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Monoclinic crystal system crystal form substance and preparation method thereof

A technology of monoclinic crystal system and crystal form, which is applied in the field of monoclinic crystal system crystal form and its preparation, and can solve the problems of slow temperature rise, high red phosphorus vapor pressure, slow sample speed and the like

Active Publication Date: 2022-05-06
SHANGHAI TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When synthesizing metal phosphorus-rich compounds, there is a large temperature difference between the melting points of red phosphorus and metal elements. Therefore, it is necessary to slowly raise the temperature under the premise of adding a large amount of flux (such as Sn) to prevent the quartz tube from bursting, resulting in normal pressure. The sample preparation speed of the solid phase method is very slow (more than half a month)
Another point, also the most important point, is that the vapor pressure of red phosphorus is very high (4357 kPa at 590 degrees Celsius, about 41 atmospheres). risks of

Method used

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  • Monoclinic crystal system crystal form substance and preparation method thereof
  • Monoclinic crystal system crystal form substance and preparation method thereof
  • Monoclinic crystal system crystal form substance and preparation method thereof

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preparation example Construction

[0033]The second aspect of the present invention provides a method for preparing the monoclinic crystal form described in the first aspect of the present invention, the method comprising the following steps:

[0034] 1) Compressing elemental molybdenum and red phosphorus into tablets and wrapping hexagonal boron nitride to prepare inclusions;

[0035] 2) reacting the inclusions described in step 1) at 900-1100° C. under a pressure of 4-6 GPa to obtain a monoclinic crystal form.

[0036] In the method for synthesizing monoclinic crystals provided by the present invention, the step 1) is to compress elemental molybdenum and red phosphorus into tablets and then wrap hexagonal boron nitride to prepare inclusions. Among them, elemental molybdenum and red phosphorus need to be limited in a suitable ratio range. The molar ratio of elemental molybdenum to red phosphorus is 1:2.5-3.5. In one embodiment, the molar ratio of the elemental molybdenum to red phosphorus is 1:2.5-3; or 1:3-...

Embodiment 1

[0049] 1) Preparation of cylindrical reactants of molybdenum and red phosphorus under normal pressure

[0050] Mix chemically pure elemental molybdenum and red phosphorus in a molar ratio of 1:2.5 in a glove box, and mortar them in an agate mortar for half an hour. The reactant powder was compressed into a cylinder with a diameter of 3.5 mm and a height of 3.2 mm by a powder tablet press (pressure: 5 MPa). Because red phosphorus reacts with noble metal Pt under high temperature and high pressure, different from the sample wrapped with noble metal in the existing high temperature and high pressure experiment, the sample reactant in the present invention is wrapped with high temperature and high pressure resistant and chemically stable hexagonal boron nitride, Reduce the chance of generating impurity.

[0051] 2) Put the above sample and the hexagonal boron nitride protective sheath together into a tantalum heating furnace. Then put the sample into the high-pressure assembly f...

Embodiment 2

[0054] 1) Preparation of cylindrical reactants of molybdenum and red phosphorus under normal pressure

[0055] Chemically pure elemental molybdenum and red phosphorus were mixed uniformly in a glove box at a molar ratio of 1:3, and ground in an agate mortar for half an hour. The molybdenum phosphorus powder was compressed into a cylinder with a diameter of 3.5 mm and a height of 3.2 mm with a powder tablet press. The initial reactant of the cylindrical sample is protected by a hexagonal boron nitride tube and a disc to reduce the probability of generating impurity phases.

[0056] 2) Put the above sample and the hexagonal boron nitride protective sheath together into a tantalum heating furnace. Then put the sample into a high-pressure assembly for high-pressure high-temperature synthesis. The sample synthesis is carried out on a 2,000-ton Kawai-type large-cavity press. First slowly increase the pressure to 6GPa at room temperature, then start the heating program to heat up t...

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Abstract

The invention relates to the technical field of new material preparation, in particular to a monoclinic crystal system crystal form substance and a preparation method thereof. The molecular formula of the monoclinic crystal system crystal form substance is MoP2; the monoclinic crystal system crystal form substance comprises the following unit cell parameters of alpha = 90 degrees, beta = 119.192 + / -0.006 degrees and gamma = 90 degrees, the crystal form space group is C2 / m, and the crystal system belongs to a monoclinic system. According to the present invention, the limitation that the high red phosphorus vapor pressure easily causes the explosion of the quartz tube can be overcome by using the high temperature and high pressure conditions so as to prepare the MoP2 single crystal with the bottom-centered monoclinic structure, the crystal has the good crystallization quality, the single-crystal X-ray diffraction results prove that the single-crystal has the single phase, and the single-crystal X-ray diffraction results show that the single-crystal does not contain the impurities or the koelreuteria paniculata crystal.

Description

technical field [0001] The invention relates to the technical field of preparation of new materials, in particular to a monoclinic crystal form and a preparation method thereof. Background technique [0002] In recent years, due to the rich crystal structure types and novel physical and chemical properties of the metal phosphorus-rich compound TPn (T is a metal, and the value of n is 2, 2.5, 3 and 4, etc.), it has aroused extensive research interests of researchers. TP 2 It is an important system in metal phosphorus-rich compounds. In the periodic table of chemical elements, Cr, Mo and W belong to the same main group, and these three metal elements can chemically react with red phosphorus to form CrP 2 , MoP 2 and WP 2 . At present, the crystal structures of these three compounds reported in the literature are: CrP 2 It has a bottom center monoclinic structure (space group: C2 / m), MoP 2 Orthogonal structure with bottom center (space group: Cmc2 1 ). while WP 2 Ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/10C30B1/12C30B1/02
CPCC30B29/10C30B1/12C30B1/02
Inventor 于振海刘晓磊郭艳峰
Owner SHANGHAI TECH UNIV
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