Method of purifying environment-friendly type ultra-fine diamond
A purification method and diamond technology, applied in the field of new materials, can solve the problems of serious pollution, lack of impurity analysis results, and high requirements for purification equipment, and achieve the effects of short reaction time, reduced equipment requirements, and less harm.
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Embodiment 1
[0021] The raw diamond powder is pulverized by a jet mill to obtain ultrafine (ultrafine means particle size <5 μm) diamond micropowder.
[0022] Take by weighing 1.01g ultrafine diamond powder (this micropowder burns through 1000 ℃, loss on ignition is 97.10wt%, silicon dioxide content is 2.50wt%), in the reactor of 6ml polytetrafluoroethylene liner, add 1.5ml concentration is 50% g*ml -1 Ammonium fluoride solution (50% g*ml -1 Indicates that 100ml of solvent contains 50g of ammonium fluoride solute), and the concentration of 0.5ml is 45% g*ml -1 Ammonium cerium sulfate solution (45% g*ml -1 Indicates that 100ml of solvent contains 45g of ammonium cerium sulfate solute), ultrasonic treatment for 0.5 hours; the reaction kettle was put into an oven, heated at 160°C for 8 hours, after cooling, the reaction kettle was taken out; after cooling, the supernatant was poured out, and the diamond was rinsed out. Add nitric acid to adjust the pH value of the solution below 3, and ult...
Embodiment 2
[0024] Weigh 1.00g of crushed ultrafine diamond powder (the powder is burned at 1000°C, the loss on ignition is 99.70wt%, and the silicon dioxide content is 0.25wt%); in a 60ml polytetrafluoroethylene-lined reaction kettle , add 15ml concentration of 4% g*ml -1 Sodium fluoride solution, 5ml concentration is 15% g*ml -1 Ammonium persulfate solution, 5ml concentration is 65% g*ml -1 For ceric sulfate solution, ultrasonically treat it for 0.5 hours; put it in an oven and heat it at 200°C for 10 hours; after cooling, open the reaction kettle and pour out the supernatant, rinse out the diamond, add nitric acid to adjust the pH value of the solution below 3, and ultrasonically treat for 60 minutes , centrifuged and washed to pH = 4, added deionized water for ultrasonic dispersion, dried after centrifuged to obtain ultrafine diamond powder. After testing: the loss on ignition at 1000°C is 99.96wt%, and the silicon dioxide content is 0.0023wt%.
Embodiment 3
[0026] A kind of purification method of environment-friendly ultrafine diamond, it comprises the steps:
[0027] 1), the concentration of 12ml is 5% g*ml-1 The mixed salt solution (the solid content of the mixed salt is 0.6g) is mixed with 2.4g ultrafine diamond powder to obtain a solid-liquid mixture. The mixed salt is potassium permanganate, potassium persulfate and potassium fluoride, and the permanganic acid in the mixed salt solution is The solid contents of potassium, potassium persulfate, and potassium fluoride are: 0.05g, 0.05g, and 0.5g respectively (that is, the weight ratio of the first type of salt to the second type of salt is 1:5); the solid-liquid mixture is dispersed by ultrasonic waves Processing, processing time 0.5 hours;
[0028] 2), move the solid-liquid mixture through ultrasonic treatment in the reactor of 60ml polytetrafluoroethylene lining (at this moment, the filling degree of reactor is 20% V / V), reaction temperature is controlled at 120 ℃, and react...
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