Method for preparing single crystal or amorphous substance by utilizing solution freezing

An amorphous and amorphous technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of poor controllability of crystal nucleation and growth, easy generation of polycrystals or twins, etc. Large range of regulation, solve the effect that is not easy to control

Pending Publication Date: 2020-01-31
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned methods generally have problems such as poor controllability of crystal nucleation and growth, prone to polycrystals or twins, and some molecules cannot even be obt

Method used

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  • Method for preparing single crystal or amorphous substance by utilizing solution freezing
  • Method for preparing single crystal or amorphous substance by utilizing solution freezing
  • Method for preparing single crystal or amorphous substance by utilizing solution freezing

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Experimental program
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Embodiment approach

[0209] According to an embodiment of the present invention, the method for cultivating a single crystal further includes the following steps:

[0210] (b1) transferring the single crystal of the quasi-crystalline substance prepared above to the mother liquor of the quasi-crystalline substance for cultivation;

[0211] (b2) Collecting the single crystal in step (b1).

[0212] According to an embodiment of the present invention, the transfer is any method known to those skilled in the art that can remove a single crystal, including but not limited to optical microscope transfer, scanning electron microscope transfer, dual-beam electron microscope transfer , Transmission electron microscope transfer in one or a combination of several.

[0213] According to an embodiment of the present invention, the mother liquor is a mother liquor system known by those skilled in the art and compatible with the single crystal phase to be cultivated, for example, it can be a saturated solution s...

Embodiment 1

[0218] Prepare an anthracene solution with a concentration of 100 μM in dimethyl sulfoxide, take 100 mL of the solution into a beaker with a graduated cylinder, and place it in a -24°C refrigerator to cool down slowly for 15 minutes. In a completely frozen state, place it in a -10°C refrigerator for aging for 20 minutes (with a heating rate of less than 10°C / min), then freeze-dry the sample and completely sublimate the solid organic solvent to obtain an anthracene single crystal. Finally, a single crystal with better quality is selected from the beaker (the selection method is a routine choice for those skilled in the art, such as judging by the morphology and structure) and moved to a saturated anthracene organic solvent solution, placed at a temperature of 25 ° C, and a relative humidity For a period of time under a constant temperature and humidity environment of 40%, larger organic anthracene single crystals (such as figure 1 shown).

Embodiment 2

[0220] Prepare an anthracene solution with a concentration of 10mM in dimethyl sulfoxide, take 2mL of the solution with a syringe, spread it on a silicon wafer, place it in a -24°C refrigerator and slowly cool it down to complete freezing, and finally place it in a -15°C refrigerator Medium aging for 30 minutes, followed by rapid cooling to quickly remove the frozen organic solvent to obtain a single crystal. Finally, select a single crystal with better quality from the silicon wafer and move it to a saturated anthracene solution, and place it in a constant temperature and humidity environment with a temperature of 25°C and a relative humidity of 40% for a period of time, and then a larger volume of anthracene single crystal can be grown. .

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Abstract

The invention relates to the technical field of preparation of single crystals or amorphous substances, in particular to a method for preparing a quasi-crystalline substance single crystal or an amorphous substance. According to the method, nucleation and crystallization of the quasi-crystalline substance are induced through solution freezing, crystallization of the dissolved quasi-crystalline substance is achieved in the freezing process of the solution, and single crystals or amorphous substances of the quasi-crystalline substance are rapidly and effectively prepared. Meanwhile, the problemthat single crystals or amorphous substances of molecules are difficult to crystallize in traditional pseudo-crystalline substance single crystal preparation and culture is solved. According to the method, the acquisition of the pseudo-crystalline substance single crystal or amorphous substance under extremely low solution concentration is realized for the first time; and the problems of difficultcontrol of single crystal formation, easy formation of polycrystals and twin crystals and the like caused by too fast aggregation of quasi-crystalline substances under high concentration are also solved. The method is wide in application range and suitable for existing quasi-crystalline substances.

Description

[0001] This application claims the priority of the prior application of the patent application No. 2018112792457 submitted to the State Intellectual Property Office of China on October 30, 2018. The entirety of the application is incorporated by reference into this application. technical field [0002] The invention relates to the technical field of preparation of single crystals or amorphous substances, in particular to a method for inducing crystallization of solute molecules or forming amorphous substances by freezing a solution. Preparation of shapes. Background technique [0003] Single crystals play a pivotal role in various modern scientific fields, such as organic molecules and protein structure analysis, optoelectronic devices, medicine, aerospace and other fields. At present, the methods of molecular crystallization have been widely studied, and the commonly used methods include slow solvent evaporation method, cooling method, liquid phase diffusion method, polyme...

Claims

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Application Information

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IPC IPC(8): C30B7/08C30B29/54
CPCC30B7/08C30B29/54
Inventor 王健君范庆瑞周昕吕健勇
Owner INST OF CHEM CHINESE ACAD OF SCI
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