US2003132123A1PendingUtilityA1

Methods of forming titanium-based and zirconium-based mixed-metal materials

40
Priority: Oct 24, 2000Filed: Jan 21, 2003Published: Jul 17, 2003
Est. expiryOct 24, 2020(expired)· nominal 20-yr term from priority
C22B 34/1263C23C 14/3414C22B 34/14C22C 14/00
40
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Claims

Abstract

The invention encompasses methods of forming titanium-based mixed-metal materials and zirconium-based mixed-metal materials utilizing one or more of a reduction process, electrolysis process and iodide process. The invention also encompasses a sputtering target comprising zirconium and one or more elements selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, Ti, V, W, Y, and Yb. The invention also encompasses a sputtering target comprising titanium and boron.

Claims

exact text as granted — not AI-modified
1 . A method of forming a titanium-based mixed-metal product, comprising combining a mixture of titanium halide and at least one metal halide with a reducing agent to produce a mixed-metal product comprising titanium and at least one metal corresponding to the at least one metal of the at least one metal halide; wherein, 
 the at least one metal of the at least one metal halide is selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y, Yb and Zr;    the mixed-metal product is at least 99.95% pure; and    the mixed-metal product comprises greater than 0.05% of the at least one metal.    
     
     
         2 . The method of  claim 1  wherein the mixed-metal product comprises greater than 0.1% of the at least one metal.  
     
     
         3 . The method of  claim 1  wherein the mixed-metal product comprises greater than 0.5% of the at least one metal.  
     
     
         4 . The method of  claim 1  wherein the at least one metal is only one metal.  
     
     
         5 . The method of  claim 1  wherein the at least one metal is two metals.  
     
     
         6 . The method of  claim 1  wherein the at least one metal comprises Zr.  
     
     
         7 . The method of  claim 1  wherein the at least one metal comprises Hf.  
     
     
         8 . A method of forming a titanium-based mixed-metal product, comprising electrolytically depositing a mixed-metal product comprising a mixture of titanium and at least one other metal, the at least one other metal being selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y, Yb and Zr; wherein 
 the mixed-metal product is at least 99.95% pure; and    the mixed-metal product comprises greater than 0.05% of the at least one other metal.    
     
     
         9 . The method of  claim 8  wherein the mixed-metal product comprises greater than 0.1% of the at least one other metal.  
     
     
         10 . The method of  claim 8  wherein the mixed-metal product comprises greater than 0.5% of the at least one other metal.  
     
     
         11 . The method of  claim 8  wherein the at least one other metal is only one other metal.  
     
     
         12 . The method of  claim 8  wherein the at least one other metal is two other metals.  
     
     
         13 . The method of  claim 8  wherein the at least one metal comprises Zr.  
     
     
         14 . The method of  claim 8  wherein the at least one metal comprises Hf.  
     
     
         15 . A method of forming a titanium-based mixed-metal product, comprising: 
 providing a mixture of titanium and least one other metal in a reaction apparatus with iodine gas and a heated substrate; the at least one other metal being selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y, Yb and Zr;    reacting the titanium and the at least one other metal with the iodine gas to form titanium iodide and an iodide of the at least one other metal;    transferring the titanium iodide and the iodide of the at least one other metal to the heated substrate, and utilizing heat from the substrate to decompose the iodides and produce a mixed-metal product comprising titanium and the at least one other metal; wherein 
 the mixed-metal product is at least 99.95% pure; and  
 the mixed-metal product comprises greater than 0.05% of the at least one other metal.  
   
     
     
         16 . The method of  claim 15  wherein the mixed-metal product comprises greater than 0.1% of the at least one other metal.  
     
     
         17 . The method of  claim 15  wherein the mixed-metal product comprises greater than 0.5% of the at least one other metal.  
     
     
         18 . The method of  claim 15  wherein the at least one other metal is only one other metal.  
     
     
         19 . The method of  claim 15  wherein the at least one other metal is two other metals.  
     
     
         20 . The method of  claim 15  wherein the at least one metal comprises Zr.  
     
     
         21 . The method of  claim 15  wherein the at least one metal comprises Hf.  
     
     
         22 . A method of forming a zirconium-based mixed-metal product, comprising combining a mixture of zirconium halide and at least one metal halide with a reducing agent to produce a mixed-metal product comprising zirconium and at least one metal corresponding to the at least one metal of the at least one metal halide; wherein, 
 the at least one metal of the at least one metal halide is selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, Ti, V, W, Y, and Yb;    the mixed-metal product is at least 99.95% pure; and    the mixed-metal product comprises greater than 0.05% of the at least one metal.    
     
     
         23 . The method of  claim 22  wherein the mixed-metal product comprises greater than 0.1% of the at least one metal.  
     
     
         24 . The method of  claim 22  wherein the mixed-metal product comprises greater than 0.5% of the at least one metal.  
     
     
         25 . The method of  claim 22  wherein the at least one metal is only one metal.  
     
     
         26 . The method of  claim 22  wherein the at least one metal is two metals.  
     
     
         27 . The method of  claim 22  wherein the at least one metal comprises Ti.  
     
     
         28 . The method of  claim 22  wherein the at least one metal comprises Hf.  
     
     
         29 . A method of forming a zirconium-based mixed-metal product, comprising electrolytically depositing a mixed-metal product comprising a mixture of zirconium and at least one other metal, the at least one other metal being selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, Ti, V, W, Y, and Yb; wherein 
 the mixed-metal product is at least 99.95% pure; and    the mixed-metal product comprises greater than 0.05% of the at least one other metal.    
     
     
         30 . The method of  claim 29  wherein the mixed-metal product comprises greater than 0.1% of the at least one other metal.  
     
     
         31 . The method of  claim 29  wherein the mixed-metal product comprises greater than 0.5% of the at least one other metal.  
     
     
         32 . The method of  claim 29  wherein the at least one other metal is only one other metal.  
     
     
         33 . The method of  claim 29  wherein the at least one other metal is two other metals.  
     
     
         34 . The method of  claim 29  wherein the at least one metal comprises Ti.  
     
     
         35 . The method of  claim 29  wherein the at least one metal comprises Hf.  
     
     
         36 . A method of forming a zirconium-based mixed-metal product, comprising: 
 providing a mixture of zirconium and least one other metal in a reaction apparatus with iodine gas and a heated substrate; the at least one other metal being selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, Ti, V, W, Y, and Yb;    reacting the zirconium and the at least one other metal with the iodine gas to form zirconium iodide and an iodide of the at least one other metal;    transferring the zirconium iodide and the iodide of the at least one other metal to the heated substrate, and utilizing heat from the substrate to decompose the iodides and produce a mixed-metal product comprising zirconium and the at least one other metal; wherein 
 the mixed-metal product is at least 99.95% pure; and  
 the mixed-metal product comprises greater than 0.05% of the at least one other metal.  
   
     
     
         37 . The method of  claim 36  wherein the mixed-metal product comprises greater than 0.1% of the at least one other metal.  
     
     
         38 . The method of  claim 36  wherein the mixed-metal product comprises greater than 0.5% of the at least one other metal.  
     
     
         39 . The method of  claim 36  wherein the at least one other metal is only one other metal.  
     
     
         40 . The method of  claim 36  wherein the at least one other metal is two other metals.  
     
     
         41 . The method of  claim 36  wherein the at least one metal comprises Ti.  
     
     
         42 . The method of  claim 36  wherein the at least one metal comprises Hf.  
     
     
         43 . A method of forming a titanium-based mixed-metal ingot, comprising: 
 combining a mixture of titanium halide and one or more other metal halides with a reducing agent to produce a mixed-metal product; wherein the one or more other metal halides are selected from the group consisting of halides of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y, Yb and Zr;    melting the mixed-metal product to form a molten mixed-metal material; and    cooling the molten mixed-metal material into a mixed-metal ingot; the ingot comprising titanium and one or more other metals; the one or more other metals corresponding to one or more of the other metals of the one or more metal halides; the titanium being the majority element of the ingot; the ingot having a purity of titanium and the one or more other metals of at least 99.95%.    
     
     
         44 . The method of  claim 43  wherein the titanium halide is a titanium chloride, and wherein the other metal halides are metal chlorides.  
     
     
         45 . The method of  claim 43  wherein the ingot has a purity of the titanium and the one or more other metals of at least 99.995%.  
     
     
         46 . The method of  claim 43  wherein the ingot has a purity of the titanium and the one or more other metals of at least 99.9995%.  
     
     
         47 . The method of  claim 43  wherein the one or more other metals comprise zirconium.  
     
     
         48 . The method of  claim 43  wherein the one or more other metals is only one other metal and consists of zirconium.  
     
     
         49 . The method of  claim 43  further comprising forming a sputtering target from the ingot.  
     
     
         50 . A method of forming a zirconium-based mixed-metal ingot, comprising: 
 combining a mixture of zirconium halide and one or more other metal halides with a reducing agent to produce a mixed-metal product;    melting the mixed-metal product to form a molten mixed-metal material; and    cooling the molten mixed-metal material into a mixed-metal ingot, the ingot comprising zirconium and one or more other metals corresponding to the one or more other metals of the one or more metal halides, the zirconium being the majority element of the ingot; the ingot having a purity of zirconium and the one or more other metals of at least 99.95%.    
     
     
         51 . The method of  claim 50  wherein the zirconium halide is a zirconium chloride, and wherein the other metal halides are metal chlorides.  
     
     
         52 . The method of  claim 50  wherein the ingot has a purity of the zirconium and the one or more other metals of at least 99.995%.  
     
     
         53 . The method of  claim 50  wherein the ingot has a purity of the zirconium and the one or more other metals of at least 99.9995%.  
     
     
         54 . The method of  claim 50  wherein the one or more other metals are selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, Ti, V, W, Y, and Yb.  
     
     
         55 . The method of  claim 50  wherein the one or more other metals comprise titanium.  
     
     
         56 . The method of  claim 50  wherein the one or more other metals is only one other metal and consists of titanium.  
     
     
         57 . The method of  claim 50  wherein the reducing agent is selected from the group consisting of sodium metal and magnesium metal.  
     
     
         58 . The method of  claim 50  further comprising forming a sputtering target from the ingot.  
     
     
         59 . A method of forming a titanium-based mixed-metal ingot, comprising: 
 electrolytically depositing a mixture of titanium and at least one other metal, the deposited mixture being a mixed-metal product;    melting the mixed-metal product to form a molten mixed-metal material; and    cooling the molten mixed-metal material into a mixed-metal ingot, the ingot comprising the titanium and the at least one other metal, the titanium being the majority element of the ingot; the ingot having a purity of titanium and the at least one other metal of at least 99.95%.    
     
     
         60 . The method of  claim 59  wherein the at least one other metal that is deposited has a deposition reduction potential within ±0.7 volts of the reduction potential for conversion of Ti 2+  to elemental Ti.  
     
     
         61 . The method of  claim 59  wherein the at least one other metal that is deposited has a deposition reduction potential within ±0.5 volts of the reduction potential for conversion of Ti 2+  to elemental Ti.  
     
     
         62 . The method of  claim 59  wherein the at least one other metal that is deposited includes Zr.  
     
     
         63 . The method of  claim 59  wherein the at least one other metal that is deposited is only one other metal and consists of Zr.  
     
     
         64 . The method of  claim 59  further comprising: 
 combining a mixture of titanium halide and metal halide with a reducing agent to produce a mixed-metal feedstock, the metal halide comprising the at least one other metal; and  
 wherein the electrolytically depositing utilizes the mixed-metal feedstock as an anode and comprises transferring titanium and the at least one other metal from the anode to a cathode whereupon the titanium and at least one other metal are deposited as the mixed-metal product.  
 
     
     
         65 . A method of forming a zirconium-based mixed-metal ingot, comprising: 
 electrolytically depositing a mixture of zirconium and at least one other metal, the deposited mixture being a mixed-metal product;    melting the mixed-metal product to form a molten mixed-metal material; and    cooling the molten mixed-metal material into a mixed-metal ingot, the ingot comprising the zirconium and the at least one other metal, the zirconium being the majority element of the ingot; the ingot having a purity of zirconium and the at least one other metal of at least 99.95%.    
     
     
         66 . The method of  claim 65  wherein the at least one other metal that is deposited has a deposition reduction potential within ±0.7 volts of the reduction potential for conversion of Zr 2+  to elemental Zr.  
     
     
         67 . The method of  claim 65  wherein the at least one other metal that is deposited has a deposition reduction potential within ±0.5 volts of the reduction potential for conversion of Zr 2+  to elemental Zr.  
     
     
         68 . The method of  claim 65  wherein the at least one other metal that is deposited includes Ti.  
     
     
         69 . The method of  claim 65  wherein the at least one other metal that is deposited is only one other metal and consists of Ti.  
     
     
         70 . The method of  claim 65  further comprising: 
 combining a mixture of zirconium halide and metal halide with a reducing agent to produce a mixed-metal feedstock, the metal halide comprising the at least one other metal; and  
 wherein the electrolytically depositing utilizes the mixed-metal feedstock as an anode and comprises transferring zirconium and the at least one other metal from the anode to a cathode whereupon the zirconium and at least one other metal are deposited as the mixed-metal product.  
 
     
     
         71 . A method of forming a titanium-based mixed-metal ingot, comprising: 
 providing a mixture of titanium and least one other metal in a reaction apparatus with iodine gas and a heated substrate;    reacting the titanium and the at least one other metal with the iodine gas to form titanium iodide and an iodide of the at least one other metal;    transferring the titanium iodide and the iodide of the at least one other metal to the heated substrate, and utilizing heat from the substrate to decompose the iodides and produce a mixed-metal product, the mixed-metal product comprising titanium and the at least one other metal;    melting the mixed-metal product to form a molten mixed-metal material; and    cooling the molten mixed-metal material into a mixed-metal ingot, the ingot comprising the titanium and the at least one other metal, the titanium being the majority element of the ingot; the ingot having a purity of titanium and the at least one other metal of at least 99.95%.    
     
     
         72 . The method of  claim 71  wherein the at least one other metal is selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y, Yb and Zr.  
     
     
         73 . The method of  claim 71  wherein the at least one other metal comprises zirconium.  
     
     
         74 . The method of  claim 71  wherein the at least one other metal is only one other metal and consists of zirconium.  
     
     
         75 . The method of  claim 71  further comprising forming the mixture of titanium and the at least one other metal by combining a mixture of titanium halide and metal halide with a reducing agent to produce the mixture, the metal halide comprising the at least one other metal.  
     
     
         76 . The method of  claim 71  further comprising forming the mixture of titanium and the at least one other metal by electrolytically depositing the mixture of titanium and the at least one other metal.  
     
     
         77 . The method of  claim 76  further comprising: 
 combining a mixture of titanium halide and metal halide with a reducing agent to produce a mixed-metal feedstock, the metal halide comprising the at least one other metal; and  
 wherein the electrolytically depositing utilizes the mixed-metal feedstock as an anode and comprises transferring titanium and the at least one other metal from the anode to a cathode whereupon the titanium and at least one other metal are deposited as the mixture of titanium and the at least one other metal.  
 
     
     
         78 . A method of forming a zirconium-based mixed-metal ingot, comprising: 
 providing a mixture of zirconium and least one other metal in a reaction apparatus with iodine gas and a heated substrate;    reacting the zirconium and the at least one other metal with the iodine gas to form zirconium iodide and an iodide of the at least one other metal;    transferring the zirconium iodide and the iodide of the at least one other metal to the heated substrate, and utilizing heat from the substrate to decompose the iodides and produce a mixed-metal product, the mixed-metal product comprising zirconium and the at least one other metal;    melting the mixed-metal product to form a molten mixed-metal material; and    cooling the molten mixed-metal material into a mixed-metal ingot, the ingot comprising the zirconium and the at least one other metal, the zirconium being the majority element of the ingot; the ingot having a purity of zirconium and the at least one other metal of at least 99.95%.    
     
     
         79 . The method of  claim 78  wherein the at least one other metal is selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, Ti, V, W, Y, and Yb.  
     
     
         80 . The method of  claim 78  wherein the at least one other metal comprises titanium.  
     
     
         81 . The method of  claim 78  wherein the at least one other metal is only one other metal and consists of titanium.  
     
     
         82 . The method of  claim 78  further comprising forming the mixture of zirconium and the at least one other metal by combining a mixture of zirconium halide and metal halide with a reducing agent to produce the mixture, the metal halide comprising the at least one other metal.  
     
     
         83 . The method of  claim 78  further comprising forming the mixture of zirconium and the at least one other metal by electrolytically depositing the mixture of zirconium and the at least one other metal.  
     
     
         84 . The method of  claim 83  further comprising: 
 combining a mixture of zirconium halide and metal halide with a reducing agent to produce a mixed-metal feedstock, the metal halide comprising the at least one other metal; and  
 wherein the electrolytically depositing utilizes the mixed-metal feedstock as an anode and comprises transferring zirconium and the at least one other metal from the anode to a cathode whereupon the zirconium and at least one other metal are deposited as the mixture of zirconium and the at least one other metal.  
 
     
     
         85 . A sputtering target comprising Zr and one or more elements selected from the group consisting of Al, B, Ba, Be, Ca, Ce, Co, Cs, Dy, Er, Fe, Gd, Hf, Ho, La, Mg, Mn, Mo, Nb, Nd, Ni, Pr, Sc, Sm, Sr, Ta, V, W, Y, and Yb; the Zr being the majority element of the target.  
     
     
         86 . The sputtering target of  claim 85  wherein the Zr concentration within the target is at least 70%.  
     
     
         87 . The sputtering target of  claim 85  wherein the Zr concentration within the target is at least 90%.  
     
     
         88 . The sputtering target of  claim 85  wherein the Zr concentration within the target is at least 94%.  
     
     
         89 . The sputtering target of  claim 85  wherein the Zr concentration within the target is at least 97%.  
     
     
         90 . The sputtering target of  claim 85  wherein the Zr concentration within the target is less than 98%.  
     
     
         91 . The sputtering target of  claim 85  wherein the total non-zirconium metal content of the target is in a range of from 0.001% to 50% of the ingot.  
     
     
         92 . The sputtering target of  claim 85  wherein the total non-zirconium metal content of the target is in a range of 0.001% to 10% of the ingot.  
     
     
         93 . The sputtering target of  claim 85  wherein the total non-zirconium metal content of the target is at least 0.01% of the ingot.  
     
     
         94 . The sputtering target of  claim 85  wherein the total non-zirconium metal content of the target is at least 0.1% of the ingot.  
     
     
         95 . The sputtering target of  claim 85  wherein the total non-zirconium metal content of the target is at least 1% of the ingot.  
     
     
         96 . The sputtering target of  claim 85  wherein the total non-zirconium metal content of the target is at least 2% of the ingot.  
     
     
         97 . The sputtering target of  claim 85  consisting of Zr and Ti.  
     
     
         98 . A sputtering target comprising Zr and Ti; the Zr being the majority element of the target and being present to a concentration within the target of at least 55%.  
     
     
         99 . The sputtering target of  claim 98  wherein the Zr concentration within the target is at least 70%.  
     
     
         100 . The sputtering target of  claim 98  wherein the Zr concentration within the target is at least 90%.  
     
     
         101 . The sputtering target of  claim 98  wherein the Zr concentration within the target is at least 94%.  
     
     
         102 . The sputtering target of  claim 98  wherein the Zr concentration within the target is at least 97%.  
     
     
         103 . The sputtering target of  claim 98  wherein the Zr concentration within the target is less than 98%.  
     
     
         104 . A sputtering target comprising Ti and B; the Ti being the majority element of the target.  
     
     
         105 . The sputtering target of  claim 104  wherein the Ti concentration within the target is at least 70%.  
     
     
         106 . The sputtering target of  claim 104  wherein the Ti concentration within the target is at least 90%.  
     
     
         107 . The sputtering target of  claim 104  wherein the Ti concentration within the target is at least 94%.  
     
     
         108 . The sputtering target of  claim 104  wherein the Ti concentration within the target is at least 97%.  
     
     
         109 . The sputtering target of  claim 108  wherein the B content of the target is greater than 5 ppm.  
     
     
         110 . The sputtering target of  claim 108  wherein the B content of the target is greater than 50 ppm.  
     
     
         111 . The sputtering target of  claim 108  wherein the B content of the target is greater than 500 ppm.  
     
     
         112 . The sputtering target of  claim 108  wherein the B content of the target is greater than one part per thousand.  
     
     
         113 . The sputtering target of  claim 104  wherein the Ti concentration within the target is less than 98%.  
     
     
         114 . The sputtering target of  claim 104  wherein the B content of the target is greater than 5 ppm.  
     
     
         115 . The sputtering target of  claim 104  wherein the B content of the target is greater than 50 ppm.  
     
     
         116 . The sputtering target of  claim 104  wherein the B content of the target is greater than 500 ppm.  
     
     
         117 . The sputtering target of  claim 104  wherein the B content of the target is greater than one part per thousand.  
     
     
         118 . The sputtering target of  claim 104  consisting of Ti and B.

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