Preparation method of cerium dioxide fluoride polishing powder under microwave condition
A technology of fluorinated cerium dioxide and polishing powder, which is applied in the preparation/treatment of rare earth metal compounds, chemical instruments and methods, rare earth metal oxyhalides, etc., and can solve the problems of increasing equipment, consuming time, and reducing product purity. , to achieve the effects of weakening agglomeration, reducing surface scratches, and simplifying the process flow
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Embodiment 1
[0037] Example 1 (no microwave control group)
[0038] A preparation method of fluorinated ceria polishing powder under a water bath condition, comprising the following steps:
[0039] (1) Take Ce (NO 3 ) 3 ·6H 2 O, NH 4 HCO 3 and NH 4 F was dissolved in deionized water, and 500 mL of 0.0582 mol / L cerium nitrate aqueous solution, 125 mL of 1.047 mol / L ammonium bicarbonate aqueous solution and 125 mL of 0.126 mol / L ammonium fluoride aqueous solution were prepared; The influence of polishing powder preparation does not study the influence of the above-mentioned component content on the polishing powder. The above-mentioned component dosage is a preferred solution in the research process of the present invention, and its selection range satisfies the following conditions:
[0040] A.NH 4The amount of F is 5% to 7% of the quality of the final product as the fluorine element;
[0041] B.NH 4 HCO 3 and Ce(NO 3 ) 3 ·6H 2 The molar ratio of O is more than 4.5:1;
[0042]...
Embodiment 2
[0054] A preparation method of fluorinated ceria polishing powder under microwave conditions, comprising the following steps:
[0055] (1) Take Ce (NO 3 ) 3 ·6H 2 O, NH 4 HCO 3 and NH 4 F was dissolved in deionized water, and 500 mL of 0.0582 mol / L cerium nitrate aqueous solution, 125 mL of 1.047 mol / L ammonium bicarbonate aqueous solution and 125 mL of 0.126 mol / L ammonium fluoride aqueous solution were prepared;
[0056] (2) get the cerium nitrate solution configured in the above (1) and put it into the microwave reactor for microwave heating, the heating temperature is to 65 ° C, and get the ammonium fluoride solution in the above (1) and add it, and stir magnetically evenly;
[0057] (3) get the ammonium bicarbonate solution configured in the above-mentioned (1), add the cerium nitrate and ammonium fluoride mixed solution obtained in the above-mentioned (2), stir magnetically and react 75min at a constant temperature of 65 ℃ in a microwave mode;
[0058] In steps (2)...
Embodiment 1、2
[0065] Embodiment 1,2 comparative analysis is as follows:
[0066] (1) as figure 1 Shown is the SEM image of the precursor cerium carbonate under the water bath condition prepared in Example 1, such as figure 2 Shown is the SEM image of the precursor cerium carbonate under microwave conditions prepared in Example 2; the comparison of the two SEM images shows that the cerium carbonate particles prepared under microwave conditions are more rounded and have better particle dispersibility.
[0067] (2) as image 3 Shown is the SEM image of fluorinated ceria under the water bath condition prepared in Example 1, such as Figure 4 Shown is the SEM image of fluorinated ceria under microwave conditions prepared in Example 2; by comparison, it can be seen that the ceria particles prepared under water bath conditions have large-scale agglomeration, while the ceria particles prepared under microwave conditions The dispersibility of cerium dioxide particles is good, indicating that mic...
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