Methods of making titanium diboride powders
View Patent ↗The present disclosure is directed towards methods of making titanium diboride products in various sizes. An aspect of the method provides (a) selecting a target average particle size for a target titanium diboride product; (b) selecting at least one processing variable from the group consisting of: an amount of sulfur, an inert gas flow rate, a soak time, and a reaction temperature; (c) selecting a condition of the processing variable based upon the target average particle size; and (d) producing an actual titanium diboride product having an actual average particle size using the at least one processing variable, wherein due to the at least one processing variable, the actual average particle size corresponds to the target average particle size.
1. A method comprising:
(a) selecting a target average particle size for a target titanium diboride product;
(b) selecting an amount of sulfur based upon the target average particle size;
(c) producing an actual titanium diboride product via a reaction having the amount of sulfur present in a precursor mixture, wherein the titanium diboride product comprises an average particle, wherein, due to the amount of sulfur, the average particle size corresponds to the target average particle size.
2. The method of claim 1 , further wherein the producing step comprises
an average particle size within about 20% of the average particle size of the target titanium diboride product.
3. The method of claim 1 further comprising a reaction temperature, wherein the reaction temperature is at least about 1300° C.
4. The method of claim 1 further comprising a soak time, wherein the soak time is at least about 0.5 hr.
5. The method of claim 1 further comprising an inert gas flow rate wherein the inert gas flow rate is in the range of at least about 0.5 liters per minute through a reaction vessel comprising a volume of at least 0.7 liters.
6. The method of claim 1 , wherein the producing step further comprises carbothermically reacting.
7. The method of claim 1 , further comprising:
de-agglomerating the actual titanium diboride product.
8. The method of claim 1 , wherein the producing step further comprises:
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.
9. A method comprising:
(a) selecting a target average particle size for a target titanium diboride product;
(b) selecting an amount of sulfur based upon the target average particle size;
(c) producing an actual titanium diboride product by reacting a precursor mixture comprising a titanium source, a boron source, a carbon source, and the amount of sulfur, wherein the titanium diboride product comprises an average particle size, wherein, due to the amount of sulfur, the average particle size corresponds to the target average particle size.
10. The method of claim 9 , wherein the carbon source comprises the amount of sulfur.
11. The method of claim 10 , wherein the producing step further comprises:
preparing an agglomerated mixture including:
mixing into a liquid the boron source; the carbon source; the titanium source, and optional additives to form a suspension; and
drying the suspension to produce the agglomerated precursor mixture.
12. The method of claim 11 , wherein the drying step further comprises spray drying.
13. The method of claim 9 , further comprising:
selecting at least one processing variable from the group consisting of: an inert gas flow rate, a soak time, and a reaction temperature; and
selecting a condition of the processing variable based upon at least one of:
the target average particle size; and
the amount of sulfur.
14. The method of claim 9 , further comprising:
deagglomerating the actual titanium diboride product to remove a plurality of agglomerations in the actual titanium diboride product.
15. The method of claim 9 , wherein deagglomerating further comprises:
milling the titanium diboride product for a length of time based upon the amount of sulfur in the precursor mixture.
16. The method of claim 9 , wherein the producing step comprises carbothermically reacting.
17. A method comprising:
(a) selecting a target average particle size for a target titanium diboride product;
(b) selecting an amount of sulfur based upon the target average particle size;
(c) preparing a precursor mixture by forming a spray dried suspension of: a titanium source, a boron source, and a carbon source, the precursor mixture including the amount of sulfur; and
(d) producing an actual titanium diboride product by carbothermically reacting a precursor mixture, wherein the actual titanium diboride product comprises an actual average particle size, wherein, due to the amount of sulfur, the average particle size corresponds to the target average particle size.
18. The method of claim 17 , further comprising the step of:
processing the actual titanium diboride product into a product selected from: a cathode; and a structure of an aluminum electrolysis cell.
19. The method of claim 17 , comprising de-agglomerating the actual titanium diboride product to break up agglomerations of the actual titanium diboride particles.