High precision rare earth polishing powder and preparation thereof
A rare earth polishing powder, high-precision technology, applied in chemical instruments and methods, polishing compositions containing abrasives, other chemical processes, etc. Fluctuation and other problems, to achieve the effect of easy control of polishing accuracy stability, easy control of wear resistance, and small fluctuation of product quality
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Embodiment 1
[0033] (1) Preparation of seed crystals: Heat 1 L of 20 g / L oxalic acid solution to a temperature of 70° C., add ammonia water with a weight concentration of 12.5% until the pH is 5.5, add 50 g / L lanthanum cerium chloride solution, and heat at 70° C. React for 0.5h and age for 2h to obtain lanthanum cerium oxalate crystal seeds with a particle size distribution between 0.50 and 0.70 μm, see figure 1 ;
[0034] (2) Precipitation: Add 2.5 g Lanthanum cerium oxalate seed crystals, at 50°C, add an aqueous solution of sodium bicarbonate with a mass fraction of 25% while stirring until the pH value is 6, to obtain precipitated lanthanum cerium carbonate;
[0035] (3) Fluorination: add 9.9 g of hydrofluoric acid aqueous solution with a weight concentration of 15% to lanthanum cerium carbonate, react at room temperature for 0.5 h, and perform fluorination;
[0036] (4) Roasting: The partially fluorinated lanthanum cerium carbonate is filtered and washed with a centrifuge, dried in...
Embodiment 2
[0038] (1) Preparation of seed crystals: 1L concentration of 50g / L oxalic acid solution is heated to a temperature of 70°C, and the mass concentration of 12.5% ammonia is added until the pH is 4.5, slowly adding 100g / L lanthanum cerium chloride solution, React at 70°C for 1.5 hours, crystallize for 4 hours, and the particle size distribution of the obtained lanthanum cerium praseodymium oxalate crystal seeds is between 0.60 and 0.90 μm;
[0039](2) Precipitation: Add 22.5g of lanthanum cerium praseodymium oxalate seed crystals to 1L of lanthanum cerium chloride aqueous solution with a concentration of 150g / L, and add 25% sodium bicarbonate aqueous solution while stirring until the pH Value is 7, obtains the lanthanum cerium carbonate of precipitation;
[0040] (3) Fluorination: 28.8 g of hydrofluoric acid aqueous solution with a weight concentration of 15% was added to lanthanum cerium carbonate, and reacted for 1 hour at room temperature to carry out fluorination;
[0041]...
Embodiment 3
[0043] (1) Preparation of seed crystals: Heat 1L of 50g / L oxalic acid solution to a temperature of 70°C, add ammonia water with a mass concentration of 12.5% until the pH is 5, slowly add 100g / L lanthanum cerium nitrate solution at 80°C Reaction for 1.0h, aging for 3h, the particle size distribution of lanthanum cerium oxalate seeds is between 0.80-1.00μm;
[0044] (2) Precipitation: Add 10 g of lanthanum cerium oxalate seed crystals to 1 L of lanthanum cerium nitrate aqueous solution with a concentration of 100 g / liter, and add 25% ammonium bicarbonate aqueous solution while stirring until the pH value is 6.5, obtaining precipitated lanthanum cerium carbonate;
[0045] (3) Fluorination: adding 28.8 g of hydrofluoric acid aqueous solution with a weight concentration of 15% to lanthanum cerium carbonate and reacting for 1 hour at room temperature for fluorination;
[0046] (4) Roasting: filter and wash the partially fluorinated lanthanum cerium carbonate with a centrifuge, d...
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