CN112897568B - Layered copper hydroxychloride powder material and preparation method thereof - Google Patents
Layered copper hydroxychloride powder material and preparation method thereof Download PDFInfo
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- CN112897568B CN112897568B CN202110323216.1A CN202110323216A CN112897568B CN 112897568 B CN112897568 B CN 112897568B CN 202110323216 A CN202110323216 A CN 202110323216A CN 112897568 B CN112897568 B CN 112897568B
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- WXPGPKJWYVVOTR-UHFFFAOYSA-N copper;hypochlorous acid Chemical compound [Cu].ClO WXPGPKJWYVVOTR-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000000463 material Substances 0.000 title claims abstract description 38
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910003460 diamond Inorganic materials 0.000 claims description 17
- 239000010432 diamond Substances 0.000 claims description 17
- 230000009471 action Effects 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 37
- 239000007788 liquid Substances 0.000 abstract description 12
- 238000009987 spinning Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- -1 hydroxy halide Chemical class 0.000 abstract description 4
- 238000001308 synthesis method Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000000696 magnetic material Substances 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 230000005469 synchrotron radiation Effects 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000010979 ruby Substances 0.000 description 4
- 229910001750 ruby Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000005283 ground state Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910019891 RuCl3 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910003118 ZnCu3(OH)6Cl2 Inorganic materials 0.000 description 1
- 229910001563 bainite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/04—Halides
- C01G3/05—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention relates to a layered copper hydroxychloride powder material and a preparation method thereof, belonging to the technical field of preparation of quasi-two-dimensional layered metal hydroxy halide crystal materials. Pure copper hydroxychloride (Cu (OH) Cl) crystal powder with a layered monoclinic structure is used as an initial raw material, the initial raw material is pressurized to 18.7-28.4 GPa in a high-pressure Device (DAC), and the pressure is relieved to normal pressure, so that two powder materials with different structures and mixed coexistence of copper hydroxychloride (Cu (OH) Cl) are obtained. The invention obtains the copper hydroxychloride Cu (OH) Cl crystal material with a layered orthogonal structure which can still exist stably under normal pressure for the first time by a high-pressure synthesis method, and is expected to be applied to the fields of quantum spinning liquid, spinning electronics, frustrated magnetic materials and the like; and has the advantages of simple process, room temperature synthesis, short synthesis time, high repeatability and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of quasi-two-dimensional layered metal hydroxy halide crystal materials, and particularly relates to a method for synthesizing a layered orthogonal structured copper hydroxychloride (Cu (OH) Cl) crystal material under high pressure to obtain the layered orthogonal structured copper hydroxychloride (Cu (OH) Cl) crystal material which can exist stably under normal pressure.
Background
The triangular lattice antiferromagnet material is the main research object of the magnetic resistance material, and has many newSuch as quantum spin liquids; quantum spin liquids are a novel magnetic ground state proposed by p.w. anderson in 1973; it means that a new quantum state with magnetic order can not appear in the system under the condition of zero temperature because of strong quantum fluctuation. Compared with the traditional magnetic ordered material, the ground state of the quantum spinning liquid is not represented by a completely determined order parameter, and meanwhile, no symmetry is broken, and the phase category cannot be explained by the Landman phase transition theory. With the intensive research on quantum spinning liquid, the quantum spinning liquid is found to be helpful to some extent for understanding the mechanism of high-temperature superconductivity and quantum critical phenomenon. In addition, the quantum spinning liquid is also a very typical topological ground state, and the quantum spinning liquid is expected to be realized in quantum computation of topological protection. The quantum spin liquid candidate materials discovered so far are: (1) cage structure compound material: ZnCu3(OH)6Cl2、ZnCu3(OH)6FCl、ZnCu3(OH)6FBr and the like; (2) triangular lattice compound material: YbMgGaO4、YbZnGaO 4Etc.; (3) kitaev material: alpha-RuCl3。
The triangular lattice cu (oh) Cl has a magnetodielectric effect and possibly multiferroic transitions, which is called mineral bainite. In past studies, one has identified unconventional magnetic transitions and their relationship to the geometric frustration in the transition metal hydroxyhalide series M (oh) X, where M represents the ion: cu2+、Ni2+、Co2+、Fe2+And Mn2+And X represents a halogen ion: cl-、Br-Or I-These hydroxy salts are widely found in nature as minerals and biominerals.
The high pressure science is to make the substance in a higher pressure environment, and then observe the change of the physical and chemical properties of the material under the condition of extremely high pressure by changing the pressure environment. The high pressure can shorten the atomic distance and change the electronic structure and spatial arrangement of the material, thereby causing the material to have different transformation from the normal pressure structure and property, or causing the material to generate a new substance structure. A Diamond Anvil Cell (DAC) is an important working instrument in high-voltage research. Bridgman anvil was designed by professor p.w. bridgman of the harvard university in the united states as early as the 30's 20 th century. According to the large-mass support principle, the DAC generates a high-pressure environment by pressing sample cavities in the upper diamond anvil and the lower diamond anvil, and the smaller the size of the diamond anvil surface is, the larger the generated pressure is. The pressure of the diamond anvil can reach 10GPa at the early stage, the pressure can reach 1TPa at present, and the static temperature can also reach more than 6000K because the secondary anvil is introduced. The diamond anvil cell mainly comprises three parts: the diameter of the two diamond anvil blocks is about 0.1 mm-1 mm, and most of the two diamond anvil blocks select the diamond with moderate price and good light transmittance in the experiment. The most commonly used method for calibrating the pressure of the diamond anvil at present comprises the following steps: (1) a phase change method, (2) an equation of state method, and (3) a spectroscopic method. The most common method is spectroscopy, which is to calibrate the pressure in the diamond pressing cavity by using the fluorescence of the ruby according to the dependence of the peak position of the R1 linear fluorescence peak of the ruby on the temperature and the pressure. The pressure transmission medium can be divided into solid, liquid and gas states according to the material form; the solid pressure transmission medium comprises NaCl, KBr, MgO and the like; the liquid pressure transmission medium comprises silicon oil, methanol, ethanol and the like, and the gaseous pressure transmission medium comprises gas substances such as H2, He, Ne, Ar and the like; from the viewpoint of the ability to transmit hydrostatic pressure, gaseous pressure-transmitting media are preferred, liquid being the next to solid being the last.
The method of the invention obtains the layered orthogonal structure copper hydroxychloride (Cu (OH) Cl) powder material which can stably exist under normal pressure for the first time through a high-pressure synthesis method, and has not been reported before.
Disclosure of Invention
The invention provides a simple method for preparing copper hydroxychloride (Cu (OH) Cl) powder material and a high-pressure synthesis method thereof, aiming at overcoming the problems and defects existing in the background technology, the method takes pure layered monoclinic structured copper hydroxychloride (Cu (OH) Cl) crystal powder as an initial raw material, and adopts a diamond anvil cell press to prepare Cu (OH) Cl mixed powder at high pressure and room temperature, wherein the Cu (OH) Cl mixed powder material with a layered orthorhombic structure is difficult to obtain under normal pressure.
The copper (Cu (OH) chloride hydroxide powder material is a Cu (OH) Cl mixed powder material with a layered monoclinic structure and a layered orthorhombic structure, is different from a film in the prior art and is powder, and the layered orthorhombic structure Cu (OH) Cl crystal structure is stable at normal temperature and normal pressure.
The specific technical scheme of the invention is as follows:
a layered copper hydroxychloride powder material is a mixed powder composed of copper hydroxychloride (Cu (OH) Cl) crystals having a layered monoclinic structure and a layered orthorhombic structure, wherein the mass ratio of the orthorhombic structured and monoclinic structured copper hydroxychloride is 3: 7.
The copper hydroxychloride with the layered orthogonal structure is obtained under the high-pressure condition by taking the copper hydroxychloride with the layered monoclinic structure as an initial raw material, and stably exists under the conventional condition after the pressure is completely released.
A preparation method of a layered copper hydroxychloride powder material comprises the steps of taking pure copper hydroxychloride (Cu (OH) Cl) crystal powder with a layered monoclinic structure as an initial raw material, pressurizing the initial raw material to 18.7-28.4 GPa in a high-pressure Device (DAC), converting 30% -70% of the copper hydroxychloride with the layered monoclinic structure into the copper hydroxychloride with a layered orthorhombic structure under the action of pressure, and obtaining two-phase coexisting powder of the copper hydroxychloride (Cu (OH) Cl) under high pressure; and releasing the pressure completely, and releasing the pressure to normal pressure to obtain the powder material in which two kinds of copper hydroxychlorides (Cu (OH) Cl) with different structures coexist in a mixed mode, wherein the mass ratio of the orthogonal structure to the monoclinic structure is 3: 7.
The experimental preparation was carried out at room temperature.
The pure copper hydroxychloride (Cu (OH) Cl) crystal with the layered monoclinic structure can be synthesized by a solid phase method in the prior art, such as the method disclosed in CN 110316753A, the particle size of the synthesized copper hydroxychloride (Cu (OH) Cl) crystal with the layered monoclinic structure is 0.7-1.5 mu m, the space group is P21/a, and the monoclinic crystal is obtained.
The method of the invention obtains the stable copper hydroxychloride (Cu (OH) Cl) crystal material with a layered orthogonal structure at normal pressure by a high-pressure synthesis method for the first time.
The invention has the beneficial effects that: according to the product obtained by the preparation method, the crystal structure of the sample is characterized by using synchrotron radiation XRD, and the product is found to have a stable layered orthogonal structure in a part of copper hydroxychloride (Cu (OH) Cl) crystals under high pressure, and the orthogonal structure is still maintained in the part of the sample after pressure relief, so that the product has the advantages of simple process, room-temperature synthesis, short synthesis time, high repeatability and the like.
Drawings
FIG. 1 is a XRD data pattern of pure copper hydroxychloride (Cu (OH) Cl) crystal powder having a layered monoclinic structure as an initial raw material in example 1.
FIG. 2 is an SEM photograph of pure copper hydroxychloride (Cu (OH) Cl) crystal powder having a lamellar monoclinic structure as a starting material in example 1.
FIG. 3 is an XRD data pattern of a powder material in which a copper hydroxychloride (Cu (OH) Cl) having a lamellar monoclinic structure and a lamellar orthorhombic structure coexist in a mixed state at a high pressure of 18.7GPa in example 1.
FIG. 4 is an XRD data pattern of a powder material in which a copper hydroxychloride (Cu (OH) Cl) having a lamellar monoclinic structure and a lamellar orthorhombic structure coexist in a mixed state at a high pressure of 28.4GPa in example 1.
Figure 5 is a synchrotron radiation XRD data pattern of the sample of example 1 as a function of pressure.
Figure 6 is a synchrotron radiation XRD data pattern of the sample after pressure relief in example 1.
Detailed Description
Example 1 synthesis of layered orthorhombic structured crystalline material of copper hydroxychloride (cu (oh) Cl).
The synthesis of the mixed powder of copper hydroxychloride (Cu (OH) Cl) containing a layered orthogonal structure is carried out in a symmetrical diamond anvil cell, the symmetrical diamond anvil cell is used for pressurizing, the size of the diamond anvil cell surface is 0.3mm, and a sealing gasket is made of a T301 stainless steel sheet. A small hole with the diameter of 0.15mm is drilled on the prepressed gasket, a small piece of ruby is placed in the small hole, and a medium is transmitted by methyl-ethyl alcohol (the volume ratio of methyl alcohol to ethyl alcohol is 4: 1). The pressure is calibrated by adopting the technology of standard ruby fluorescence pressing. Pure copper hydroxychloride (cu (oh) Cl) crystals with a lamellar monoclinic structure synthesized by a solid phase method were put into a diamond anvil press, and the sample was pressurized to 28.4 GPa. At 18.7GPa, part (about 30%) of the crystals of copper hydroxychloride (Cu (OH) Cl) with a lamellar monoclinic structure is transformed into copper hydroxychloride with a lamellar orthorhombic structure, i.e. a two-phase coexisting powder of copper hydroxychloride (Cu (OH) Cl) is obtained at high pressure; the pressure is completely released and is released to normal pressure, and the powder material with two different structures of copper hydroxychloride (Cu (OH) Cl) mixed and coexisting is still obtained.
FIG. 1 shows XRD data patterns of pure copper hydroxychloride (Cu (OH) Cl) crystal powder having a lamellar monoclinic structure as a starting material.
FIG. 2 shows SEM pictures of starting pure copper hydroxychloride (Cu (OH) Cl) crystal powders with lamellar monoclinic structure.
FIG. 3 shows XRD data of powder materials with mixed coexistence of copper hydroxychloride (Cu (OH) Cl) having a lamellar monoclinic structure and a lamellar orthorhombic structure at a high pressure of 18.7 GPa.
FIG. 4 shows XRD data of a powder material in which a lamellar monoclinic structure and copper hydroxychloride (Cu (OH) Cl) having a lamellar orthorhombic structure coexist in a mixed state at a high pressure of 28.4 GPa.
FIG. 5 shows a synchrotron radiation XRD data plot of the sample as a function of pressure, at 18.7GPa, a portion of the copper hydroxychloride (Cu (OH) Cl) powder with a lamellar monoclinic structure has been converted into copper hydroxychloride (Cu (OH) Cl) with a lamellar orthorhombic structure.
FIG. 6 shows a synchrotron radiation XRD data pattern of a sample after pressure relief, which shows that the prepared sample is a powder material with a lamellar monoclinic structure and a mixed coexistence of copper hydroxychloride (Cu (OH) Cl) with a lamellar orthorhombic structure.
Claims (2)
1. A preparation method of a layered copper hydroxychloride powder material comprises the steps of taking pure copper hydroxychloride crystal powder with a layered monoclinic structure as an initial raw material, pressurizing the initial raw material to 18.7-28.4 GPa in a high-pressure device, and converting 30-70% of the copper hydroxychloride with the layered monoclinic structure into copper hydroxychloride with a layered orthorhombic structure under the action of pressure, namely obtaining two-phase coexisting powder of the copper hydroxychloride under high pressure; and (3) completely releasing the pressure, and releasing the pressure to normal pressure to obtain the powder material in which two kinds of copper hydroxychlorides with different structures coexist in a mixed manner, wherein the mass ratio of the orthogonal structure to the monoclinic structure copper hydroxychlorides is 3: 7.
2. The method of claim 1, wherein the high pressure device is a diamond anvil cell.
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| US5132259A (en) * | 1986-06-06 | 1992-07-21 | The Dow Chemical Company | Method for reactivating catalysts used in catalytic vapor phase process for producing dihydrocarbyl carbonates |
| CN105129749A (en) * | 2015-08-04 | 2015-12-09 | 吉林大学 | High pressure preparation method of indium nitride nano crystal powdery material |
| CN109020805A (en) * | 2018-08-03 | 2018-12-18 | 北京师范大学 | Fluorescence discoloration eutectic material and preparation method thereof under a kind of ultra-high pressure condition |
| CN109970093A (en) * | 2019-05-15 | 2019-07-05 | 吉林大学 | A kind of hydroxy chloride copper crystal and preparation method thereof |
| CN110316753A (en) * | 2019-07-15 | 2019-10-11 | 吉林大学 | A kind of hydroxy chloride copper product and its synthetic method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5132259A (en) * | 1986-06-06 | 1992-07-21 | The Dow Chemical Company | Method for reactivating catalysts used in catalytic vapor phase process for producing dihydrocarbyl carbonates |
| CN105129749A (en) * | 2015-08-04 | 2015-12-09 | 吉林大学 | High pressure preparation method of indium nitride nano crystal powdery material |
| CN109020805A (en) * | 2018-08-03 | 2018-12-18 | 北京师范大学 | Fluorescence discoloration eutectic material and preparation method thereof under a kind of ultra-high pressure condition |
| CN109970093A (en) * | 2019-05-15 | 2019-07-05 | 吉林大学 | A kind of hydroxy chloride copper crystal and preparation method thereof |
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| Title |
|---|
| Compression Behavior of Copper Hydroxyfluoride CuOHF as a Case Study of the High-Pressure Responses of the Hydrogen-Bonded Two-Dimensional Layered Materials;Tian H et al.;《JOURNAL OF PHYSICAL CHEMISTRY C》;20190924;第123卷;第25492-25500页 * |
| Pressure-Induced Phase Transformation of Botallackite α-Cu2(OH)3Cl with a Two-Dimensional Layered Structure Synthesized via a Hydrothermal Strategy;Zhao Y et al.;《JOURNAL OF PHYSICAL CHEMISTRY C》;20200409;第124卷;第9581-9590页 * |
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