E.i. Dupont De Nemours and Company

State of Oregon

Oregon State University

Arthur W Sleight

Munirpallam Appadorai Subramanian

Harold S Horowitz

Jagannatha Gopalakrishnan

Mary A Thundathil

Munirpallam A Subramanian

John S Evans

Stephan James McLain

Michael Brian D'Amore

Joe Douglas Druliner

Rashmikant M Contractor

John C Haygarth

Donald I Garnett

Howard S Jarrett

Harold H Kung

Andrew E Smith

Jun Li

Claire E Closmann

Kameswari Upadhyayula

Jinfan Huang

Novel colored compounds with a hibonite structure and a method for making the same are disclosed. The compounds may have a formula AAlMMOwhere A is typically an alkali metal, an alkaline earth metal, a rare earth metal, Pb, Bi or any combination thereof, and Mis Ni, Fe, Cu, Cr, V, Mn, or Co or any combination thereof, and Mis Ti, Sn, Ge, Si, Zr, Hf, Ga, In, Zn, Mg, Nb, Ta, Sb, Mo, W or Te or any combination thereof. Compounds with varying colors, such as blue, can be made by varying A, Mand Mand their relative amounts. Compositions comprising the compounds and methods for making and using the same are also disclosed.

Compounds comprising a hibonite structure and a method for their use

Embodiments of compositions comprising materials satisfying the general formula AMM'M&#x2033;Oare disclosed, along with methods of making the materials and compositions. In some embodiments, M and M&#x2032; are +3 cations, at least a portion of the M cations and the M&#x2032; cations are bound to oxygen in trigonal bipyramidal coordination, and the material is chromophoric. In some embodiments, the material forms a crystal structure having a hexagonal unit cell wherein edge a has a length of 3.50-3.70 &#x212b; and edge c has a length of 10-13 &#x212b;. In other embodiments, edge a has a length of 5.5-7.0 &#x212b;. In particular embodiments, M&#x2032; is Mn, and Mn is bonded to oxygen with an apical Mn&#x2014;O bond length of 1.80 &#x212b; to 1.95 &#x212b;. In some embodiments, the material is YInMnO, x is greater than 0.0 and less than 0.75, and the material exhibits a surprisingly intense blue color.

Materials with trigonal bipyramidal coordination and methods of making the same

Compositions having the nominal formulaBiSrCaCuO

Superconducting bismuth-strontium-calcium-copper oxide compositions and process for manufacture

A method for making negative thermal expansion materials having the formula

Solution method for making molybdate and tungstate negative thermal expansion materials and compounds made by the method

Low or negative thermal expansion compounds are described having a formula of A.sub.2-x.sup.3+ A.sub.y.sup.4+ M.sub.z.sup.3+ M.sub.3-y.sup.6+ P.sub.y O.sub.12. It currently is believed that y can vary from about 0 to about 2, x equals the sum of y and z and varies from about 0.1 to about 1.9. Without limitation, novel compounds satisfying the formula A.sub.2-x.sup.3+ A.sub.y.sup.4+ M.sub.z.sup.3+ M.sub.3-y.sup.6+ P.sub.y O.sub.12 where y=0 may be selected from the group consisting of Al.sub.1.5 In.sub.0.5 W.sub.3 O.sub.12, Al.sub.1.6 In.sub.0.4 W.sub.3 O.sub.12, Al.sub.1.7 In.sub.0.3 W.sub.3 O.sub.12, Al.sub.1.8 In.sub.0.2 W.sub.3 O.sub.12, YAlW.sub.3 O.sub.12, ScAlW.sub.3 O.sub.12, ScGaW.sub.3 O.sub.12, ScInW.sub.3 O.sub.12, ScHoW.sub.3 O.sub.12, ScYbMo.sub.3 O.sub.12 and ErInW.sub.3 O.sub.12. Without limitation, novel compounds satisfying the formula A.sub.2-x.sup.3+ A.sub.y.sup.4+ M.sub.z.sup.3+ M.sub.3-y.sup.6+ P.sub.y O.sub.12 where y=2 may be selected from the group consisting of Hf.sub.2 WP.sub.2 O.sub.12 and Hf.sub.2 MoP.sub.2 O.sub.12. The present invention also provides compositions useful for decreasing the positive thermal expansion of a material or materials included in the compositions. The compositions comprise at least a first material and a second material where the first material has low or negative thermal expansion properties and the second material exhibits positive thermal expansion. Novel compositions and methods for making and using such compositions can be made using a first material selected, without limitation, from the group consisting of Al.sub.2 W.sub.3 O.sub.12, Al.sub.2 Mo.sub.3 O.sub.12, In.sub.2 W.sub.3 O.sub.12, Al.sub.1.5 In.sub.0.5 W.sub.3 O.sub.12, Al.sub.1.6 In.sub.0.4 W.sub.3 O.sub.12, Al.sub.1.7 In.sub.0.3 W.sub.3 O.sub.12, Al.sub.1.8 In.sub.0.2 W.sub.3 O.sub.12, YAlW.sub.3 O.sub.12, ScAlW.sub.3 O.sub.12, ScGaW.sub.3 O.sub.12, ScInW.sub.3 O.sub.12, ScHoW.sub.3 O.sub.12, ScYbMo.sub.3 O.sub.12, ErInW.sub.3 O.sub.12, Al.sub.1.68 Sc.sub.0.02 In.sub.0.3 W.sub.3 O.sub.12, Zr.sub.2 WP.sub.2 O.sub.12, Zr.sub.2 MoP.sub.2 O.sub.12, Hf.sub.2 WP.sub.2 O.sub.12 and Hf.sub.2 MoP.sub.2 O.sub.12. A general method for making compounds having low or negative thermal expansion, and compositions containing such compounds, also is described. The first step of the method comprises purposefully designing compounds to be low or negative thermal expansion compounds according to rules derived empirically. The second step comprises making those compounds designed according to the rules. Examples of negative thermal expansion materials made by such method include NbO.sub.2 F and TaO.sub.2 F.

Materials with low or negative thermal expansion

An improved process for calcination and activation of a catalyst containing mixed oxides of vanadium and phosphorus (V/P/O) comprising the steps of calcining a hydrated V/P/O or V/P/O- SiO.sub.2 catalyst precursor at a temperature range of 375.degree. to 400.degree. C. for sufficient time to dehydrate said catalyst precursor while simultaneously and continuously controlling the oxygen level such as to maintain the Vox in the range of 3.825 to 4.175; and then activating the dehydrated catalyst precursor by further heating at a range of 340.degree. to 500.degree. C. in the presence of a gaseous atmosphere containing n-butane at a partial pressure not exceeding 0.20 atm while simultaneously and continuously controlling the oxygen level such as to maintain the Vox in the range of 3.95 to 4.15. Such a V/P/O catalyst is useful in the preparation of maleic anhydride from n-butane.

Process for the calcination/activation of V/P/O catalyst

A method for making tungstate compounds according to the formula XW.sub.2 O.sub.8, wherein X is selected from the group consisting of zirconium, hafnium, and combinations thereof, is described. Also described are compositions that include the tungstate compounds, and a method for reducing the positive thermal expansion of a material using such tungstate compounds. Substantially single phase compounds can be made by practicing the method, which method also reduces the synthesis time relative to known methods, and expands the reactants that can be used for the synthesis over the methods reported previously. The tungstate compounds generally can be made by forming a solution, particularly an aqueous solution, comprising a W.sup.6+ compound and a second metal compound wherein the metal is selected from the group consisting of Zr.sup.4+, Hf.sup.4+ and combinations thereof. The solvent is removed from the solution by any known method to leave the solutes as a solid product. The solid product is then heated to a temperature of greater than about 600.degree. C., preferably at least about 1165.degree. C., more preferably from about 1165.degree. C. to about 1250.degree. C., and even more preferably to about 1200.degree. C. The heated product is then cooled to ambient temperature, generally relatively rapidly, to produce substantially single phase tungstate compounds.

Negative thermal expansion materials

Compounds that satisfy the general formula A.sub.1-Y.sup.4+ A.sub.Y.sup.1+ A.sub.Y.sup.3+ V.sub.2-X E.sub.X O.sub.7 exhibit isotropic NTE behavior above a temperature of about 100.degree. C. Y is from about 0.0 to about 0.4, and more preferably is about 0.2. X is from about 0.6 to about 1.4, and is more preferably about 1. Particularly suitable NTE compounds have X about 1 and Y about 0. A.sup.4+ is selected from the group consisting of Hf, Zr, Zr.sub.a M.sub.b, Hf.sub.a M.sub.b and mixtures thereof wherein a plus b equals one and M is selected from the group consisting of Ti, Ce, Th, U, Mo, W, Pb, Sn, Ge and Si. More preferably, A.sup.4+ is selected from the group consisting of Hf and Zr. A.sup.1+ is selected from the group consisting of the alkali earth metals, A.sup.3+ is selected from the group consisting of the rare earth metals, and E is selected from the group consisting of P and As. The NTE materials may be incorporated into compositions such as epoxy and ceramic compositions.

Negative thermal expansion material

Compounds that satisfy the general formula A.sub.1-Y.sup.4+ A.sub.Y.sup.1+ A.sub.Y.sup.3+ V.sub.2-X P.sub.X O.sub.7 exhibit isotropic NTE behavior in the range of normal ambient temperatures. Y is from about 0.0 to about 0.4, and more preferably is about 0.2. X is from about 0.6 to about 1.4, and is more preferably about 1. Particularly suitable NTE compounds have X about 1 and Y about 0. A.sup.4+ is selected from the group consisting of Hf, Zr, Zr.sub.a M.sub.b, Hf.sub.a M.sub.b and mixtures thereof wherein a plus b equals one and M is selected from the group consisting of Ti, Ce, Th, U, Mo, Pt, Pb, Sn, Ge and Si. More preferably, A.sup.4+ is selected from the group consisting of Hf and Zr. A.sup.1+ is selected from the group consisting of the alkali earth metals, and A.sup.3+ is selected from the group consisting of the rare earth metals. Such NTE materials exhibit isotropic negative linear expansion at a temperature below about 100.degree. C. The NTE materials also may be incorporated into compositions such as epoxy and ceramic compositions.

Nonlinear optical materials having the general formula Ca.sub.1.40-X M.sub.X V.sub.0.98.+-.0.05 O.sub.4.00.+-.0.08 wherein X is 0.07 to 0.43 and M is selected from the group consisting of Bi, La, Ce, Y, Pm, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, and mixtures thereof are described. Compositions satisfying this formula belong to the space group R3c wherein a=b=10.8.+-.0.1 .ANG., and c=38.0.+-.0.3 .ANG.. These NLO compositions are capable of doubling the frequency of light at about 0.1 to about 3.3 times the efficiency of KH.sub.2 PO.sub.4 (KDP). No damage to the NLO material is observed when they are exposed to high-power lasers.

Nonlinear optical material

Compositions having the nominal formula Bi.sub.2 Sr.sub.3-x Y.sub.x Cu.sub.2 O.sub.8+y wherein x is from about 0.05 to about 0.45 and y is from about 0 to about 1 are superconducting.

Bi.sub.2 Sr.sub.3-x Y.sub.x Cu.sub.2 O.sub.8+y superconducting metal

A process for preparing the superconductive material MBa.sub.2 Cu.sub.3 O.sub.x, M being, inter alia, yttrium and x being from about 6.5-7 and a precursor material MBa.sub.2 Cu.sub.3 O.sub.y, y being from about 6-6.5, by controlled heating and cooling in a controlled atmosphere.

Process for making superconductors and their precursors

Compositions containing a phase having the formula LA.sub.2-x Na.sub.x CuOz wherein x is about 0.1 to about 0.3 and z is about 3.8 to about 4.2 are superconducting. Processes for manufacturing such compositions and for using them are disclosed.

Lanthanum: sodium copper superconducting metal oxide compositions and

Decomposition of water into hydrogen and oxygen by sunlight is accomplished by using a rhodate p-type semiconductor as cathode and an n-type semiconductor or a metal as anode. A cell exposed to sunlight using a rhodate cathode and an n-type TiO.sub.2 anode decomposes the contained water and also generates electric power.

Photolysis of water using rhodate semiconductive electrodes

Process for regenerating a spent catalyst, which catalyst contains potassium, cobalt, nickel, iron, bismuth, phosphorus and molybdenum and sufficient oxygen to satisfy the valence of the other elements therein, on a support, e.g. silicon oxide, wherein at least a portion of the molybdenum has been lost during ammoxidation, comprising impregnating said catalyst with bismuth and molybdenum in solution so that at least some of the molybdenum lost is replaced, e.g., a typical impregnating solution is prepared by dissolving molybdenum trioxide and phosphoric acid in water, adding nitric acid and finally dissolving bismuth nitrate pentahydrate in the resultant solution.

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Philomath, OR, United States of America

Arthur W Sleight