Method for preparing single crystal or amorphous substance by using aqueous solution

A technology of amorphous matter and aqueous solution, which is applied in the direction of single crystal growth, chemical instruments and methods, and solutions from liquid solvents at room temperature, etc., which can solve the problems of polycrystal formation, difficulty in single crystal growth, and poor controllability of crystal nucleation and growth. and other issues, to achieve a wide range of control and universal effects

Pending Publication Date: 2019-12-24
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 methods generally have problems such as poor controllability of crystal nucleation and growth, difficulty in growing single crystals, and easy generation o

Method used

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  • Method for preparing single crystal or amorphous substance by using aqueous solution
  • Method for preparing single crystal or amorphous substance by using aqueous solution
  • Method for preparing single crystal or amorphous substance by using aqueous solution

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Experimental program
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Effect test

Embodiment approach

[0153] According to an embodiment of the present invention, the method for cultivating a single crystal further includes the following steps:

[0154] (b1) transferring the single crystal of the quasi-crystalline substance prepared above to the mother liquor of the quasi-crystalline substance for cultivation;

[0155] (b2) Collecting the single crystal in step (b1).

[0156] 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.

[0157] According to an embodiment of the present invention, the mother liquor is a mother liquor system known by those skilled in the art that is compatible with the single crystal phase to be cultivated.

[0158] The present invention will be f...

Embodiment 1

[0161] Use ultrapure water to prepare a copper sulfate solution with a concentration of 500μM, take 100ml of the solution into a beaker with a measuring cylinder, place it in a -24°C refrigerator and slowly cool it down to complete freezing, and finally place it in a -15°C refrigerator for aging After 30 minutes, the sample was freeze-dried, and the solid ice was completely sublimated to obtain a single crystal. Finally, select a single crystal with better quality from the beaker and move it to a saturated copper sulfate aqueous 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 larger copper sulfate crystals can grow. , see the test results in the attached figure 1 . Depend on figure 1 It can be seen that the obtained crystal is a single crystal.

Embodiment 2

[0163] Prepare a copper sulfate solution with a concentration of 10mM in ultrapure water, take 30 μL 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 -18°C refrigerator Medium aging for 40min, followed by quenching to remove ice, can obtain single crystal. Finally, select a single crystal with better quality from the silicon wafer and move it to a saturated copper sulfate aqueous 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 a larger volume of copper sulfate can be grown. crystals.

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Abstract

The invention relates to the field of single crystal preparation, in particular to a method for preparing a single crystal or an amorphous substance by using an aqueous solution, which is suitable forpreparing and culturing any water-soluble molecular single crystal or amorphous substance. The method comprises the following steps: (a1) preparing an aqueous solution of a quasi-crystalline substance; (a2) freezing the water solution of the quasi-crystalline substance in the step (a1), and optionally aging the water solution to prepare a mono-crystal or amorphous substance-ice mixed system containing the quasi-crystalline substance; optionally, (a3) separating the monocrystal or amorphous substance-ice mixed system of the quasi-crystalline substance in the step (a2) to obtain the monocrystalor amorphous substance of the quasi-crystalline substance. The method aims at the defects that the molecular nucleation and aggregation speed is difficult to control and the like in the process of culturing the single crystal or amorphous substance by the traditional method; the invention provides the method for inducing nucleation and crystallization of solute molecules by freezing an aqueous solution for the first time, so that the solute molecule single crystal or amorphous substance is rapidly and effectively prepared.

Description

[0001] This application claims the priority of the earlier application of the patent application number 2018112792527 submitted to the State Intellectual Property Office of China on October 30, 2018, and the title of the invention is "A method for preparing and cultivating single crystals using aqueous solution". This application is incorporated by reference in its entirety. technical field [0002] The invention relates to the field of preparation of single crystals or amorphous substances, in particular to a method for preparing single crystals or amorphous substances using an aqueous solution, and the method is applicable to the preparation of any water-soluble molecular single crystal or amorphous substances. [0003] technical background [0004] Single crystal plays a pivotal role in various modern scientific fields, such as organic molecule and protein structure analysis, optoelectronic devices, medicine and aerospace and other fields. At present, the methods of molecu...

Claims

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Application Information

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