Salt-assisted ultrasonic disaggregation of nanodiamond
Methods for disaggregating nanodiamond clusters, for example, by using ultrasound to break apart nanodiamond aggregates in a sodium chloride aqueous slurry. Compositions, such as aqueous nanodiamond dispersions and dry particulate compositions that may be produced using these methods.
1. A method of disaggregating nanodiamond clusters, the method comprising:
(a) combining aggregated nanodiamond clusters with a disaggregating agent in a liquid medium comprising a solvent, with the disaggregating agent being present in a concentration above its solubility limit in the solvent to form a mixture of solvent, disaggregating agent, and nanodiamond clusters; and
(b) sonicating the mixture for a time sufficient to produce nanodiamond particles having a median particle size less than the median particle size of the aggregated nanodiamond clusters,
wherein a mass ratio of disaggregating agent to nanodiamond particles in the liquid medium is from about 10:1 to about 100:1.
2. The method of claim 1 wherein the disaggregating agent comprises a crystalline inorganic salt.
3. The method of claim 2 wherein the disaggregating agent comprises a halide salt.
4. The method of claim 2 wherein the disaggregating agent comprises a chloride salt.
5. The method of claim 4 wherein the disaggregating agent comprises sodium chloride.
6. The method of claim 1 wherein the disaggregating agent comprises a crystalline sugar, organic acid, or organic salt.
7. The method of claim 1 wherein the disaggregating agent comprises a chloride, sulfate, or nitrate of gadolinium, copper, nickel, iron, or cobalt.
8. The method of claim 1 wherein the disaggregating agent comprises sodium chloride.
9. The method of claim 8 wherein the solvent comprises a non-aqueous organic solvent.
10. The method of claim 9 wherein the disaggregating agent is at least partially soluble in the solvent component, and wherein the liquid medium comprises the disaggregating agent in an amount that exceeds its solubility limit in the solvent component.
11. The method of claim 10 wherein the liquid medium comprises the disaggregating agent in an amount of greater than 200% of its solubility limit in the solvent component.
12. The method of claim 1 wherein the mass ratio of the disaggregating agent to the nanodiamond in the liquid medium is at least about 150:1.
13. The method of claim 1 wherein the liquid medium is sonicated for a period of from about 30 minutes to about 120 minutes.
14. The method of claim 1 further comprising a separation step wherein at least a portion of the disaggregating agent is separated from the nanodiamond particles by dissolving at least a portion of the disaggregating agent in an eluting solvent in which the nanodiamond particles are substantially insoluble and in which the disaggregating agent is soluble.
15. The method of claim 14 wherein the eluting solvent comprises water.
16. The method of claim 1 comprising an air oxidation step prior to the disaggregation step, wherein said air oxidation step comprises heating the aggregated nanodiamond clusters in air at a temperature of at least about 350° C. for a period of at least about 5 minutes.
17. The method of claim 1 wherein the method is performed in the absence of ceramic or metallic milling media.
18. The method of claim 1 wherein:
the mixture of solvent, disaggregating agent, and nanodiamond clusters comprises sodium chloride as the disaggregating agent and water as the solvent;
the sodium chloride is present in a concentration greater than 200% of its solubility limit in the water;
the disaggregating agent is present in a mass ratio to the nanodiamond clusters of at least about 150:1;
the nanodiamond clusters are present in a concentration of at least about 30 g/L; and
the sonication is for between about 5 minutes to about 120 minutes.
19. The method of claim 1 comprising an ozone oxidation step prior to the disaggregation step.
20. The method of claim 1 wherein:
the mixture of solvent, disaggregating agent, and nanodiamond clusters comprises sodium chloride as the disaggregating agent and water as the solvent;
the sodium chloride is present in a concentration greater than 200% of its solubility limit in the water;
the disaggregating agent is present in a mass ratio to the nanodiamond clusters of at least about 20:1;
the nanodiamond clusters are present in a concentration of at least about 30 g/L; and
the sonication is for between about 30 minutes to about 120 minutes.
21. The method of claim 1 wherein:
the mixture of solvent, disaggregating agent, and nanodiamond clusters comprises sodium chloride as the disaggregating agent and water as the solvent;
the sodium chloride is present in a concentration greater than 200% of its solubility limit in the water;
the disaggregating agent is present in a mass ratio to the nanodiamond clusters of from about 25:1 to about 75:1;
the nanodiamond clusters are present in a concentration of at least about 30 g/L; and
the sonication is for between about 30 minutes to about 120 minutes.