown in figure 1b, or figure 2b, or figure 3 b.
According to the invention, the RhO 2 The crystals have an XRD pattern substantially as shown in figure 1c, or figure 2c, or figure 3 c.
The invention also provides the RhO 2 The preparation method of the crystal comprises the following steps:
by adopting a high-temperature water solution method, A x RhO 2 Heating in deionized water to prepare RhO 2 A crystal; wherein A is selected from one of K, rb and Cs; x is selected from a number between 0.2 and 0.9, preferably 0.4 to 0.8.
Wherein the A x RhO 2 Is prepared by methods commonly used in the art, for example by the methods described in the paper S.H.Yao et al, structure and physical properties of K 0.63 RhO 2 A process for the preparation of single crystals, AIP Advances 2,042140 (2012) (DOI: 10.1063/1.4767464).
According to the invention, A is preferably Cs; x is a fraction, for example x is 0.2, 0.63, 0.5, 0.72, 0.8, 0.85, 0.9.
According to the invention, the A x RhO 2 The mass volume ratio of the deionized water to the deionized water is 30-100mg/L, preferably 50mg/L.
According to the present invention, the heating temperature is 30-100deg.C, preferably 60-90deg.C, for example, 30 deg.C, 40 deg.C, 50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 100deg.C; the heating time is 0.5h-10h, for example, 0.5h, 1h, 2h, 4h, 5h, 7h, 8h, 9h, 10h.
The invention also provides the RhO 2 The application of the monocrystal is applied to electronic components, preferably a temperature-sensitive sensor or a switch;or in low-power electronic components and electronic logic components.
Compared with the prior art, the invention has the advantages that:
(1) RhO of the invention 2 The crystal has a new structure which has never been reported before, namely in a trigonal system, the space group is(No. 164) lattice constant +.>The crystals exhibit novel transport properties, i.e. behave as a metal at high temperatures, with metal insulator transitions at 100-150K, and insulator behavior at temperatures below this. Theoretical fitting analysis shows that the metal insulator transition is a Mott transition caused by electron association and spin-orbit coupling, namely RhO with new structure 2 Is a mote insulator.
(2) RhO of the invention 2 The size of the single crystal reaches millimeter level, and the single crystal has high crystal quality.
(3) RhO of the invention 2 The preparation method of the high-temperature solution of the crystal has the advantages of simple device, easy operation and the like.
(4) The RhO is 2 The crystal is used as a Mott insulator material, has important research value on the aspects of associated physics, spintronics, high-temperature superconducting exploration and the like, can promote the development of basic disciplines, and can be used for developing new-generation functional devices, such as temperature-sensitive sensors or switches, low-energy-consumption electronic elements and novel electronic logic elements.
Drawings
FIG. 1 shows RhO prepared in example 1 of the present invention 2 An (a) photomicrograph of a single crystal; (b) EDS maps; (c) XRD pattern; (d) a temperature dependence curve of the resistance.
FIG. 2 is a RhO prepared in example 2 of the present invention 2 An (a) photomicrograph of a single crystal; (b) EDS maps; (c) XRD pattern; (d) a temperature dependence curve of the resistance.
FIG. 3 is a RhO prepared in example 3 of the present invention 2 An (a) photomicrograph of a single crystal; (b) EDS maps; (c) XRD pattern; (d) a temperature dependence curve of the resistance.
Detailed Description
The technical scheme of the invention will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
In the experiment, water is high-purity deionized water, and a precursor A x RhO 2 (a=k, rb, cs) can be prepared by a person skilled in the art according to the prior art, see for example paper s.h. yao et al Structure and physical properties of K 0.63 RhO 2 single crystals,AIP Advances 2,042140(2012)(DOI：10.1063/1.4767464)。
Example 1
Cs by high temperature solution method 0.5 RhO 2 Preparation of RhO by single crystal as precursor 2 Crystal body
Taking 5mg Cs 0.5 RhO 2 Putting the crystal into a beaker, pouring 100ml of deionized water into the beaker, putting the beaker into a heat-collecting type constant-temperature heating magnetic stirrer, setting the heating temperature to be 60 ℃, and obtaining the new structure RhO with millimeter level, flat surface and luster after 1h 2 The single crystal had a maximum size of about 3mm, and the optical photograph thereof was shown in FIG. 1 (a).
As shown in FIG. 1 (b), the X-ray energy spectrum analysis (EDS) test shows that the crystal only contains Rh and O elements; as shown in fig. 1 (c), according to the X-ray diffraction (XRD) test result, the diffraction peak was sharp and the half-width was narrow, indicating that the above-mentioned preparation substance was single crystal; all diffraction peaks were (00 l) peaks, indicating that the sample grew along the ab-plane and no impurity peaks were present. As shown in FIG. 1 (d), the above-mentioned crystals were measured by a comprehensive property measurement System (PPMS)The resistivity at 2-300K indicates that the transport properties of the above crystals exhibit insulator behavior. The fitting result of the upper right corner of FIG. 1 (d) shows that the RhO 2 Is a mote insulator.
Example 2
Cs by high temperature solution method 0.5 RhO 2 Preparation of RhO by single crystal as precursor 2 Crystal body
Taking 5mg Cs 0.5 RhO 2 Putting the crystal into a beaker, pouring 100ml of deionized water into the beaker, putting the beaker into a heat-collecting type constant-temperature heating magnetic stirrer, setting the heating temperature to 90 ℃, and obtaining the new-structure RhO with millimeter level, flat surface and luster after 1h 2 The single crystal had a maximum size of about 3mm, and the optical photograph thereof was shown in FIG. 2 (a).
As shown in FIG. 2 (b), the X-ray energy spectrum analysis (EDS) test shows that the crystal contains only Rh and O elements. As shown in fig. 2 (c), according to the X-ray diffraction (XRD) test result, the diffraction peak was sharp and the half-width was narrow, indicating that the above-mentioned preparation substance was single crystal; all diffraction peaks were (00 l) peaks, indicating that the sample grew along the ab-plane and no impurity peaks were present. As shown in FIG. 2 (d), the resistivity of the above crystal at 2-300K was measured by a comprehensive property measurement system (PPMS), and the result showed that the transport property of the above crystal exhibited an insulator behavior. The fitting result in the upper right corner of FIG. 2 (d) shows that the RhO 2 Is a mote insulator.
Example 3
Cs by high temperature solution method 0.5 RhO 2 Preparation of RhO by single crystal as precursor 2 Crystal body
Taking 5mg Cs 0.5 RhO 2 Putting the crystal into a beaker, pouring 100ml deionized water into the beaker, putting the beaker into a heat-collecting type constant-temperature heating magnetic stirrer, setting the heating temperature to be 60 ℃, and obtaining the new-structure RhO with millimeter level, flat surface and luster after 2 hours 2 The maximum size of the single crystal was about 4mm, and the optical photograph thereof was shown in FIG. 3 (a).
As shown in FIG. 3 (b), the X-ray energy spectrum analysis (EDS) test shows that the crystal contains only Rh and O elements. As shown in fig. 3 (c), according to X-ray diffraction (XRD) The test result shows that the diffraction peak is sharp and the half-width is very narrow, and the prepared substance is single crystal; all diffraction peaks were (00 l) peaks, indicating that the sample grew along the ab-plane and no impurity peaks were present. As shown in FIG. 3 (d), the resistivity of the above crystal at 2-300K was measured by a comprehensive property measurement system (PPMS), and the result showed that the transport property of the above crystal exhibited an insulator behavior. The fitting result in the upper right corner of FIG. 3 (d) shows that the RhO 2 Is a mote insulator.
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, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (12)
1. RhO (RhO) 2 A crystal, characterized in that the RhO 2 The crystal belongs to a trigonal system, and the space group isThe lattice constants of the two layers are a=3.1 a, b=3.1 a and c=4.4 a;
the crystals exhibit metallic behavior at high temperatures, with metallic insulator transitions occurring at 100-150K, below which the insulator behavior is exhibited.
2. The crystal according to claim 1, wherein the formula is:wherein ρ (T) is the resistivity at temperature T, a being a constant; t is the temperature in K;
according to Mott jump conductance theory, analysis by resistance temperature dependence test shows that the metal insulator transition of the crystal is a Mott transition caused by electron association and spin-orbit coupling, namely the RhO 2 The crystal is a type of mote insulator.
3. According to claim 1Is characterized in that the RhO is 2 The crystal is single crystal, rhO 2 The single crystal has at least one dimension of the order of millimeters.
4. The crystal of claim 3 wherein the RhO 2 The single crystal has at least one dimension of 1mm or more.
5. The crystal of claim 4 wherein the RhO 2 The single crystal has at least one dimension of 1-4. 4 mm.
6. A crystal according to claim 3, wherein the single crystal is in the form of a sheet, yellowish.
7. RhO according to any one of claims 1 to 6 2 The preparation method of the crystal is characterized by comprising the following steps: will A x RhO 2 Heating in deionized water to prepare RhO 2 A crystal;
wherein A is selected from one of K, rb and Cs; x is selected from a number between 0.2 and 0.9.
8. The method of claim 7, wherein a is x RhO 2 The mass volume ratio of the deionized water to the deionized water is 30-100mg/L.
9. The method of claim 7, wherein the heating temperature is 30-100 ℃.
10. RhO according to any one of claims 1 to 6 2 The crystal is applied to electronic components.
11. Use according to claim 10 for a temperature sensitive sensor or switch.
12. The use according to claim 10, in low-power electronic components and electronic logic components.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007083576A1 (en) * | 2006-01-17 | 2007-07-26 | Matsushita Electric Industrial Co., Ltd. | Thermoelectric material, thermoelectric converter using same, and electronic device and cooling device comprising such thermoelectric converter |
| CN108531974A (en) * | 2018-04-17 | 2018-09-14 | 南京大学 | A kind of large scale Rb0.5RhO2Or Cs0.5RhO2The growing method of crystal |
| CN113149093A (en) * | 2021-03-11 | 2021-07-23 | 南京大学 | RhO of hexagonal system2Crystal, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6881260B2 (en) * | 2002-06-25 | 2005-04-19 | Micron Technology, Inc. | Process for direct deposition of ALD RhO2 |
| JP2020001997A (en) * | 2017-08-21 | 2020-01-09 | 株式会社Flosfia | Manufacturing method of crystal film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007083576A1 (en) * | 2006-01-17 | 2007-07-26 | Matsushita Electric Industrial Co., Ltd. | Thermoelectric material, thermoelectric converter using same, and electronic device and cooling device comprising such thermoelectric converter |
| CN108531974A (en) * | 2018-04-17 | 2018-09-14 | 南京大学 | A kind of large scale Rb0.5RhO2Or Cs0.5RhO2The growing method of crystal |
| CN113149093A (en) * | 2021-03-11 | 2021-07-23 | 南京大学 | RhO of hexagonal system2Crystal, preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Enhanced thermoelectric properties in a layered rhodium oxide with a trigonal symmetry;Kobayashi, W.;Phys. Rev. B;第76卷(第24期);245102 * |
| 层状三角晶格氧化物KxRhO2晶体的生长与物性研究;张滨滨;中国博士学位论文全文数据库工程科技Ⅰ辑(第8期);B014-405 * |
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