Granted Patent B2

US 9,802,829 · App. 15/297,997 · Granted Oct 31, 2017

Abstract

Claims (47)

1. A method of making a titanium diboride product having a target average particle size, comprising the following steps:

i) providing a precursor mixture comprising a titanium source, a boron source, a carbon source and an amount of sulfur;

ii) controlling the amount of sulfur in the precursor mixture, wherein the amount of sulfur is based on the target average particle size;

iii) reacting the precursor mixture in a reactor to form an actual titanium diboride product having an actual average particle size;

iv) deagglomerating the actual titanium diboride product to remove a plurality of agglomerations in the titanium diboride product,

wherein, due to the amount of sulfur, the actual average particle size corresponds to the target average particle size;

wherein the average particle size is of the titanium diboride product measured by a particle size distribution of the titanium diboride product,

wherein the particle size distribution of the titanium diboride product is between a D50 value of 1.45 μm and a D50 value of 9.56 μm,

wherein the D50 value of 1.45 μm means that 50% of the particles are smaller than 1.45 μm while the other 50% of the particles are equal to or greater than 1.45 μm,

wherein the D50 value of 9.56 μm means that 50% of the particles are smaller than 9.56 μm while the other 50% of the particles are equal to or greater than 9.56 μm,

wherein the relationship between the D50 value of the particle size distribution of the average particle size of the titanium diboride product and the amount of sulfur follows the following equation:

Avg=6.2+0.2×% S+2.2×ln(0.1+% S),

wherein:

Avg=the D50 value of the particle size distribution of the average particle size of the titanium diboride product, and

% S=weight percent of sulfur, and

wherein the amount of sulfur refers to the weight percent present as the precursor mixture, wherein the amount of sulfur is greater than 0.0 and less than 4.0% by weight.

2. The method of claim 1 , wherein the sulfur-containing compound additives are metal sulfides and metal sulfates.

3. The method of claim 1 , wherein the reacting step comprises carbothermically reacting the precursor mixture.

4. The method of claim 1 , wherein a condition of an at least one processing variable is based on the target average particle size and/or the amount of sulfur.

5. The method of claim 1 , wherein reacting the precursor mixture further comprises controlling at least one processing variable from a group, comprising a soak time, a reaction temperature and an inert gas flow rate.

6. The method of claim 1 , wherein the method further comprises the step of producing the precursor mixture, wherein producing the precursor mixture comprises the following steps:

mixing into a liquid to form a suspension:

a boron source;

a carbon source;

a titanium source; and

drying the suspension to produce the precursor mixture having a plurality of agglomerations.

7. The method of claim 1 , wherein the step of deagglomerating includes milling of the titanium diboride product.

8. The method of claim 1 , further comprising the step of processing the actual titanium diboride product into one of: a cathode; and a structure of an aluminum electrolysis cell.

9. A method comprising:

i) providing a precursor mixture comprising a titanium source, a boron source, a carbon source and an amount of sulfur, wherein the amount of sulfur is no greater than 1% by weight of sulfur present in the precursor mixture;

ii) reacting the precursor mixture in a reactor to form a titanium diboride product having an average particle size of no greater than 7 μm;

wherein the average particle size of the titanium diboride product is controlled by selecting the amount of sulfur present in the precursor mixture,

wherein the average particle size of the titanium diboride product is smaller with a low amount of sulfur and larger with a higher amount of sulfur.

10. The method of claim 9 , wherein the reacting step comprises carbothermically reacting the precursor mixture.

11. The method of claim 9 , wherein the condition of the at least one processing variable is based on the target average particle size and/or the amount of sulfur.

12. The method of claim 9 , wherein the method further comprises the step of producing the precursor mixture, wherein producing the precursor mixture comprises the following steps:

mixing into a liquid to form a suspension:

a boron source;

a carbon source;

a titanium source; and

drying the suspension to produce the precursor mixture having a plurality of agglomerations.

13. The method of claim 9 , wherein the method includes a step of deagglomerating the actual titanium diboride product to remove a plurality of agglomerations in the titanium diboride product.

14. The method of claim 13 , wherein the step of deagglomerating includes milling of the titanium diboride product.

15. The method of claim 9 , further comprising the step of processing the actual titanium diboride product into one of: a cathode; and a structure of an aluminum electrolysis cell.

16. The method of claim 5 , wherein the reaction temperature is at least about 1300° C.; wherein the soak time is at least about 0.5 h; wherein the inert gas flow rate is in the range of at least about 0.5 liters per minute.

17. The method of claim 6 , wherein the drying step comprises spray drying.

18. The method of claim 12 , wherein the drying step comprises spray drying.

Assignments (8)