Synthetic spinels and processes for making them
First Claim
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1. A process for making a synthetic spinel having the general formula R2+ O.R23+ O3, said process comprising:
- (1) mixing, to a homogeneous consistency;
(i) a composition of R2+ [A] ("the R2+ [A] composition") having a R2+ [A] compound whose chemical particles are in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, (ii) a composition of R3+ [B] ("the R3+ [B] composition") having a R3+ [B] compound whose chemical particles are also in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, and mixed such that the starting ratio of R2+ atoms to R3+ atoms is from about 0.5 to about 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium constitutes from about 50 to about 90 weight percent of said total mixture and wherein;
(i) R2+ is a first metallic atom having a first, positive, oxidation state, (ii) R3+ is a second metallic atom having a second, positive, oxidation state higher than the first positive oxidation state of the first metallic atom, and (iii) the R2+ [A] compound is introduced to the R3+ [B] compound in the form of a R2+ [A] composition having a pH from about 3.5 to about 6.5 and [A] and [B] are nonmetallic atoms which each carry a net negative charge when respectively chemically bonded to the R2+ and R3+ metallic atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];
(2) spray-drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the R2+ [A] compound and the R3+ [B] compound through the liquid medium, (ii) segregation of the R2+ [A] compound and the R3+ [B] compound into discrete enclaves within a resulting synthetic spinel is precluded and (iii) finely divided, solid, particles are obtained wherein the starting ratio of R2+ atoms to R3+ atoms of the total mixture is substantially maintained in said particles; and
(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of R2+ oxide (R2+ O) and R3+ oxide (R23+ O3) having a range of molecular ratios of R2+ O to R23+ O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the R2+ O and in the R23+ O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of R2+ and R3+.
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Abstract
Spinels can be synthesized by uniformly dispersing predetermined quantities of ingredient compounds whose particles have sizes no greater than about 5 nanometers in a liquid medium, arresting the ingredient compounds in a solid matrix by spray drying said liquid medium and then calcining the resulting particles to form a solid solution of oxides of said compounds in a crystalline lattice which is substantially free of undesired complex compounds of the ingredient compounds.
38 Citations
92 Claims
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1. A process for making a synthetic spinel having the general formula R2+ O.R23+ O3, said process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a composition of R2+ [A] ("the R2+ [A] composition") having a R2+ [A] compound whose chemical particles are in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, (ii) a composition of R3+ [B] ("the R3+ [B] composition") having a R3+ [B] compound whose chemical particles are also in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, and mixed such that the starting ratio of R2+ atoms to R3+ atoms is from about 0.5 to about 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium constitutes from about 50 to about 90 weight percent of said total mixture and wherein;
(i) R2+ is a first metallic atom having a first, positive, oxidation state, (ii) R3+ is a second metallic atom having a second, positive, oxidation state higher than the first positive oxidation state of the first metallic atom, and (iii) the R2+ [A] compound is introduced to the R3+ [B] compound in the form of a R2+ [A] composition having a pH from about 3.5 to about 6.5 and [A] and [B] are nonmetallic atoms which each carry a net negative charge when respectively chemically bonded to the R2+ and R3+ metallic atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];(2) spray-drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the R2+ [A] compound and the R3+ [B] compound through the liquid medium, (ii) segregation of the R2+ [A] compound and the R3+ [B] compound into discrete enclaves within a resulting synthetic spinel is precluded and (iii) finely divided, solid, particles are obtained wherein the starting ratio of R2+ atoms to R3+ atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of R2+ oxide (R2+ O) and R3+ oxide (R23+ O3) having a range of molecular ratios of R2+ O to R23+ O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the R2+ O and in the R23+ O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of R2+ and R3+. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13)
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14. A process for making a synthetic spinel having the general formula Mg O.Al2 O3, said process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a liquid composition of magnesium (Mg[A], "the magnesia") having a Mg[A] compound whose chemical particles are in a size range from molecular size to particles having average diameters of no more than about 5 nanometers, (ii) a liquid composition of aluminum (Al[B], "the alumina") having an Al[B] compound whose chemical particles are also in a size range from molecular size to particles having average diameters no more than about 5 nanometers, and mixed such that the starting ratio of magnesium atoms to aluminum atoms is substantially from 0.5 to 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium constitutes from about 50 to about 90 weight percent of said total mixture and wherein the Mg[A] compound is introduced to the Al[B] compound in the form of a magnesia composition having a pH from about 3.5 to 6.5 and [A] and [B] are nonmetallic atoms which carry a net negative charge when respectively chemically bonded to the magnesia and alumina atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];(2) spray drying the total mixture under such conditions that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the magnesia and the alumina through the liquid medium, (ii) segregation of the magnesia and the alumina into discrete enclaves within a resulting synthetic spinel is precluded and (iii) finely divided, solid, particles are obtained wherein the starting ratio of magnesium atoms to aluminum atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of magnesium oxide (MgO) and aluminum oxide (Al2 O3) having a range of molecular ratios of MgO to Al2 O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the MgO and in the Al2 O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of magnesium and aluminum. - View Dependent Claims (15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26)
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27. A spinel having the general formula R2+ O.R3+ O3, made by a process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a composition of R2+ [A] ("the R2+ [A] composition") having a R2+ [A] compound whose chemical particles are in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, (ii) a composition R3+ [B] ("the R3+ [B] composition") having a R3+ [B] compound whose chemical particles are also in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, and mixed such that the starting ratio of R2+ atoms to R3+ atoms is from about 0.5 to about 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium constitutes from about 50 to about 90 weight percent of said total mixture and wherein (i) R2+ is a first metallic atom having a first, positive, oxidation state, (ii) R3+ is a second metallic atom having a second, positive, oxidation state higher than the first positive oxidation state of the first metallic atom and (iii) the R2+ [A] compound is introduced to the R3+ [B] compound in the form of a R2+ [A] composition having a pH from about 3.5 to about 6.5 and [A] and [B] are nonmetallic atoms which carry a net negative charge when respectively chemically bonded to the R2+ and R3+ metallic atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];(2) spray drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the R2+ A] compound and the R3+ [B] compound through the liquid medium, (ii) segregation of the R2+ [A] compound and the R3+ [B] compound into discrete enclaves within a resulting synthetic spinel is precluded, (iii) finely divided, solid, particles are obtained wherein the starting ratio of R2+ atoms to R3+ atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of R2+ oxide (R3+ O) and R3+ oxide (R23+ O3) having a range of molecular ratios of R3+ O to R23+ O3) from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the R2+ O and in the and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of R2+ and R3+. - View Dependent Claims (28, 29, 30, 31, 32, 33, 34, 35)
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36. A spinel having the general formula MgO. Al2 O3, made by a process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a composition of magnesium (Mg[A], "the magnesia") having a Mg[A] compound whose chemical particles are in a size range from molecular size to particles having average diameters no more than about 5 nanometers, (ii) a composition of aluminum (Al[B], "the alumina") having an Al[B] compound whose chemical particles are also in a size range from molecular size to particles having average diameters no more than about 5 nanometers, and mixed such that the starting ratio of magnesium atoms to aluminum atoms is substantially from 0.5 to 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium constitutes from about 50 to about 90 weight percent of said total mixture and wherein the Mg[A] compound is introduced to the Al[B] compound in the form of a magnesia composition having a pH from about 3.5 to about 6.5 and [A] and [B] are each nonmetallic elements which bear a net negative charge when respectively chemically bonded to the magnesia and alumina atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic elements of [A] and [B];(2) spray drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the magnesia and the alumina through the liquid medium, (ii) segregation of the magnesia and the alumina into discrete enclaves within a resulting synthetic spinel is precluded, and (iii) finely divided, solid, particles are obtained wherein the starting ratio of magnesium atoms to aluminum atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid particles under conditions which produce crystals of a solid solution of magnesium oxide (MgO) and aluminum oxide (Al2 O3) having a range of molecular ratios of MgO to Al2 O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the MgO and in the Al2 O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of magnesium and aluminum. - View Dependent Claims (37, 38, 39, 40, 41, 42, 43, 44, 45, 46)
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47. A process for making a synthetic spinel having the general formula R2 O.R23+ O3, said process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a composition of R2+ [A] ("the R2+ O[A] composition") having a R2+ [A] compound whose chemical particles are in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, (ii) a composition of R3+ [B] ("the R3+ [B] composition") having a R3+ [B] compound whose chemical particles are of a size greater than 5 nanometers, but less than about 60 nanometers, and which have a three dimensional crystalline lattice structure having three axes wherein the crystalline lattice structure having three axes has lattice spacings which are unequal along at least two of the three axes, and which can be broken down into particles having ultimate crystallite sizes of less than about 5 nanometers by physico-chemical forces applied during a mixing step of said process, and mixed such that the starting ratio of R2+ atoms to R3+ atoms is from about 0.5 to about 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium is capable of breaking down particles of R3+ [B] compound to ultimate crystallite sizes of less than 5 nanometers and which constitutes from about 50 to about 90 weight percent of said total mixture and wherein;
(i) R2+ is a first metallic atom having a first, positive, oxidation state, (ii) R3+ is a second metallic atom having a second, positive, oxidation state higher than the first positive oxidation state of the first metallic atom, and (iii) the R2+ [A] compound is introduced to the R3+ [B] compound in the form of a R2+ [A] composition having a pH from about 3.5 to about 6.5 and [A] and [B] are comprised of nonmetallic atoms which carry a net negative charge when they are, respectively, chemically bonded to the R2+ and R3+ metallic atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];(2) spray-drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the R2+ [A] compound and the R3+ [B] compound through the liquid medium, (ii) segregation of the R2+ [A] compound and the R3+ [B] compound into discrete enclaves within a resulting synthetic spinel is precluded and (iii) finely divided, solid, particles are obtained wherein the starting ratio of R2+ atoms to R3+ atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of R2+ oxide (R2+ O) and R3+ oxide (R23+ O3) having a range of molecular ratios of R2+ O to R23+ O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the R2+ O and in the and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of R2+ and R3+. - View Dependent Claims (48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59)
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60. A process for making a synthetic spinel having the general formula Mg O.Al2 O3, said process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a liquid composition of magnesium (Mg[A], "the magnesia") having a Mg[A] compound whose chemical particles are in a size greater than 5 nanometers, but less than about 60 nanometers, and which have a three dimensional crystalline lattice structure having three axes wherein the crystalline lattice structure having three axes has lattice spacings which are unequal along at least two of the three axes, and which can be broken down into particles having ultimate crystallite sizes of less than about 5 nanometers by physico-chemical forces applied during a mixing step of said process, (ii) a liquid composition of aluminum (Al[B], "the alumina") having an Al[B] compound whose chemical particles are also in a size greater than 5 nanometers, but less than about 60 nanometers, and which have a three dimensional crystalline lattice structure having three axes wherein the crystalline lattice structure having three axes has lattice spacings which are unequal along at least two of the three axes, and which can be broken down into particles having ultimate crystallite sizes of less than about 5 nanometers by physico-chemical forces applied during a mixing step of said process, and mixed such that the starting ratio of magnesium atoms to aluminum atoms is substantially from 0.5 to 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium is capable of breaking down the particles of the R2+ [A] compound and the R3+ [B] compound to their respective ultimate crystallite sizes and which constitutes from about 50 to about 90 weight percent of said total mixture and wherein the Mg[A] compound is introduced to the Al[B] compound in the form of a magnesia composition having a pH from about 3.5 to 6.5 and [A] and [B] are nonmetallic atoms which carry a net negative charge when respectively chemically bonded to the magnesia and alumina atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];(2) spray drying the total mixture under such conditions that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the magnesia and the alumina through the liquid medium, (ii) segregation of the magnesia and the alumina into discrete enclaves within a resulting synthetic spinel is precluded and (iii) finely divided, solid, particles are obtained wherein the starting ratio of magnesium atoms to aluminum atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of magnesium oxide (MgO) and aluminum oxide (Al2 O3) having a range of molecular ratios of MgO to Al2 O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the MgO and in the Al2 O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of magnesium and aluminum. - View Dependent Claims (61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72)
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73. A spinel having the general formula R2+ O.R3+ O3, made by a process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a composition of R2+ [A] ("the R2+ [A] composition") having a R2+ [A] compound whose chemical particles are in a size range from molecular size to particles having average diameters not greater than about 5 nanometers, (ii) a composition R3+ [B] ("the R3+ [B] composition") having a R3+ [B] compound whose chemical particles are of a size greater than 5 nanometers, but less than about 60 nanometers, and which have a three dimensional crystalline lattice structure having three axes wherein the crystalline lattice structure having three axes has lattice spacings which are unequal along at least two of the three axes, and which can be broken down into particles having ultimate crystallite sizes of less than about 5 nanometers, and mixed such that the starting ratio of R2+ atoms to R3+ atoms is from about 0.5 to about 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium is capable of breaking down the particles of the R3+ [B] compound to ultimate crystallite sizes of less than 5 nanometers and which constitutes from about 50 to about 90 weight percent of said total mixture and wherein (i) R2+ is a first metallic atom having a first, positive, oxidation state, (ii) R3+ is a second metallic atom having a second, positive, oxidation state higher than the first positive oxidation state of the first metallic atom and (iii) the R2+ [A] compound is introduced to the R3+ [B] compound in the form of a R2+ [A] composition having a pH from about 3.5 to about 6.5 and [A] and [B] are nonmetallic atoms which carry a net negative charge when respectively chemically bonded to the R2+. and R3+ metallic atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic atoms of [A] and [B];(2) spray drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the R2+ [A] compound and the R3+ [B] compound through the liquid medium, (ii) segregation of the R2+ [A] compound and the R3+ [B] compound into discrete enclaves within a resulting synthetic spinel is precluded, (iii) finely divided, solid, particles are obtained, and (iv) wherein the starting ratio of R2+ atoms to atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of R2+ oxide (R2+ O) and R3+ oxide (R23+ O3) having a range of molecular ratios of R2+ O to (R23+ O3) from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the R2+ O and in the R23+ O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of R2+ and R3+. - View Dependent Claims (74, 75, 76, 77, 78, 79, 80, 81)
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82. A spinel having the general formula MgO. Al2 O3, made by a process comprising:
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(1) mixing, to a homogeneous consistency;
(i) a composition of magnesium (Mg[A], "the magnesia") having a Mg[A] compound whose chemical particles are in a size greater than 5 nanometers, but less than about 60 nanometers, and which have a three dimensional crystalline lattice structure having three axes wherein the crystalline lattice structure having three axes has lattice spacings which are unequal along at least two of the three axes, and which can be broken down into particles having ultimate crystallite sizes of less than about 5 nanometers by physicochemical forces applied during a mixing step of said process, (ii) a composition of aluminum (Al[B], "the alumina") having an Al[B] compound whose chemical particles are also in a size greater than 5 nanometers, but less than about 60 nanometers, and which have a three dimensional crystalline lattice structure having three axes wherein the crystalline lattice structure having three axes has lattice spacings which are unequal along at least to of the three axes, and which can be broken down into particles having ultimate crystallite sizes of less than about 5 nanometers, and mixed such that the starting ratio of magnesium atoms to aluminum atoms is substantially from 0.5 to 1.25 and (iii) such amounts of a liquid medium necessary to produce a total mixture having a pH from about 3.5 to about 6.5 and wherein the liquid medium is capable of breaking down the particles of the R2+ [A] compound and the R3+ [B] compound to their respective ultimate crystallite sizes and which constitutes from about 50 to about 90 weight percent of said total mixture and wherein the Mg[A] compound is introduced to the Al[B] compound in the form of a magnesia composition having a pH from about 3.5 to about 6.5 and [A] and [B] are nonmetallic atoms which bear a net negative charge when respectively chemically bonded to the magnesia and alumina atoms and which, when subjected to prolonged heating in the presence of oxygen at elevated temperatures of calcination, will form gaseous oxides of the nonmetallic elements of [A] and [B];(2) spray drying the total mixture under conditions such that;
(i) the liquid medium is flashed to a gaseous state at such a rate as to arrest migration of the magnesia and the alumina through the liquid medium, (ii) segregation of the magnesia and the alumina into discrete enclaves within a resulting synthetic spinel is precluded and (iii) finely divided, solid, particles are obtained wherein the starting ratio of magnesium atoms to aluminum atoms of the total mixture is substantially maintained in said particles; and(3) calcining the finely divided, solid, particles under conditions which produce crystals of a solid solution of magnesium oxide (MgO) and aluminum oxide (Al2 O3) having a range of molecular ratios of MgO to Al2 O3 from about 1.0 to about 2.5 and drive off, as gases, substantially all other elements present in the crystal (i.e., other than those elements contained in the MgO and in the Al2 O3) and thereby producing a synthetic spinel which contains no more than about 5% by weight complex compounds of magnesium and aluminum. - View Dependent Claims (83, 84, 85, 86, 87, 88, 89, 90, 91, 92)
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Specification