US4732741A — Method of making beta"-alumina

Claim 1

Independent Claim 315 words

A method of making beta"-alumina which comprises dispersing in a precursor for aluminium oxide a member of the group comprising sodium oxide and its precursors, and dispersing in the precursor of aluminium oxide a spinel stabilizer which is a member of the group comprising spinel-forming oxides and the precursors thereof, to form a mixture, and then heating the mixture to a temperature at which the precursor of aluminium oxide is converted to beta"-alumina, the precursor of aluminium oxide being one which, when calcined in air by itself, has a calcination product which, when subjected to X-ray diffraction is defined herein, displays an X-ray diffraction trace whose peak with the highest intensity in the 2(theta) range of 44°-48° and whose peak with the highest intensity in the 2(theta) range of 63°-69° respectively have maximum intensities and integrated intensities which comply with equations (I) and (II): A/S is greater than 0.03 (I); and B/S is greater than 0.04 (II), in which: ##EQU4## in counts per second/2(theta)° for the calcination product in the 2(theta) range 44°-48°; ##EQU5## in counts per second/2(theta)° for the calcination product in the 2(theta) range 63°-69°; ##EQU6## in counts per second/2(theta)° for the 211 peak in a rutile (TiO 2 ) standard occuring in the 2(theta) range 52°-56°; maximum intensity=the maximum intensity in counts per second above background displayed by the peak with the highest intensity in the 2(theta) range in question; and integrated intensity=the area under the peak, above background, in the 2(theta) range in question, in units of 2(theta)°×counts per second. A, B and S being mean values for at least five samples having a standard deviation of less than 10% and the rutile standard being the intensity standard rutile of the National Bureau of Standards of the United States Department of Commence accorded standard material No. 674 and having a d-spacing of 1.6874 Angstrom units for the 211 peak in question.

Claim 2

Independent Claim 315 words

A method of making beta"-alumina which comprises dispersing in a precursor for aluminium oxide a member of the group comprising sodium oxide and its precursors, and dispersing in the precursor of aluminium oxide a spinel stabilizer which is a member of the group comprising spinel-forming oxides and the precursors thereof, to form a mixture, and then heating the mixture to a temperature at which the precursor of aluminium oxide is converted to beta"-alumina, the precursor of aluminium oxide being one which, when calcined in air by itself, has a calcination product which, when subjected to X-ray diffraction is defined herein, displays an X-ray diffraction trace whose peak with the highest intensity in the 2(theta) range of 44°-48° and whose peak with the highest intensity in the 2(theta) range of 63°-69° respectively have maximum intensities and integrated intensities which comply with equations (I) and (II): A/S is greater than 0.03 (I); and B/S is greater than 0.04 (II), in which: ##EQU4## in counts per second/2(theta)° for the calcination product in the 2(theta) range 44°-48°; ##EQU5## in counts per second/2(theta)° for the calcination product in the 2(theta) range 63°-69°; ##EQU6## in counts per second/2(theta)° for the 211 peak in a rutile (TiO 2 ) standard occuring in the 2(theta) range 52°-56°; maximum intensity=the maximum intensity in counts per second above background displayed by the peak with the highest intensity in the 2(theta) range in question; and integrated intensity=the area under the peak, above background, in the 2(theta) range in question, in units of 2(theta)°×counts per second. A, B and S being mean values for at least five samples having a standard deviation of less than 10% and the rutile standard being the intensity standard rutile of the National Bureau of Standards of the United States Department of Commence accorded standard material No. 674 and having a d-spacing of 1.6874 Angstrom units for the 211 peak in question.

Claim 3

Dependent Claim 78 words

A method as claimed in claim 1, in which the precursor of aluminium oxide is such that said calcination product displays an X-ray diffraction trace whose peaks with the highest intensity in the 2(theta) ranges respectively of 44°-48° and 63°-69° have maximum intensities and integrated intensities which comply respectively with equations (III) andd (IV): A/S is greater than 0.05 (III); and B/S is greater than 0.05 (IV), wherein A, B and S are as defined in claim 1.

Claim 4

Dependent Claim 77 words

A method as claimed in claim 2, in which the precursor of aluminium oxide is such that said calcination product displays an X-ray diffraction trace whose peaks with highest intensities in the 2(theta) ranges respectively of 44°-48° and 63°-69° have maximum intensities and integrated intensities which comply respectively with equations (V) and (VI): A/S is greater than 0.09 (V); and B/S is greater than 0.07 (VI), wherein A, B and S are as defined in claim 1.

Claim 5

Dependent Claim 68 words

A method as claimed in claim 1, in which the precursor of aluminium oxide is hydrated and is a member of the group comprising monohydrates of alumina in accordance with the formula Al 2 O 3 .mH 2 O in which m is from 1.3 and trihydrates of alumina in accordance with the formula Al 2 O 3 .nH 2 in which n is from 3 to 3.5.

Claim 6

Dependent Claim 114 words

A method as claimed in claim 4, in which the precursor of aluminium oxide is a monohydrate of alumina which is a boehmite, the boehmite having an average crystallite size as determined by X-ray line broadening and scanning electron microscopy of at least 100 Angstrom units, an average basal plane spacing as determined by X-ray diffraction of at most 6.8 Angstrom units, a mass loss on heating at 10° C./min from ambient temperature in air to 700° C. of at most 20% by mass, and, when heated at 10° C./min from ambient temperature in air up to 700° C., a maximum rate of mass loss occurring at a temperature of at least 400° C.

Claim 7

Dependent Claim 55 words

A method as claimed in claim 5, in which said average cystallite size is at least 1000 Angstrom units, said basal plane spacing is at most 6.5 Angstrom units, and said mass loss on heating is at most 17%, and said maximum rate of mass loss occurs at a temperature of at least 500° C.

Claim 8

Dependent Claim 17 words

A method as claimed in claim 5 or claim 6, in which the boehmite is hydrothermally prepared.

Claim 9

Dependent Claim 114 words

A method as claimed in claim 4, in which the precursor of aluminium oxide is a trihydrate of alumina and is a bayerite, the bayerite having an average crystallite size as determined by X-ray line broadening and scanning electron microscopy of at least 100 Angstrom units, an average basal plane spacing as determined by X-ray diffraction of at most 4.9 Angstrom units, a mass loss on heating at 10° C./min from ambient temperature in air to 700° C. of at most 40% by mass, and, when heated at 10° C./min from ambient temperature in air up to 700° C., a maximum rate of mass loss occurring at a temperature of at least 240° C.

Claim 10

Dependent Claim 54 words

A method as claimed in claim 8, in which said average crystallite size is at least 500 Angstrom units, said basal plane spacing is at most 4.75 Angstrom units, said mass loss on heating is at most 37%, and said maximum rate of mass loss occurs at a temperature of at least 260° C.

Claim 11

Dependent Claim 25 words

A method as claimed in claim 1, in which the mixture which is heated is formulated to contain, after heating, from 7-10% by mass soda.

Claim 12

Dependent Claim 25 words

A method as claimed in claim 1, in which the spinel stabilizer is a member of the group comprising lithia, magnesia, and the precursors thereof.

Claim 13

Dependent Claim 32 words

A method as claimed in claim 11, in which the mixture which is heated is formulated to contain, after heating, lithia as its spinel stabilizer, in a proportion of 0.05-1.0% by mass.

Claim 14

Dependent Claim 32 words

A method as claimed in claim 11, in which the mixture which is heated is formulated to contain, after heating, magnesia as its spinel stabilizer, in a proportion of 0.25-5% by mass.

Claim 15

Dependent Claim 24 words

A method as claimed in claim 1, in which the soda and spinel stabilizer are dispersed in the precursor of aluminium oxide by milling.

Claim 16

Dependent Claim 38 words

A method as claimed in claim 14, in which the milling is wet milling until 80% by mass of the milled material is less than 55,000 Angstrom units in size, the milled material being spray-dried prior to heating.

Claim 17

Dependent Claim 32 words

A method as claimed in claim 1, in which the precursor aluminium oxide is calcined by heating to a temperature of 250°-1,100° C., prior to mixing with the soda and spinel stabilizer.

Claim 18

Dependent Claim 55 words

A method as claimed in claim 1, in which the heating of the mixture is according to a heating regime whereby the temperature of the mixture is progressively increased to a maximum temperature, and is thereafter cooled according to a cooling regime whereby the temperature of the heated product is progressively cooled to ambient temperature.

Claim 19

Dependent Claim 24 words

A method as claimed in claim 17, in which the maximum temperature is held for a predetermined period, after which said cooling takes place.

Claim 20

Dependent Claim 24 words

A method as claimed in claim 1, in which the heating of the mixture is to a maximum temperature of at least 1,100° C.

Claim 21

Dependent Claim 29 words

A method as claimed in claim 19, in which the heating of the mixture is to a maximum temperature sufficient to form a unitary self-supporting mass from the mixture.

Claim 22

Dependent Claim 27 words

A method as claimed in claim 20, in which said mixture is formed in a green state into an artifact, prior to the heating of the mixture.

Claim 23

Dependent Claim 36 words

A method as claimed in claim 21, in which the mixture in dry powder form and containing less than 10% by mass moisture is formed into the artifact by pressing to a pressure of 5,000-100,000 psi.

Claim 24

Dependent Claim 22 words

A method as claimed in claim 22, in which the pressing is isostatic pressing and is to a pressure of 30,000-60,000 psi.

Claim 25

Dependent Claim 22 words

A method as claimed in claim 20, in which the heating of the mixture is to a maximum temperature of 1,550°-1,700° C.

Claim 26

Dependent Claim 59 words

A method as claimed in claim 20, in which the rate of heating the mixture is between 150° and 250° C./h from a temperature of at least 550° C. up to a temperature not closer than 100° C. to said maximum temperature, and then at a rate of at most 100° C./h until the maximum temperature has been reached.

Claim 27

Dependent Claim 33 words

A method as claimed in claim 25, in which the rate of heating of the mixture from ambient temperature up to said temperature of at least 550° C. is at most 100° C./h.

Claim 28

Dependent Claim 48 words

A method as claimed in claim 20, in which the precursor of aluminium oxide is calcined by heating to a temperature of 250°-1,100° C., prior to mixing with the soda and spinel stabilizer, and in which the average rate of heating of the mixture is above 50° C./min.

Claim 29

Dependent Claim 22 words

A method as claimed in claim 20, in which the average rate of heating is in the range of 100° C./min-200° C./min.

Claim 30

Dependent Claim 16 words

A method as claimed in claim 20, in which the mixture which is heated comprises alpha-alumina.

Claim 31

Dependent Claim 36 words

A method as claimed in claim 29, in which the alpha-alumina is present in a proportion of at most 95% by mass of the mass of precursor of aluminium oxide in the mixture which is heated.

Claim 32

Dependent Claim 37 words

A method as claimed in claim 29, in which the alpha-alumina is present in a proportion of at least 5% by mass of the mass of the precursor of aluminium oxide in the mixture which is heated.

Claim 33

Dependent Claim 37 words

A method as claimed in claim 30, in which the alpha-alumina is present in a proportion of at least 5% by mass of the mass of the precursor of aluminium oxide in the mixture which is heated.

Claim 34

Dependent Claim 16 words

A method as claimed in claim 20, in which the mixture which is heated comprises gibbsite.

Claim 35

Dependent Claim 42 words

A method as claimed in claim 33, in which the gibbsite is present in a proportion of at least 5% by mass and at most 95% by mass of the mass of precursor of aluminium oxide in the mixture which is heated.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1991-03-22	1991-09-21	1992-03-22	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1995-03-22	1995-09-21	1996-03-22	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1999-03-22	1999-09-21	2000-03-22	$7700.00	Window Closed / Lapsed

Method of making beta"-alumina

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