# US 10,766,784 B2 · Method of manufacturing semiconductor material from mayenite

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 10,766,784 B2
- Document ID: US10766784B2
- Status: Granted
- Kind: B2
- Application number: 16/232,033
- Filed: 2018-12-25
- Published: 2020-02-27
- Granted: 2020-09-08
- Earliest claimed: 2018-08-22
- Assignees: Wuhan University
- Applicants: Wuhan University
- Inventors: Shengwen Tang; Wenzhi Yu; Wei Zhou; Yang Li; Hubao A
- Web page: https://patentgrep.com/patent/US10766784B2

## CPC

- C01F 7/164: Calcium aluminates
- C30B 29/22: Complex oxides
- C30B 13/34: characterised by the seed, e.g. by its crystallographic orientation
- C30B 15/36: characterised by the seed, e.g. its crystallographic orientation
- C30B 23/00: Single-crystal growth by condensing evaporated or sublimed materials
- C30B 29/20: Aluminium oxides
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/02: obtained by optical microscopy
- C01P 2004/03: obtained by SEM
- C01P 2004/80: Particles consisting of a mixture of two or more inorganic phases
- C01P 2006/40: Electric properties
- 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})
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A method of preparation of semiconductor material. The method includes: adding an organic substance containing a benzene ring and dodecacalcium hepta-aluminate (12CaO.7Al2O3 or C12A7) to a test tube, and sealing the test tube; heating the test tube to a temperature of 200-300° C., and holding the temperature for 1 to 3 hours; and continuously heating the test tube to a temperature of 900-1300° C., and holding the temperature for 10-120 hours.

## Claims

### Claim 1

A method, comprising:
(1) adding an organic substance containing a benzene ring and dodecacalcium hepta-aluminate (C12A7) to a test tube, and sealing the test tube;
(2) heating the test tube to a temperature of 200-300° C., and holding the temperature for 1 to 3 hours; and
(3) continuously heating the test tube to a temperature of 900-1300° C., and holding the temperature for 10-120 hours.

### Claim 2 (depends on 1)

The method of claim 1, wherein the dodecacalcium hepta-aluminate is a monocrystalline or polycrystalline material.

### Claim 3 (depends on 2)

The method of claim 2, wherein the polycrystalline material of the dodecacalcium hepta-aluminate is prepared as follows:
weighing calcium nitrate tetrahydrate and aluminum nitrate nonahydrate according to a stoichiometric ratio thereof of 12 to 14; weighing urea which is three times a total stoichiometry of the calcium nitrate tetrahydrate and the aluminum nitrate nonahydrate, mixing and stirring the calcium nitrate tetrahydrate, the aluminum nitrate nonahydrate, and the urea with deionized water, to form a transparent solution;
transferring the transparent solution to a corundum crucible, heating a muffle furnace to 500° C., calcining the corundum crucible in the muffle furnace for 2 hours, and cooling the muffle furnace, to yield polycrystalline C12A7 powders; and
pressing the polycrystalline C12A7 powders into a tablet having a thickness of 0.5-0.8 mm under a pressure of 100-200 megapascal.

### Claim 4 (depends on 2)

The method of claim 2, wherein the monocrystalline material of the dodecacalcium hepta-aluminate is prepared using a floating zone (FZ) method or Czochralski (CZ) method, and the Czochralski (CZ) method comprises:
dissolving a polycrystalline C12A7 in a crystal grower, using platinum wire as a seed crystal and pulling out a crystal, allowing the crystal to grow, and cooling the crystal to room temperature in 30 to 50 hours to obtain a C12A7 monocrystalline block; and
cutting the monocrystalline block into sheets having a thickness of about 0.8 mm.

### Claim 5 (depends on 1)

The method of claim 1, further comprising degreasing and dehydroxylating the dodecacalcium hepta-aluminate prior to (1).

### Claim 6 (depends on 5)

The method of claim 5, wherein degreasing and dehydroxylating the dodecacalcium hepta-aluminate comprises: heating the dodecacalcium hepta-aluminate to a temperature of 1100° C., holding the temperature for 15 hours, and cooling.

### Claim 7 (depends on 1)

The method of claim 1, wherein calcium (Ca) and aluminum (Al) in the dodecacalcium hepta-aluminate is partially substituted by iron (Fe), magnesium (Mg) or rare-earth metal elements; the rare-earth metal elements are selected from europium (Eu), dysprosium (Dy), erbium (Er), holmium (Ho), and ytterbium (Yb), and a substitution ratio is 0 to 5% by mole; and the anion O2− in the dodecacalcium hepta-aluminate is replaced by H−, O−, OH− or halogen ions, and the halogen ions are F− or Cl−.

### Claim 8 (depends on 1)

The method of claim 1, wherein a weight ratio of the organic substance containing a benzene ring to the dodecacalcium hepta-aluminate in the test tube is between 10:1 and 1:50.

### Claim 9 (depends on 1)

The method of claim 1, wherein the test tube is a quartz test tube, a corundum test tube or a ceramic test tube, and the test tube is provided with a stopper.

### Claim 10 (depends on 1)

The method of claim 1, wherein the organic substance containing a benzene ring is chlorobenzene, o-dichlorobenzene, bromobenzene, benzoic acid, phthalic acid, benzaldehyde, benzonitrile, anisole, benzenesulfonic acid, acetophenone, phenylacetamide, methyl benzoate, phenol, styrene, aniline, p-phenylenediamine, or a mixture thereof.

### Claim 11 (depends on 1)

The method of claim 1, wherein a purity of the organic substance containing a benzene ring is not lower than an industrial grade.