Method of manufacturing semiconductor material from mayenite

Patent metadata

Field	Value
Publication number	US-10766784-B2
Application number	US-201816232033-A
Country	US
Kind code	B2
Filing date	Dec 25, 2018
Priority date	Aug 22, 2018
Publication date	Sep 8, 2020
Grant date	Sep 8, 2020

Abstract

A method of preparation of semiconductor material. The method includes: adding an organic substance containing a benzene ring and dodecacalcium hepta-aluminate (12CaO.7Al 2 O 3 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.

First claim

What is claimed is:

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.

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

3. 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.

4. 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.

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

6. 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.

7. 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 O 2− in the dodecacalcium hepta-aluminate is replaced by H − , O − , OH − or halogen ions, and the halogen ions are F − or Cl − .

8. 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.

9. 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.

10. 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.

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

Assignees

• Univ Wuhan

Inventors

• Tang Shengwen
• Yu Wenzhi
• Zhou Wei
• Li Yang
• A Hubao

Classifications

• C30B15/00

  Single-crystal growth by pulling from a melt, e.g. Czochralski method (under a protective fluid C30B27/00) · CPC title

• C30B29/20

  Aluminium oxides · CPC title

• C01P2004/80

  Particles consisting of a mixture of two or more inorganic phases · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C30B13/34

  characterised by the seed, e.g. by its crystallographic orientation · CPC title