Zirconia sol, process of making and composite material
First Claim
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1. A zirconia sol comprising:
- an aqueous phase having dispersed therein a plurality of substantially non-associated single crystal zirconia particles having an average primary particle size about 20 nm or less and a dispersion index ranging from about 1-3, wherein the zirconia particles have a crystallinity index of about 0.65 or greater and about 70% or greater combined cubic and tetragonal crystal lattice structure in the absence of an effective amount of a crystal phase stabilizer.
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Abstract
A zirconia sol comprising an aqueous phase having dispersed therein a plurality of single crystal zirconia particles having an average primary particle size less than about 20 nm. The zirconia sols are substantially non associated having a dispersion index ranging from about 1-3 and are highly crystalline exhibiting a crystallinity index of about 0.65 or greater. Of the crystalline phase, about 70% or greater exists in combined cubic and tetragonal crystal lattice structures without a crystal phase stabilizer. Also described is a hydrothermal method of making zirconia sols having substantially non-associated zirconia particles and composite materials made from the zirconia sols.
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Citations
34 Claims
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1. A zirconia sol comprising:
an aqueous phase having dispersed therein a plurality of substantially non-associated single crystal zirconia particles having an average primary particle size about 20 nm or less and a dispersion index ranging from about 1-3, wherein the zirconia particles have a crystallinity index of about 0.65 or greater and about 70% or greater combined cubic and tetragonal crystal lattice structure in the absence of an effective amount of a crystal phase stabilizer. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17)
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14. The zirconia sol of claim 13, wherein the polyether carboxylic acid is selected from the group consisting of 2-[2-(2-methoxyethoxy)ethoxy] acetic acid and 2-(2-methoxyethoxy) acetic acid.
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15. The zirconia sol of claim 1 further including a polyether carboxylic acid wherein at least a portion of the polyether carboxylic acid is adsorbed onto the zirconia particles.
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16. The zirconia sol of claim 1, wherein the aqueous phase comprises a mixture of water and at least one carboxylic acid.
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17. The zirconia sol of claim 1, wherein the zirconia particles have a cube-like shape.
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18. A process for preparing a zirconia sol comprising the steps of:
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(a) providing an aqueous solution comprising a polyether acid zirconium salt; and
(b) hydrolyzing the aqueous solution of the polyether acid zirconium salt by heating the solution at a temperature and a pressure sufficient to convert the polyether acid zirconium salt into crystalline zirconia particles. - View Dependent Claims (19, 20, 21, 22, 23, 24, 25, 26, 27, 28)
(A) reacting an aqueous solution or sol of a zirconium salt with a polyether carboxylic acid to form an aqueous solution comprising a polyether acid zirconium salt and a free acid; and
(B) optionally, removing at least a portion of the free acid.
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20. The process for preparing a zirconia sol of claim 19, wherein step (B) comprises:
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(1) drying the aqueous solution of the polyether acid zirconium salt; and
(2) dispersing the dried acid polyether acid zirconium salt in water to form an aqueous solution.
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21. The process for preparing a zirconia sol of claim 19, wherein the polyether carboxylic acid has the general formula:
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22. The process for preparing a zirconia sol of claim 19, wherein the polyether carboxylic acid is selected from the group consisting of 2-[2-(2-methoxyethoxy)ethoxy] acetic acid and 2-(2-methoxyethoxy) acetic acid.
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23. The process for preparing a zirconia sol of claim 19, wherein the zirconium salt has the general formula:
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24. The process for preparing a zirconia sol of claim 19, wherein the zirconium salt is zirconium acetate.
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25. The process for preparing a zirconia sol of claim 18, wherein the temperature ranges from about 140-250°
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26. The process for preparing a zirconia sol of claim 18, wherein the pressure ranges from about 1-30 bars.
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27. A zirconia sol prepared according to the process of claim 18.
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28. A zirconia sol prepared according to the process of claim 18, said zirconia sol comprising:
an aqueous phase having dispersed therein a plurality of substantially non-associated single crystal zirconia particles having an average primary particle size about 20 nm or less and a dispersion index ranging from about 1-3, wherein the zirconia particles have a crystallinity index of about 0.65 or greater and about 70% or greater combined cubic and tetragonal crystal lattice structure in the absence of an effective amount of a crystal phase stabilizer.
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29. A composite material comprising:
an organic matrix material having dispersed therein a plurality of single crystal zirconia particles having an average primary particle size less than about 20 nm and having a dispersion index ranging from about 1-3, wherein the zirconia particles have a crystallinity index of about 0.65 or greater and about 70% or greater combined cubic and tetragonal crystal lattice structure in the absence of an effective amount of a crystal phase stabilizer. - View Dependent Claims (30, 31, 32, 33, 34)
Specification