阅读说明：本技术 一种氧化钆纳米粉体的微波煅烧制备方法 (Microwave calcination preparation method of gadolinium oxide nano powder ) 是由 黄志民 黄慨 顾传君 冼学权 黄绍权 黄华林 于 2020-04-24 设计创作，主要内容包括：本发明公开了一种氧化钆纳米粉体的微波煅烧制备方法,包括如下步骤,(1)原料准备：在氯化钆溶液中加入凝胶作为表面活性剂,混合均匀,得到经过表面处理的氯化钆溶液；(2)超声沉淀：在超声搅拌条件下将草酸溶液缓慢滴加至经过表面处理的氯化钆溶液中,经过过滤洗涤得到白色沉淀；(3)微波加热煅烧：将白色沉淀置于微波反应器中进行微波加热煅烧,微波的频率为915±50MHz或2450±50MHz,微波功率为1-10kw,时间为1-6h,最终得到白色粉末状氧化钆。本发明采用凝胶作为表面活性剂,通过超声震荡分散,在以微波加热煅烧的方法制备得到纳米级的氧化钆粉体。(The invention discloses a microwave calcination preparation method of gadolinium oxide nano powder, which comprises the following steps of (1) preparing raw materials: adding gel serving as a surfactant into the gadolinium chloride solution, and uniformly mixing to obtain a gadolinium chloride solution subjected to surface treatment; (2) ultrasonic precipitation: slowly dripping an oxalic acid solution into the gadolinium chloride solution subjected to surface treatment under the ultrasonic stirring condition, and filtering and washing to obtain a white precipitate; (3) microwave heating and calcining: and placing the white precipitate in a microwave reactor for microwave heating calcination, wherein the frequency of the microwave is 915 +/-50 MHz or 2450 +/-50 MHz, the microwave power is 1-10kw, and the time is 1-6h, and finally obtaining white powdery gadolinium oxide. The invention adopts gel as a surfactant, and prepares nano-scale gadolinium oxide powder by a microwave heating and calcining method through ultrasonic oscillation dispersion.)

1. A microwave calcination preparation method of gadolinium oxide nano powder is characterized by comprising the following steps: comprises the following steps of (a) carrying out,

(1) preparing raw materials: adding gel serving as a surfactant into the gadolinium chloride solution, and uniformly mixing to obtain a gadolinium chloride solution subjected to surface treatment;

(2) ultrasonic precipitation: slowly dripping an oxalic acid solution into the gadolinium chloride solution subjected to surface treatment under the ultrasonic stirring condition, and filtering and washing to obtain a white precipitate;

(3) microwave heating and calcining: and placing the white precipitate in a microwave reactor for microwave heating calcination, wherein the frequency of the microwave is 915 +/-50 MHz or 2450 +/-50 MHz, the microwave power is 1-10kw, and the time is 1-6h, and finally obtaining white powdery gadolinium oxide.

2. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 1, characterized in that: the gel in the step (1) is natural aloe or a mixture of natural aloe and citric acid.

3. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 2, characterized in that: the ratio of the natural aloe to the citric acid is 1: 0.1-1.

4. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 1, characterized in that: the addition amount of the gel is 10-15% of the concentration ratio of the gadolinium chloride solution.

5. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 1, characterized in that: the concentration of the gadolinium chloride solution in the step (1) is 0.1-1.5 mol/L.

6. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 1, characterized in that: the ultrasonic frequency of the step (2) is 30-45kHz, and the time is 0.5-2 h.

7. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 1, characterized in that: the temperature for microwave heating and calcining in the step (3) is 800-1100 ℃.

8. The microwave calcination preparation method of gadolinium oxide nano-powder according to claim 1, characterized in that: the microwave output mode comprises two modes of continuous waves and pulse waves or two combinations of the continuous waves and the pulse waves.

Technical Field

The invention belongs to the field of rare earth, and particularly relates to a microwave calcination preparation method of gadolinium oxide nano powder.

Background

Gadolinium oxide is widely used in the fields of catalysis, ceramics, glass industry, solid oxide fuel cells, luminescent materials, polishing materials, nuclear materials and the like. With the scientific and technical law stick, manufacturers have higher requirements on the physical properties of gadolinium oxide. At present, in the methods for preparing gadolinium oxide, a chemical precipitation method is mostly adopted, ammonium bicarbonate and oxalic acid are adopted as precipitating agents, and then gadolinium oxide is prepared by high-temperature firing. The gadolinium oxide prepared by the method is generally large in particle size and mostly micron-sized particles, and the prepared particles are uneven in particle size, poor in particle size and difficult to control in shape.

Disclosure of Invention

The invention aims to provide a microwave calcination preparation method of gadolinium oxide nano powder, which adopts gel as a surfactant and prepares the nano-scale gadolinium oxide powder by a microwave heating calcination method through ultrasonic oscillation dispersion.

The purpose of the invention is realized by the following technical scheme:

a microwave calcination preparation method of gadolinium oxide nano powder comprises the following steps,

(1) preparing raw materials: adding gel serving as a surfactant into the gadolinium chloride solution, and uniformly mixing to obtain a gadolinium chloride solution subjected to surface treatment;

(2) ultrasonic precipitation: slowly dripping an oxalic acid solution into the gadolinium chloride solution subjected to surface treatment under the ultrasonic stirring condition, and filtering and washing to obtain a white precipitate;

(3) microwave heating and calcining: and placing the white precipitate in a microwave reactor for microwave heating calcination, wherein the frequency of the microwave is 915 +/-50 MHz or 2450 +/-50 MHz, the microwave power is 1-10kw, and the time is 1-6h, and finally obtaining white powdery gadolinium oxide.

Preferably, in the step (1), the gel is natural aloe or a mixture of natural aloe and citric acid.

Preferably, the ratio of the natural aloe to the citric acid is 1: 0.1-1.

Preferably, the gel is added in an amount of 10-15% of the gadolinium chloride solution.

Preferably, the concentration of the gadolinium chloride solution in the step (1) is 0.1-1.5 mol/L.

Preferably, the ultrasonic frequency of the step (2) is 30-45kHz, and the time is 0.5-2 h.

Preferably, the temperature for microwave heating and calcining in the step (3) is 800-1100 ℃.

Preferably, the microwave output means includes two or a combination of continuous waves and pulsed waves.

The invention has the following beneficial effects:

1. the invention adopts the gel as the surfactant, and the gel and the generated precipitate form surface coverage by controlling the addition amount of the gel, thereby inhibiting the growth of the precipitate particles and being beneficial to the subsequent preparation of the nano powder particles.

2. The invention adopts an ultrasonic precipitation method, and the formed precipitation particles are uniformly dispersed in the solution through ultrasonic oscillation, thereby preventing the agglomeration after the precipitation is generated and ensuring that the prepared precipitation particles are more uniform.

3. The invention can obtain the precipitated particles with different particle sizes by controlling the addition amount of the gel and the frequency and time of the ultrasonic treatment.

4. The method adopts a microwave heating and calcining method to calcine the prepared precipitate, controls the temperature and time of heating and calcining by controlling the microwave frequency, is easy to control, simultaneously adopts microwave heating, enables the interior of the material to generate resonance to generate heat through specific microwave frequency oscillation, simultaneously heats the interior and the exterior, has high heat transfer efficiency, avoids the agglomeration phenomenon of particles due to uneven heating of the interior and the exterior, and prepares the nano powder with uniform granularity and good dispersibility.

Detailed Description

In order to make those skilled in the art better understand the technical solutions in the present application, the following will clearly and completely describe the technical solutions in the present application with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and all other embodiments obtained by a person of ordinary skill in the art without making creative efforts based on the embodiments in the present application shall fall within the protection scope of the present application.