CN111533157A - Microwave calcination preparation method of gadolinium oxide nano powder - Google Patents
Microwave calcination preparation method of gadolinium oxide nano powder Download PDFInfo
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- CN111533157A CN111533157A CN202010330372.6A CN202010330372A CN111533157A CN 111533157 A CN111533157 A CN 111533157A CN 202010330372 A CN202010330372 A CN 202010330372A CN 111533157 A CN111533157 A CN 111533157A
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Abstract
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.
Description
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.
Example 1
A microwave calcination preparation method of gadolinium oxide nano powder comprises the following steps,
(1) preparing raw materials: adding natural aloe gel into gadolinium chloride solution with the concentration of 0.1mol/L, and uniformly mixing to obtain gadolinium chloride solution subjected to surface treatment; the addition amount of the natural aloe gel is 10 percent of the concentration ratio of the gadolinium chloride solution;
(2) ultrasonic precipitation: under the condition of ultrasonic stirring, slowly dripping an oxalic acid solution into a gadolinium chloride solution subjected to surface treatment, and filtering and washing to obtain a white precipitate; the ultrasonic frequency is 30kHz, and the time is 2 h;
(3) microwave heating and calcining: placing the white precipitate in a microwave reactor, and carrying out microwave heating calcination for 6h at the frequency of 915 +/-50 MHz, the microwave power of 1kw and the temperature of 800 ℃ to finally obtain white powdery gadolinium oxide; the microwave output mode is a continuous wave mode.
Example 2
A microwave calcination preparation method of gadolinium oxide nano powder comprises the following steps,
(1) preparing raw materials: adding gel into gadolinium chloride solution with the concentration of 1.5mol/L, and uniformly mixing to obtain gadolinium chloride solution subjected to surface treatment; the gel is prepared from natural aloe and citric acid according to the proportion of 1: 0.1, wherein the addition amount of the gel is 15% of the concentration ratio of the gadolinium chloride solution;
(2) ultrasonic precipitation: under the condition of ultrasonic stirring, slowly dripping an oxalic acid solution into a gadolinium chloride solution subjected to surface treatment, and filtering and washing to obtain a white precipitate; the ultrasonic frequency is 45kHz, and the time is 0.5 h;
(3) microwave heating and calcining: placing the white precipitate in a microwave reactor, and carrying out microwave heating calcination for 1h at the frequency of 2450 +/-50 MHz, the microwave power of 10kw and the temperature of 1100 ℃ to finally obtain white powdery gadolinium oxide; the microwave output mode is a pulse wave mode.
Example 3
A microwave calcination preparation method of gadolinium oxide nano powder comprises the following steps,
(1) preparing raw materials: adding gel into gadolinium chloride solution with the concentration of 0.5mol/L, and uniformly mixing to obtain gadolinium chloride solution subjected to surface treatment; the gel is prepared from natural aloe and citric acid according to the proportion of 1: 1, the addition amount of the gel is 12% of the concentration ratio of the gadolinium chloride solution;
(2) ultrasonic precipitation: under the condition of ultrasonic stirring, slowly dripping an oxalic acid solution into a gadolinium chloride solution subjected to surface treatment, and filtering and washing to obtain a white precipitate; the ultrasonic frequency is 35kHz, and the time is 1 h;
(3) microwave heating and calcining: placing the white precipitate in a microwave reactor, and carrying out microwave heating calcination for 4 hours at the frequency of 915 +/-50 MHz1, the microwave power of 4kw and the temperature of 1000 ℃ to finally obtain white powdery gadolinium oxide; the microwave output mode is a combination mode of continuous waves and pulse waves.
Example 4
A microwave calcination preparation method of gadolinium oxide nano powder comprises the following steps,
(1) preparing raw materials: adding gel into gadolinium chloride solution with the concentration of 1.0mol/L, and uniformly mixing to obtain gadolinium chloride solution subjected to surface treatment; the gel is prepared from natural aloe and citric acid according to the proportion of 1: 0.6, wherein the addition amount of the gel is 14% of the gadolinium chloride solution concentration ratio;
(2) ultrasonic precipitation: under the condition of ultrasonic stirring, slowly dripping an oxalic acid solution into a gadolinium chloride solution subjected to surface treatment, and filtering and washing to obtain a white precipitate; the ultrasonic frequency is 40kHz, and the time is 1.5 h;
(3) microwave heating and calcining: placing the white precipitate in a microwave reactor, and carrying out microwave heating calcination for 2h at the frequency of 2450 +/-50 MHz, the microwave power of 8kw and the temperature of 900 ℃ to finally obtain white powdery gadolinium oxide; the microwave output mode is a combination mode of continuous waves and pulse waves.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art. The invention is therefore not to be limited to the specific details described herein, without departing from the general concept as defined by the appended claims and their equivalents.
Claims (8)
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.
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