Methods of making a niobium metal oxide
View Patent ↗Methods to at least partially reduce a niobium oxide are described wherein the process includes heat treating the niobium oxide in the presence of a getter material and in an atmosphere which permits the transfer of oxygen atoms from the niobium oxide to the getter material, and for a sufficient time and at a sufficient temperature to form an oxygen reduced niobium oxide. Niobium oxides and/or suboxides are also described as well as capacitors containing anodes made from the niobium oxides and suboxides.
1. A method of forming a capacitor anode comprising a niobium oxide having an atomic ratio of niobium to oxygen of 1:less than 2.5, comprising forming said niobium oxide into the shape of an anode and sintering at a temperature of from about 800° C. to about 1200° C. for a time of from about 1 hour to about 10 hours;
anodizing at from about 16 to about 75 volts at a formation temperature of about 85° C.;
annealing said anode at a temperature of from about 300 to about 350° C. for a time of from about 10 minutes to about 60 minutes; and
manganizing said anode at a temperature of from about 220° to 280° C.
2. A method of forming a capacitor anode comprising a niobium oxide having an atomic ratio of niobium to oxygen of 1:less than 2.5, comprising forming said niobium oxide into the shape of an anode and sintering at a temperature of from about 800° C. to about 1200° C. for a time sufficient to form a capacitor anode.
3. The method of claim 2 , wherein said time is from about 1 hour or less to about 10 hours or more.
4. The method of claim 2 , wherein said time is from about 1 hour to about 4 hours.
5. The method of claim 2 , wherein in said sintering temperature is from about 900° to about 1200° C.
6. The method of claim 2 , wherein in said sintering temperature is from about 1000° to about 1100° C.
7. A method to achieve low shrinkage of a capacitor anode comprising forming a capacitor anode comprising a niobium oxide having an atomic ratio of niobium to oxygen 1: less than 2.5, comprising forming said niobium oxide into the shape of an anode and sintering at a temperature of from about 800° C. to about 1200° C. for a sufficient time to form a capacitor anode having capacitance.
8. The method of claim 2 , wherein said time is 1 day or more.