A kind of preparation method of fluorinated ceria polishing powder under microwave condition
A technology of lower fluoride ceria and polishing powder, which is applied in the preparation/processing of rare earth metal compounds, chemical instruments and methods, rare earth metal oxyhalide, etc., and can solve the problems of reducing product purity, increasing equipment, and taking time. , to achieve the effect of reducing surface scratches, weakening agglomeration, and simplifying the process flow.
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Embodiment 1
[0037] Embodiment 1 (no microwave control group)
[0038] A preparation method of ceria fluoride polishing powder under water bath conditions, comprising the following steps:
[0039] (1) Take Ce(NO 3 ) 3 ·6H 2 O, NH 4 HCO 3 and NH 4 F is dissolved in deionized water, configure 500mL of 0.0582mol / L cerium nitrate aqueous solution, 125mL of 1.047mol / L ammonium bicarbonate aqueous solution and 125mL of 0.126mol / L ammonium fluoride aqueous solution; The impact of polishing powder preparation does not study the impact 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 meets the following conditions:
[0040] A. NH 4The amount of F is that its fluorine element quality accounts for 5%~7% of the final product quality;
[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] C. NH 4 F ...
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 Dissolve F in deionized water, prepare 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;
[0056] (2) Put the cerium nitrate solution configured in the above (1) into a microwave reactor for microwave heating, and heat the temperature to 65° C., and add the ammonium fluoride solution in the above (1) to it, and magnetically stir evenly;
[0057] (3) Take the ammonium bicarbonate solution configured in (1) above, add the mixed solution of cerium nitrate and ammonium fluoride obtained in (2) above, stir magnetically, and react at a constant temperature of 65° C. for 75 minutes in microwave mode;
[0058] The microwave heating temperature in steps (2) and (3) is the ...
Embodiment 1、2
[0065] Embodiment 1,2 comparative analysis is as follows:
[0066] (1) if figure 1 Shown is the SEM figure of precursor cerium carbonate under the water bath condition that embodiment 1 makes, as figure 2 Shown is the SEM picture of the precursor cerium carbonate under microwave conditions prepared in Example 2; the comparison of the two SEM pictures shows that the cerium carbonate particles prepared under microwave conditions are more round and have better particle dispersibility.
[0067] (2) if image 3 Shown is the SEM figure of fluorinated cerium dioxide under the water bath condition that embodiment 1 makes, as Figure 4 Shown is the SEM figure of the fluorinated cerium oxide under the microwave condition that embodiment 2 makes; By comparison, it can be seen that the cerium oxide particles prepared under the water bath condition have a large-scale agglomeration phenomenon, while the cerium oxide particles prepared under the microwave condition The dispersibility of ...
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