Patent GB-966774-A (GB)
Title: Metal silicide compacts
IPC: C22C32/00
Filed: 1961-12-21
Abstract: Powdered compositions consisting essentially of 14-57% Si, 14-65% of each of at least two of the metals Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W and Fe, and from 5-20% ZrO2, ZnO or Cr2O3, are used for the manufacture of shaped objects by heating under pressure until a substantially homogeneous sintering and alloying of the ingredients occurs and then cooling the composition slowly to room temperature. In addition the composition may contain 1-12% of chemically combined nitrogen. Starting materials include commercial grades of ferrosilicon, silicon nitride, ferrotitanium, titanium disilicide silicotitanium, and elemental molybdenum, titanium and iron.  The binary alloys may contain up to 10% inert diluents, e.g. Al, Mn, Ca, Mg, Cu and Ni in elemental form or as the oxide.  The mesh size of all binary <PICT:0966774/C1/1> alloys and elemental metals used varied from 20-325 (U.S.standard sieve series) whereas the oxides ZrO2, ZnO, Cr2O3 had particle sizes of 600 mesh.  The compositions were weighed out and milled in presence of benzene (cyclohexane and acetone are also mentioned) which was thereafter evaporated.  A small amount of 1-5% agNaOH was added and the powder dried and passed through a 200 mesh screen, all particles being less than 10 micron in size, although acceptable products are obtained where the particle size is less than 75 micron. Fe-Mo-Si die nibs for hot metal extrusion are manufactured by forming from the prepared powders the desired shape in a mould, i.e. by applying 1000 p.s.i. at room temperature and increasing the temperature.  When the temperature is 1000 DEG  C. the pressure is raised to 2000 p.s.i. At 1300 DEG  C., 3000 p.s.i. pressure is applied and held for 15 minutes. The mould is allowed to cool in non-oxidizing conditions. The composition is treated by placing at 16 (Fig. 2), in a bore 9 in a cylindrical graphite mould 10 having a base plate 11 through which a core piece 12 extends, tamping with plunger 17 and placing the assembly in an hydraulic press. In general, pressures of 1500-5000 p.s.i. and temperatures of 1250-1800 DEG  C. may be employed.  Preferred compositions containing F3-Mo-Si or Fe-Si-Ti and ZrO2 may be sintered at 1300 DEG  C. and 3000 p.s.i. and Mo-N-Si-Ti compositions may be sintered at 1650-1675 DEG C. and 3500-4500 p.s.i. The shaped objects have high lubricity and toughness and when used for extruding metals in the form of a die nib no lubricant is required.  The compositions may be first partly reacted and then resintered to form the desired compact. Specifications 805,307, 966,778, U.S.A. Specification 2,878,113 and Canadian Specification 776,610 are referred to.ALSO:Powdered compositions consisting essentially of 14-57% Si, 14-65% of each of at least two of the metals Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W and Fe, and from 5-20% ZrO2, ZnO or Cr2O3, are used for the manufacture of shaped objects by heating under pressure until a substantially homogeneous sintering and alloying of the ingredients occurs and then cooling the composition slowly to room temperature. In addition the composition may <PICT:0966774/C6-C7/1> contain 1-12% of chemically combined nitrogen. Starting materials include commercial grades of ferrosilicon, silicon nitride, ferrotitanium, titanium disilicide silicotitanium, and elemental molybdenum, titanium and iron.  The binary alloys may contain up to 10% inert diluents, e.g. Al, Mn, Ca, Mg, Cu and Ni in elemental form or as the oxide.  The mesh size of all binary alloys and elemental metals used varied from 20-325 (U.S. standard sieve series) whereas the oxides ZrO2, ZnO, Cr2O3 had particle sizes of 600 mesh.  The compositions were weighed out and milled in presence of benzene, (cyclohexane and acetone are also mentioned) which was thereafter evaporated. A small amount of 1-5% ag NaOH was added and the powder dried and passed through a 200 mesh screen, all particles being less than 10 microns in size, although acceptable products are obtained where the particle size is less than 75 micron. Fe-Mo-Si die nibs for hot metal extrusion are manufactured by forming from the prepared powders the desired shape in a mould i.e. by applying 1000 p.s.i. at room temperature and increasing the temperature. When the temperature is 1000  DEG C. the pressure is raised to 2000 p.s.i.  At 1300  DEG C., 3000 p.s.i. pressure is applied and held for 15 minutes. The mould is allowed to cool in non-oxidizing conditions.  The composition is treated by placing at 16, Fig. 2, in a bore 9 in a cylindrical graphite mould 10 having a base plate 11 through which a core piece 12 extends, tamping with plunger 17 and placing the assembly in a hydraulic press.  In general, pressures of 1500-5000 p.s.i. and temperatures of 1250-1800  DEG C. may be employed.  Preferred compositions containing Fe-Mo-Si or Fe-Si-Ti and ZrO2 may be sintered at 1300  DEG C. and 3000 p.s.i. and Mo-N-Si-Ti compositions may be sintered at 1650-1675  DEG C. and 3500-4500 p.s.i.  The shaped objects have high lubricity and toughness and when used for extruding metals in the form of a die nib no lubricant is required. The compositions may be first partly reacted and then resintered to form the desired compact. Specifications 805,307, 966,778, U.S.A. Specification 2,878,113 and Canadian Specification 716,610 are referred to.