yttrium

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Vapourised yttrium [ca 0.9 g (10 mmol)] was cocondensed with 25 g (100 mmol) of 1,3,5-tri(tertbutyl) benzene at -196° C. over a period of 2 hours. The cocondensate was allowed to warm to room temperature under argon and the solid products extracted from the apparatus with n-hexane (ca 750 cm3). The resultant deep purple solution was filtered through a bed of Celite on a frit and the solvent removed under reduced pressure. Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar and the residue extracted with n-pentane (ca 150 cm3). The resulting solution was again filtered through Celite. Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex. The crystals were collected, washed with n-pentane at -80° C. (2×10 cm3) and dried in vacuo. Yield ca 2.4 g (40% based on yttrium). the solid products extracted from the apparatus with n-hexane (ca 750 cm3) The resultant deep purple solution was filtered through a bed of Celite on a frit the solvent removed under reduced pressure Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar the residue extracted with n-pentane (ca 150 cm3) The resulting solution was again filtered through Celite Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex The crystals were collected washed with n-pentane at -80° C. (2×10 cm3) dried in vacuo

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Vapourised yttrium [ca 0.9 g (10 mmol)] was cocondensed with 25 g (100 mmol) of 1,3,5-tri(tertbutyl) benzene at -196° C. over a period of 2 hours. The cocondensate was allowed to warm to room temperature under argon and the solid products extracted from the apparatus with n-hexane (ca 750 cm3). The resultant deep purple solution was filtered through a bed of Celite on a frit and the solvent removed under reduced pressure. Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar and the residue extracted with n-pentane (ca 150 cm3). The resulting solution was again filtered through Celite. Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex. The crystals were collected, washed with n-pentane at -80° C. (2×10 cm3) and dried in vacuo. Yield ca 2.4 g (40% based on yttrium). the solid products extracted from the apparatus with n-hexane (ca 750 cm3) The resultant deep purple solution was filtered through a bed of Celite on a frit the solvent removed under reduced pressure Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar the residue extracted with n-pentane (ca 150 cm3) The resulting solution was again filtered through Celite Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex The crystals were collected washed with n-pentane at -80° C. (2×10 cm3) dried in vacuo

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Vapourised yttrium [ca 0.9 g (10 mmol)] was cocondensed with 25 g (100 mmol) of 1,3,5-tri(tertbutyl) benzene at -196° C. over a period of 2 hours. The cocondensate was allowed to warm to room temperature under argon and the solid products extracted from the apparatus with n-hexane (ca 750 cm3). The resultant deep purple solution was filtered through a bed of Celite on a frit and the solvent removed under reduced pressure. Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar and the residue extracted with n-pentane (ca 150 cm3). The resulting solution was again filtered through Celite. Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex. The crystals were collected, washed with n-pentane at -80° C. (2×10 cm3) and dried in vacuo. Yield ca 2.4 g (40% based on yttrium). the solid products extracted from the apparatus with n-hexane (ca 750 cm3) The resultant deep purple solution was filtered through a bed of Celite on a frit the solvent removed under reduced pressure Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar the residue extracted with n-pentane (ca 150 cm3) The resulting solution was again filtered through Celite Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex The crystals were collected washed with n-pentane at -80° C. (2×10 cm3) dried in vacuo

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A preferred method for the production of the admixture needed to produce an 8 wt% Y2O3 /ZrO2 spray dried material is described herein. A clear solution of yttrium acetate was prepared by dissolving 247 g of the Y(acetate)3. 3.5 H2O (0.76 mole) in 500 cc (28 mole) of 90° C. distilled water. This solution was added to an equal volume of hot (80° C.) n-propanol. This solution must be kept hot during the synthesis. Using a heated dropping funnel, the yttrium solution was slowly added to 2.66 kg (6.3 mole) of zirconium n-propoxide. An air driven propellor stirrer was used throughout the addition, and the stirring continued for an extra 30 min. The suspension was quite thick and was improved by the addition of one gram of p-hydroxybenzoic acid (0.2 wt% of the ZrO2) in 1.3 l of n-propanol to the zirconium alkoxide prior to the addition of the yttrium solution. This solution must be kept hot during the synthesis was used throughout the addition

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A preferred method for the production of the admixture needed to produce an 8 wt% Y2O3 /ZrO2 spray dried material is described herein. A clear solution of yttrium acetate was prepared by dissolving 247 g of the Y(acetate)3. 3.5 H2O (0.76 mole) in 500 cc (28 mole) of 90° C. distilled water. This solution was added to an equal volume of hot (80° C.) n-propanol. This solution must be kept hot during the synthesis. Using a heated dropping funnel, the yttrium solution was slowly added to 2.66 kg (6.3 mole) of zirconium n-propoxide. An air driven propellor stirrer was used throughout the addition, and the stirring continued for an extra 30 min. The suspension was quite thick and was improved by the addition of one gram of p-hydroxybenzoic acid (0.2 wt% of the ZrO2) in 1.3 l of n-propanol to the zirconium alkoxide prior to the addition of the yttrium solution. This solution must be kept hot during the synthesis was used throughout the addition

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The same procedure described in Example 3 was utilized except that ZnCl2 was substituted for zinc metal but was not milled with the yttrium. The milled yttrium, without zinc metal or zinc chloride, was reacted with a solution of isopropanol (500 cc) and 3 grams of ZnCl2 over a 24 hour period. Work-up of the reaction mixture yielded 41.6 grams (a 70% yield) of yttrium isopropoxide.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The same reaction was done exactly the same way except no zinc was milled with the yttrium. The milled yttrium was reacted with isopropanol in the same way. There was very little evolution of hydrogen and work-up of the reaction solutions gave a yield of less than 10% for yttrium isopropoxide. The same reaction

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A yttrium containing solution was prepared by mixing and reacting yttrium acetate with a stoichiometric excess of 2-ethylhexanoic acid to produce yttrium tri(2-ethylhexanoate) in 2-ethylhexanoic acid. The resulting solution contained 7.01 percent by weight yttrium, based on total weight. by mixing

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Sol-gel libraries were deposited on silicon wafer substrates. Stock solutions of yttrium isopropoxide, aluminum isopropoxide, gadolinium isopropoxide and gallium isopropoxide were prepared in 2-methoxyethanol (0.25 M) refluxing under Argon for 8 hours. To each of the four stock solutions of yttrium, gadolinium, aluminum and gallium in methoxyethanol (0.25 M), 1 equivalent of 2,4-pentandione was added with stirring, followed by the addition of anhydrous ethylene glycol (15% v/v). The yttrium and gadolinium solutions contained Ce(NO)3.6H2O at 1.0 mol % as the dopant source. refluxing under Argon for 8 hours

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The precursor for the NiO gel is nickel nitrate dissolved in ethanol or isopropanol. The precursor for Y2O3 is either yttrium nitrate or yttrium isopropoxide. Yttrium nitrate solution is prepared by dissolving Y2O3 in nitric acid solution. The solution is then evaporated to dryness to prepare yttrium nitrate which is then dissolved in ethanol or isopropanol at a pH of about 3. Alternatively, yttrium sol is prepared by dissolving yttrium isopropoxide in isopropanol. The solution is then evaporated to dryness to prepare yttrium nitrate which

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: The precursor for the NiO gel is nickel nitrate dissolved in ethanol or isopropanol. The precursor for Y2O3 is either yttrium nitrate or yttrium isopropoxide. Yttrium nitrate solution is prepared by dissolving Y2O3 in nitric acid solution. The solution is then evaporated to dryness to prepare yttrium nitrate which is then dissolved in ethanol or isopropanol at a pH of about 3. Alternatively, yttrium sol is prepared by dissolving yttrium isopropoxide in isopropanol. The solution is then evaporated to dryness to prepare yttrium nitrate which

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Vapourised yttrium [ca 0.9 g (10 mmol)] was cocondensed with 25 g (100 mmol) of 1,3,5-tri(tertbutyl) benzene at -196° C. over a period of 2 hours. The cocondensate was allowed to warm to room temperature under argon and the solid products extracted from the apparatus with n-hexane (ca 750 cm3). The resultant deep purple solution was filtered through a bed of Celite on a frit and the solvent removed under reduced pressure. Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar and the residue extracted with n-pentane (ca 150 cm3). The resulting solution was again filtered through Celite. Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex. The crystals were collected, washed with n-pentane at -80° C. (2×10 cm3) and dried in vacuo. Yield ca 2.4 g (40% based on yttrium). the solid products extracted from the apparatus with n-hexane (ca 750 cm3) The resultant deep purple solution was filtered through a bed of Celite on a frit the solvent removed under reduced pressure Excess of the 1,3,5-tri(tertbutyl)benzene was then removed by the sublimation at 60° C./10-4 mbar the residue extracted with n-pentane (ca 150 cm3) The resulting solution was again filtered through Celite Concentration of the resultant solution under reduced pressure and cooling to -30° C. afforded deep purple crystals of the complex The crystals were collected washed with n-pentane at -80° C. (2×10 cm3) dried in vacuo