Abstract A solid solution of oxides of iron and of another divalent metal such as cobalt, more particularly for use in the manufacture of magnetic tapes and like magnetic carriers, is obtained first by preparing a mixed oxalate by co-precipitation of a solution of ammonium oxalate and of a solution containing Fe3 ions together with ions of the divalent metal, second by heating the mixed oxalate in air to decompose same while eliminating most of the carbon therefrom; third by heating the decomposed product in a wet hydrogen atmosphere to produce a substituted magnetic substantially free from residual carbon; and fourth by heating in air this substituted magnetite to oxidize same. The solid solution obtained corresponds to the formal ( gamma - Fe2O3)1 y (CoFe2O4)y in which y is comprised between zero and unity.
A METHOD FOR THE PREPARATION OF SOLID SOLUTIONS OF IRON AND COBALT OF THE TYPE (Y - FE2O3)1-Y (COFE2O4)Y WITH 0<Y <0.876 BY HOMOGENEOUS AND CONTROLLED SUBSTITUTION OF DIVALENT COBALT IONS FOR FE3+ IONS IN Y - FE2O3, COMPRISING THE FOLLOWING STEPS: A. PREPARING BY CO-PRECIPITATION A WATER INSOLUBLE MIXED OXALATE CONTAINING FE2+ IONS AND DIVALENT COBALT IONS, SAID MIXED OXALATE CORRESPONDING TO THE OFRMULA: FE1-XCOX(C2O4)2H2O WHEREIN THE VALUE OF X IS SUCH THAT THE RATIO OF OF COBALT TO IRON IN SAID OXALATE IS THE SAME AS THE RATIO OF COBALT TO IRON IN SAID SOLID SOLUTION; B. HEATING UNIFORMLY SAID MIXED OXALATE IN AIR AT A PROGRESSIVELY INCREASING TEMPERATURE IN THE RANGE OF 210*C TO 300*C UNTIL IT IS DECOMPOSED AND MOST OF THE RESULTANT CARBON IS ELIMATED, SAID HEATING STEP BEING STOPPED BEFORE ANY FORMATION OF RHOMBOEDRIC OXIDE A - FE2O3 AND OF SPINEL OXIDE COFE2O4; C. HEATING THE PRODUCT OF STEP B) IN A WET HYDROGEN ATMOOSPHERE CONTAINING ABOUT 7 PERCENT BY VOLUME OF STEAM AT SUCH A TEMPERATURE AS TO PRODUCE A SUBSTITUTED MAGNETITE FORMED OF CRYSTALLITES AND SUBSTANTIALLY FREE FROM RESIDUAL CARBON; D. AND HEATING IN AIR SAID SUBSTITUTED MAGNETITE TO A TEMPERATURE SUCH AS TO OXIDIZE SAME, SAID TMEPRATURE BEING BETWEEN ABOUT 210*C AND 380*C AND INCREASING IN DIRECT PROPORTION TO THE VALUE OF Y.
Claim 2
Independent Claim
222 words
A METHOD FOR THE PREPARATION OF SOLID SOLUTIONS OF IRON AND COBALT OF THE TYPE (Y - FE2O3)1-Y (COFE2O4)Y WITH 0<Y <0.876 BY HOMOGENEOUS AND CONTROLLED SUBSTITUTION OF DIVALENT COBALT IONS FOR FE3+ IONS IN Y - FE2O3, COMPRISING THE FOLLOWING STEPS: A. PREPARING BY CO-PRECIPITATION A WATER INSOLUBLE MIXED OXALATE CONTAINING FE2+ IONS AND DIVALENT COBALT IONS, SAID MIXED OXALATE CORRESPONDING TO THE OFRMULA: FE1-XCOX(C2O4)2H2O WHEREIN THE VALUE OF X IS SUCH THAT THE RATIO OF OF COBALT TO IRON IN SAID OXALATE IS THE SAME AS THE RATIO OF COBALT TO IRON IN SAID SOLID SOLUTION; B. HEATING UNIFORMLY SAID MIXED OXALATE IN AIR AT A PROGRESSIVELY INCREASING TEMPERATURE IN THE RANGE OF 210*C TO 300*C UNTIL IT IS DECOMPOSED AND MOST OF THE RESULTANT CARBON IS ELIMATED, SAID HEATING STEP BEING STOPPED BEFORE ANY FORMATION OF RHOMBOEDRIC OXIDE A - FE2O3 AND OF SPINEL OXIDE COFE2O4; C. HEATING THE PRODUCT OF STEP B) IN A WET HYDROGEN ATMOOSPHERE CONTAINING ABOUT 7 PERCENT BY VOLUME OF STEAM AT SUCH A TEMPERATURE AS TO PRODUCE A SUBSTITUTED MAGNETITE FORMED OF CRYSTALLITES AND SUBSTANTIALLY FREE FROM RESIDUAL CARBON; D. AND HEATING IN AIR SAID SUBSTITUTED MAGNETITE TO A TEMPERATURE SUCH AS TO OXIDIZE SAME, SAID TMEPRATURE BEING BETWEEN ABOUT 210*C AND 380*C AND INCREASING IN DIRECT PROPORTION TO THE VALUE OF Y.
Claim 3
Dependent Claim
27 words
In a method as claimed in claim 1, said water-insoluble mixed oxalate being heated during said second step with a temperature gradient of substantially 150*C per hour.
Claim 4
Dependent Claim
20 words
In a method as claimed in claim 2, said mixed oxalate being heated in the form of a thin layer.
Claim 5
Dependent Claim
35 words
In a method as claimed in claim 1, the product of step (b) being heated during step (c) at a temperature of substantially 260*C in said hydrogen atmosphere containing substantially 7 percent steam by volume.
Claim 6
Dependent Claim
43 words
In a method as claimed in claim 1, prior to step d, heating said substituted magnetite formed in step c Under vacuum at a temperature between 280* and 450*C to increase the dimension of said crystallites before submitting said magnetite to step d.
Claim 7
Dependent Claim
20 words
In a method as claimed in claim 1, said substituted magnetite being heated during step d. for substantially 72 hours.