Growth method and apparatus for preparing high-yield crystals

Patent metadata

Field	Value
Publication number	US-11242615-B2
Application number	US-201916627934-A
Country	US
Kind code	B2
Filing date	Apr 18, 2019
Priority date	Dec 14, 2018
Publication date	Feb 8, 2022
Grant date	Feb 8, 2022

Abstract

The invention provides a growth method for preparing high-yield crystals, belongs to the technical field of single crystal growth. Auxiliary crucibles are arranged on a crucible according to different crystal types and according to the crystal orientation of crystal growth in the main crucible, the relationship between the crystal growth direction and twin crystal orientation. By controlling the angle between the auxiliary crucibles and the main crucible, the relative position between the auxiliary crucibles each other, the auxiliary crucibles realize correction on the crystal orientation of twins generated in the main crucible crystal growth process. The growth method for preparing the high-yield crystals provided by the invention has the following advantages: the crystal orientation change caused by twins is corrected through auxiliary crucibles additionally arranged on the main crucible, and the overall yield is improved for the growth process of the dislocation crystal with large probability; the crucible position can be customized according to the influence of twins on the crystal growth direction, suitable for various crystal preparation processes, improving the yield obviously, reducing the crystal processing difficulty, and improving the material utilization rate.

First claim

The invention claimed is:

1. A growth method for preparing high-yield crystals by using a crystal growth crucible and a mated heating furnace, characterized in that, the crystal growth crucible, in a structure, comprises a main crucible sequentially provided with a seed crystal portion, a growth portion, a necking portion and a feeding growth portion from bottom to top, and auxiliary crucibles dispersed on the necking portion of the main crucible; the method sequentially comprises steps of feeding materials, vacuumizing, melting materials in the main crucible, melting materials in the auxiliary crucibles, cooling the main crucible, cooling the auxiliary crucibles successively and disassembling the furnace to remove a crystal ingot; the step of feeding materials comprises putting a seed crystal into the seed crystal portion according to a crystal plane index (h 1 k 1 l 1 ) perpendicular to a crystal growth direction; feeding a polycrystalline crushed material into the growth portion, the feeding growth portion of the main crucible and the auxiliary crucible respectively, and then feeding a sealant; and controlling an included angle between center lines of auxiliary crucible and the main crucible to be θ, and an included angle between center lines of the auxiliary crucibles to be ϕ or a multiple of ϕ, with θ and ϕ being satisfied
cos ϑ=|( h 1 h 2 +k 1 k 2 +l 1 l 2 )|/[( h 1 2 +l 1 2 +k 1 2 )( h 2 2 +l 2 2 +k 2 2 )] 0.5 ,

cos φ=|( h 3 h 4 +k 3 k 4 +l 3 l 4 )|/[( h 3 2 +l 3 2 +k 3 2 )( h 4 2 +l 4 2 +k 4 2 )] 0.5

wherein, (h 1 k 1 l 1 ) is the crystal plane index perpendicular to the crystal growth direction; after twins are generated, the crystal plane perpendicular to the crystal ingot along the crystal growth direction is converted into (h 2 k 2 l 2 ); (h 3 k 3 l 3 ) and (h 4 k 4 l 4 ) are crystal plane indices perpendicular to the crystal growth crystal plane and passing through twin lines on adjacent crystal growth crystal planes.

2. The method of claim 1 , characterized in that, the auxiliary crucible, in a structure, comprises, a connection portion connected to the necking portion of the main crucible, a branch growth portion and a balance tube sequentially from bottom to top, and a top end of the balance tube is higher than the necking portion of the crystal growth crucible.

3. The method of claim 1 , characterized in that the steps are specifically as follows:
{circle around (1)} feeding materials: putting the seed crystal into the seed crystal portion according to the crystal plane index (h 1 k 1 l 1 ) perpendicular to the crystal growth direction, putting the polycrystalline crushed material into growth portion, the feeding growth portion of the main crucible and the auxiliary crucible, respectively, and then putting the sealant;
{circle around (2)} vacuumizing: vacuumizing a furnace body, and filling inert gas to 1.8-2.5 MPa;
{circle around (3)} melting materials in the main crucible: allowing, by means of a heating assembly and thermometric couples of the main crucible, the main crucible to form a temperature gradient sequentially increased from bottom to top, and controlling the temperature at the seed crystal portion to be lower than a melting point of the crystal to enable the polycrystalline material in the main crucible to melt;
{circle around (4)} melting materials in the auxiliary crucibles: controlling, by means of heating assemblies and thermometric couples mated for each auxiliary crucible, the temperature of each auxiliary crucible to rise from bottom to top sequentially, thereby forming a temperature gradient in each auxiliary crucible from bottom to top to melt polycrystalline materials in the auxiliary crucibles;
{circle around (5)} cooling the main crucible: controlling, by means of the heating assembly and the thermometric couples of the main crucible, the main crucible to form a temperature gradient sequentially reduced from bottom to top, and controlling the temperature at the seed crystal portion to be lower than the melting point of the crystal;
{circle around (6)} cooling the auxiliary crucibles sequentially: controlling each auxiliary crucible to cool from bottom to top sequentially, and controlling the auxiliary crucible to form a temperature gradient reduced from bottom to top sequentially when a temperature at a joint of auxiliary crucible and the main crucible is lower than the melting point of the crystal, and allowing the melting point isotherms of the crystals in auxiliary crucibles same as that in the main crucible; and
{circle around (7)} controlling the heating assembly to slowly cool the main crucible and the auxiliary crucible to room temperature when the temperature at the balance tube of each auxiliary crucible is lower than the melting point of the crystal, and disassembling the furnace to remove the crystal ingot.

4. A high-yield crystal growth crucible comprising a main crucible, characterized in that, the main crucible, in a structure, comprises a main crucible seed crystal portion and a main crucible growth portion from bottom to top sequentially, and auxiliary crucibles are arranged on the main crucible along a circumferential direction; and
further characterized in that, an included angle between center lines of auxiliary crucible and the main crucible is θ, cos ϑ=|(h 1 h 2 +k 1 k 2 +l 1 l 2 )|/[(h 1 2 +l 1 2 +k 1 2 )(h 2 2 +l 2 2 +k 2 2 )] 0.5 , wherein h 1 k 1 l 1 h 2 k 2 l 2 are crystal plane indices, a crystal plane perpendicular to a crystal growth direction is (h 1 k 1 l 1 ); and the crystal plane perpendicular to the ingot in the direction of crystal growth is converted to (h 2 k 2 l 2 ) after twins are generated.

5. The crystal growth crucible of claim 4 , characterized in that, the main crucible comprises a seed crystal portion, a growth portion, a necking portion and a feeding growth portion successively from bottom to top, and the auxiliary crucible is provided at the necking portion of the main crucible; and the auxiliary crucible, in a structure, comprises a connection portion connected with the necking portion of the main crucible, a branch growth portion and a balance tube from bottom to top sequentially, wherein a top end of the balance tube is higher than the necking portion of the main crucible.

6. The crystal growth crucible of claim 4 , wherein and an included angle between center lines of the auxiliary crucibles to be ϕ or a multiple of ϕ, cos φ=|(h 3 h 4 +k 3 k 4 +l 3 l 4 )|/[(h 3 2 +l 3 2 +k 3 2 ) (h 4 2 +l 4 2 +k 4 2 )] 0.5 , wherein (h 3 k 3 l 3 ) and (h 4 k 4 l 4 ) are crystal plane indices perpendicular to the crystal growth crystal plane and passing through twin lines on adjacent crystal growth crystal planes.

7. A growth method for preparing a high-yield InP crystal, characterized by comprising the following steps:
{circle around (1)} feeding materials: putting the seed crystal into the seed crystal portion according to the crystal plane index (h 1 k 1 l 1 ) perpendicular to the crystal growth direction, putting the polycrystalline crushed material into growth portion, the feeding growth portion of the main crucible and the auxiliary crucible, respectively, and then putting the sealant;
{circle around (2)} vacuumizing: vacuumizing a furnace body, and filling inert gas to 1.8-2.5 MPa;
{circle around (3)} melting materials in the main crucible: allowing, by means of a heating assembly and thermometric couples of the main crucible, the main crucible to form a temperature gradient sequentially increased from bottom to top, and controlling the temperature at the seed crystal portion to be lower than 1060-1065° C. to enable the polycrystalline m

Assignees

• The 13Th Research Institute Of China Electronics Tech Group Corporation

Inventors

• Sun Niefeng
• Wang Shujie
• Sun Tongnian
• Liu Huisheng
• Shao Huimin
• Shi Yanlei

Classifications

• C30B11/006

  Controlling or regulating · CPC title

• C30B11/14

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

• C30B11/003

  Heating or cooling of the melt or the crystallised material · CPC title

• C30B15/002

  Continuous growth · CPC title

• C30B29/40

  AIIIBV compounds {wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi} · CPC title