CN105731518B

CN105731518B - Normal-temperature crystallization preparation method of octahedron cuprous oxide crystal

Info

Publication number: CN105731518B
Application number: CN201610032738.5A
Authority: CN
Inventors: 孟维
Original assignee: Hunan City University
Current assignee: Hunan City University
Priority date: 2016-01-19
Filing date: 2016-01-19
Publication date: 2017-05-10
Anticipated expiration: 2036-01-19
Also published as: CN105731518A

Abstract

The invention provides a normal-temperature crystallization preparation method of octahedron cuprous oxide crystal. The normal-temperature crystallization preparation method comprises the following steps: by taking copper acetate as a copper source and tartaric acid as a reducing agent, adding the two components into a proper amount of 0.1-3.0M acetic acid/sodium acetate buffer solution with the pH value of 3.0-6.5, stirring, simultaneously adding 1-20ml of a 0.1-3M/L potassium carbonate solution, stirring for 3-9 hours at the room temperature, filtering, and leaving to stand and evaporate for 1-30 days at the room temperature by using a normal-temperature crystallization preparation technique, thereby obtaining the octahedron cuprous oxide crystal. The preparation method of the cuprous oxide crystal of an octahedron structure, which is provided by the invention, is simple and feasible and has energy-saving and environment-friendly effects, raw materials are easy to obtain and low in price, the crystal is regular in crystal morphology, uniform to disperse and high in purity, and the prepared cuprous oxide crystal has wide application prospects in fields such as semiconductor materials, gas sensitive materials and photocatalysis.

Description

A kind of octahedra cuprous oxide crystal normal temperature crystallization preparation method

Technical field

The invention belongs to inorganic functional crystalline material technical field, and in particular to a kind of octahedra cuprous oxide crystal normal temperature Crystallization preparation method.

Background technology

Cuprous oxide is a kind of p-type semiconductor material of forbidden band broadband about 2.17eV, with special optics and magnetic property, Have widely at aspects such as magnetic memory apparatus, superconductor, solar cell, CO catalyst, photocatalysis, the negative materials of lithium battery Application prospect, becomes the research focus of domestic and international researcher.Cu₂O physics and chemical property are to a certain extent by it Pattern and structures shape, the product pattern obtained by different synthetic methods is different with structure, therefore, how to synthesize controllable appearance With the micro-nano Cu of structure₂O has become research emphasis.

Chinese patent（CN102849778A）Disclose a kind of octahedra cuprous oxide crystal and preparation method thereof, the patent Technology adds certain urea with copper nitrate as copper source, with water and glycerine make mixed solvent in autoclave 90-220 DEG C it is anti- Answer at least 4 hours, obtain octahedra cuprous oxide crystal crystal.Although the present invention is easy to get with raw material, process is simple, yield Height, the features such as pollution-free, but preparation process is needed in autoclave, and safety issue has to be solved, 90-220 DEG C of reaction At least 4 hours, increased energy consumption.

Chinese patent（CN102618925A）A kind of preparation method of cuprous nano octahedron material is disclosed, this is special With copper lactate as copper source, the preparation, base soln pH through base soln is adjusted sharp technology, conductive substrate is processed and Cu₂O nanometers Octahedron prepares four processing steps and prepares average-size for 150nm regular octahedron cuprous oxide, although this electrodeless heavy The advantages of area method outside need not apply power supply, energy consumption is low, product purity is high, solves Conventional electrochemical deposition and prepares cupric oxide Many problems of technique, but the method complex technical process, limit its practical application.

Chinese patent（CN103172104A）A kind of preparation method of the preparation method of nano cuprous oxide is disclosed, this is special Sharp technology adds certain NaOH with copper nitrate as copper source, adds certain hydrazine hydrate and makees to react certain under reducing agent room temperature Time obtains octahedra Cu₂O nano particles, although this method is simple, low power consumption and other advantages, but hydrazine hydrate has very strong poison Property, the problems demand of environmental pollution is solved.

The content of the invention

An object of the present invention is to overcome the deficiencies in the prior art in existing cuprous oxide preparation process, there is provided one Plant the preparation method of cuprous oxide crystal.

Weigh the cushioning liquid of the acetic acid/sodium acetate of a certain amount of copper acetate and tartaric acid addition finite concentration and pH value In, stirring while add certain density solution of potassium carbonate some, under room temperature after stirring reaction certain hour, Jing is filtered, Evaporation certain hour is stood under room temperature, you can obtain octahedra cuprous oxide crystal.

Concrete preparation and characterizing method are as follows：1）The buffer concentration of acetic acid/sodium acetate be 0.1-3.0 mol/Ls, pH It is worth for 3-6.5, consumption is 2-50 milliliters.

2）Copper acetate and tartaric mol ratio are 0.3-3.

3）One side stirring reaction is while add wet chemical concentration to be 0.1-3 mol/Ls, consumption is 1-20 milliliters.

4）It is 3-9 hours in the room temperature reaction time, Jing is filtered, and using normal temperature technology of preparing is crystallized, evaporation is stood under room temperature 1-30 days, product Jing centrifugations, deionized water and absolute ethanol washing obtain final product bolarious octahedral structure oxidation sub- after being dried Copper crystal.

5）Cuprous oxide and its purity are confirmed by XRD tests, with ESEM the size and pattern of cuprous oxide are characterized.

6）The preparation method of the octahedra cuprous oxide crystal of present invention report is simple, and energy-conserving and environment-protective, raw material is easy to get And cheap, the cuprous oxide crystal regular appearance of octahedral structure, it is uniformly dispersed, purity is high；The cuprous oxide of preparation is brilliant Body is with a wide range of applications in semi-conducting material, gas sensitive, photocatalysis field.

Description of the drawings

Fig. 1 is the XRD spectrum of the octahedra cuprous oxide crystal of the gained of embodiment 1.

Fig. 2 is the scanning electron microscopic picture of the octahedra cuprous oxide crystal of the gained of embodiment 1.

Specific embodiment

Embodiment 1：Weigh 0.198g copper acetates and 0.150gL- tartaric acid adds the acetic acid/acetic acid of 0.5M/L, pH=4.5 In the cushioning liquid of sodium, stir while add the solution of potassium carbonate 3ml of 0.8M/L, stirring reaction 4h under room temperature, Jing is filtered, Evaporation 10 days, product Jing centrifugations, deionized water and absolute ethanol washing are stood under room temperature, is placed in vacuum drying chamber in 60 DEG C 12h is dried, obtains final product bolarious octahedral structure cuprous oxide crystal.XRD is carried out to made octahedra cuprous oxide crystal Analysis, collection of illustrative plates is as shown in figure 1, there is figure to understand to occur in that phase in 2 θ=29.76 °, 36.60,42.52,61.56,73.64 and 77.56 The diffraction maximum answered, this and Cu₂The characteristic peak of O crystal standard diagrams is completely the same, shows the pure of the octahedra cuprous oxide crystal Degree is very high.Take portion of product and do sem test, product is the crystal of octahedral shape, and rib length is about 10 μm, such as Fig. 2 institutes Show.

Embodiment 2：Weigh 0.398g copper acetates and 0.251gD- tartaric acid adds the acetic acid/acetic acid of 0.3M/L, pH=5.5 In the cushioning liquid of sodium, stir while add the solution of potassium carbonate 5ml of 1.5M/L, stirring reaction 4h under room temperature, Jing is filtered, Evaporation 15 days, product Jing centrifugations, deionized water and absolute ethanol washing are stood under room temperature, is placed in vacuum drying chamber in 60 DEG C 12h is dried, obtains final product bolarious octahedral structure cuprous oxide crystal.Confirm target product and its purity by XRD analysis, The size and pattern of cuprous oxide crystal are characterized with ESEM.

Claims

1. a kind of octahedra cuprous oxide crystal normal temperature crystallization preparation method, it is characterised in that crystallize technology of preparing using normal temperature, During copper acetate, L-TARTARIC ACID or D- tartaric acid to be added the cushioning liquid of acetic acid/sodium acetate of finite concentration and pH value, then add Enter certain density solution of potassium carbonate some, under room temperature after stirring reaction certain hour, Jing is filtered, evaporation is stood under room temperature, i.e., Octahedra cuprous oxide crystal is obtained.

2. a kind of octahedra cuprous oxide crystal normal temperature crystallization preparation method as claimed in claim 1, it is characterised in that acetic acid/ The buffer concentration of sodium acetate is 0.1-3.0 mol/Ls, and pH value is 3-6.5, and consumption is 2-50 milliliters.

3. a kind of octahedra cuprous oxide crystal normal temperature crystallization preparation method as claimed in claim 1, it is characterised in that acetic acid Copper and tartaric mol ratio are 0.3-3:1.

4. a kind of octahedra cuprous oxide crystal normal temperature crystallization preparation method as claimed in claim 1, it is characterised in that carbonic acid The concentration of aqueous solution of potassium is 0.1-3 mol/Ls, and consumption is 1-20 milliliters, and one side stirring reaction is while add solution of potassium carbonate； In room temperature reaction 3-9 hours.

5. a kind of octahedra cuprous oxide crystal normal temperature crystallization preparation method as claimed in claim 1, it is characterised in that room temperature Lower standing evaporation time is 1-30 days；Product Jing centrifugations, deionized water and absolute ethanol washing time, are placed in vacuum drying chamber In be dried 12h in 60 DEG C, obtain final product bolarious octahedral structure cuprous oxide crystal.