# US 2014/0151913 A1 · Cost effective y2o3 synthesis and related functional nanocomposites

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- Number: US 2014/0151913 A1
- Document ID: US20140151913A1
- Status: Published application
- Kind: A1
- Application number: 14/070,856
- Filed: 2013-11-04
- Published: 2014-06-05
- Earliest claimed: 2012-11-30
- Assignees: Corning Incorporated
- Applicants: Corning Incorporated
- Inventors: Johnny Glen Arroyo; LinLin Chen; Weiguo Miao
- Web page: https://patentgrep.com/patent/US20140151913A1

## CPC

- C04B 35/505: based on yttrium oxide
- C01F 17/218: Yttrium oxides or hydroxides
- C04B 35/62675: {characterised by the treatment temperature}
- C04B 35/6455: {Hot isostatic pressing}
- C01P 2002/52: containing elements as dopants
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C04B 2235/3205: Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B 2235/3206: Magnesium oxides or oxide-forming salts thereof
- C04B 2235/3208: Calcium oxide or oxide-forming salts thereof, e.g. lime
- C04B 2235/3217: Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B 2235/3224: Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B 2235/3232: Titanium oxides or titanates, e.g. rutile or anatase
- C04B 2235/3244: Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B 2235/3418: Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
- C04B 2235/443: Nitrates or nitrites
- C04B 2235/444: Halide containing anions, e.g. bromide, iodate, chlorite
- C04B 2235/449: Organic acids, e.g. EDTA, citrate, acetate, oxalate
- C04B 2235/5454: nanometer sized, i.e. below 100 nm
- C04B 2235/6584: at an oxygen percentage below that of air
- C04B 2235/661: Multi-step sintering
- C04B 2235/663: Oxidative annealing
- C04B 2235/785: Submicron sized grains, i.e. from 0,1 to 1 micron
- C04B 2235/96: Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B 2235/9653: Translucent or transparent ceramics other than alumina
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

In one aspect the disclosure is directed to a method for inexpensively producing a Y2O3 nano-powder material, thereby facilitating the increased utilization of the material in different commercial application. In another aspect the disclosure is directed to Y2O3 nano-powder composite materials consisting of Y2O3 and at least one oxide selected from the group consisting of MgO, CaO, BeO2, Al2O3, TiO2, ZrO2, SiO2, HfO2, YbO2, GdO2, Lu2O3 and additional rare earth oxides.

## Claims

### Claim 1

A method of making yttrium oxide contain nano-particles, the method comprising:
preparing a solution Y(NO3)3.6H2O placing the solution in a vessel rotatable table;
preparing a solution of ammonia carbonate solution containing ammonia sulfate and 0.2-1.0 wt. % of a water soluble polyethylene glycol as a dispersant;
placing the vessel containing the Y(NO3)3 solution in a 60-80° C. water bath and titrating the Y(NO3)3 solution with the ammonium carbonate solution at the rate of 1-4 ml/min while the vessel containing the Y(NO3)3 solution was rotated at a speed in the range of 100-200 rpm to form a uniform precipitation of the yttrium nano-particles;
spinning the precipitated yttrium nano-particles with sonication for a time in the range of 2-60 minutes after completion of the titration followed by decantation of the liquid and washing the nano-particles with an alcohol/water solution;
collecting and drying the nano-particles in vacuum at a temperature in the range of 15-30° C. to provide dried yttrium oxide nano-particles; and
calcining dried yttrium oxide nano-particles at a temperature in the range of 1050° C. to 1150° C. for a time of at least 2 hours.

### Claim 2 (depends on 1)

The method according to claim 1, wherein during the titration of the Y(NO3)3 solution the pH of the solution was controlled such that the pH of the precipitated material was in the range of 8.5-9.5.

### Claim 3 (depends on 1)

The method according to claim 1, wherein during the titration of the Y(NO3)3 solution the pH of the solution was controlled such that the pH of the precipitated material was in the range of 8.7-9.0.

### Claim 4 (depends on 1)

The method according to claim 1, wherein at least one water soluble metal salt is added to the yttrium nitrate solution prior the beginning of the titration for forming a doped yttrium after calcination.

### Claim 5 (depends on 4)

The method according to claim 4, wherein the at least one water soluble metal salt is a chloride, nitrate or acetate selected from the group of metal consisting of MgO, CaO, BeO2, Al2O3, TiO2, ZrO2, SiO2, HfO2, YbO2, GdO2, Lu2O3 and the remaining rare earth metals.

### Claim 6

A method for forming a yttrium oxide article from yttrium oxide nano-particles, the method comprising:
preparing a solution Y(NO3)3.6H2O placing the solution in a vessel rotatable table;
preparing a solution of ammonia carbonate solution containing ammonia sulfate and 0.2-1.0 wt. % of a water soluble polyethylene glycol as a dispersant;
placing the vessel containing the Y(NO3)3 solution in a 60-80° C. water bath and titrating the Y(NO3)3 solution with the ammonium carbonate solution at the rate of 1-4 ml/min while the vessel containing the Y(NO3)3 solution was rotated at a speed in the range of 100-200 rpm to form a uniform precipitation of the yttrium nano-particles;
spinning the precipitated yttrium nano-particles with sonication for a time in the range of 2-60 minutes after completion of the titration followed by decantation of the liquid and washing the nano-particles with an alcohol/water solution;
collecting and drying the in vacuum at a temperature in the range of 15-30° C. to provide dried yttrium oxide nano-particles;
calcining dried yttrium oxide nano-particles at a temperature in the range of 1050° C. to 1150° C. for a time of at least 2 hours;
placing the calcined nano-particles in a hot isostatic pressing apparatus;
sintering the calcined yttrium oxide nano-particle at a temperature in the range of 1200-1500° C. for a time in the range of 4-10 hours in a 15-20% V/V O2/Ar and a pressure of 1 atmosphere;
and hot isostatic pressing by increasing the pressure to 200 MPa and holding the pressure for an additional time in the range 1 hour to 5 hours; and
cooling to obtain yttrium oxide article.

### Claim 7 (depends on 6)

The method according to claim 6, wherein during the titration of the Y(NO3)3 solution the pH of the solution was controlled such that the pH of the precipitated material was in the range of 8.5-9.5.

### Claim 8 (depends on 6)

The method according to claim 6, wherein during the titration of the Y(NO3)3 solution the pH of the solution was controlled such that the pH of the precipitated material was in the range of 8.7-9.0.

### Claim 9 (depends on 6)

The method according to claim 6, wherein at least one water soluble metal salt is added to the yttrium nitrate solution prior the beginning of the titration for forming a doped yttrium after calcination.

### Claim 10 (depends on 4)

The method according to claim 4, wherein the at least one water soluble metal salt is a chloride, nitrate or acetate selected from the group of metal consisting of MgO, CaO, BeO2, Al2O3, TiO2, ZrO2, SiO2, HfO2, YbO2, GdO2, Lu2O3 and the remaining rare earth metals.

### Claim 11 (depends on 10)

The method according to claim 10, wherein the yttrium oxide article contain the at least one selected metal as a metal oxide.