CN111893575A - Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference - Google Patents

Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference Download PDF

Info

Publication number
CN111893575A
CN111893575A CN202010783301.1A CN202010783301A CN111893575A CN 111893575 A CN111893575 A CN 111893575A CN 202010783301 A CN202010783301 A CN 202010783301A CN 111893575 A CN111893575 A CN 111893575A
Authority
CN
China
Prior art keywords
crucible
layer
crystal growth
raw material
material synthesis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010783301.1A
Other languages
Chinese (zh)
Inventor
霍晓青
周传新
刘禹岑
周金杰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CETC 46 Research Institute
Original Assignee
CETC 46 Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CETC 46 Research Institute filed Critical CETC 46 Research Institute
Priority to CN202010783301.1A priority Critical patent/CN111893575A/en
Publication of CN111893575A publication Critical patent/CN111893575A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/12—Single-crystal growth directly from the solid state by pressure treatment during the growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a method for synthesizing arsenic, germanium and cadmium raw materials and growing single crystals by improving crucible pressure difference in a progressive manner. Correspondingly putting raw materials of arsenic, germanium, cadmium or arsenic, germanium and cadmium into a first layer crucible for raw material synthesis or single crystal growth, then putting the first layer crucible into a second layer crucible, calculating the space volume between the first layer crucible and the second layer crucible, calculating according to a formula PV = nRT, and putting a proper mass of a Cd elementary substance between the first layer crucible and the second layer crucible. According to the same method, the second layer of crucible is placed into the third layer of crucible, a proper amount of Cd simple substance is taken and placed, the pressure difference between the crucibles is gradually reduced, and the experimental safety is ensured. Through the design, the pressure of a growth crucible can be relieved in a segmented mode during synthesis of arsenic, germanium and cadmium raw materials or crystal growth, the risk of the experimental process is reduced, and the safety factor is improved. The method can ensure the safety of the operation of the arsenic germanium cadmium raw material synthesis and the single crystal growth.

Description

Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference
Technical Field
The invention relates to a raw material synthesis and single crystal growth method of chalcopyrite semiconductor crystal arsenic germanium cadmium, in particular to a raw material synthesis and single crystal growth method of arsenic germanium cadmium by adopting progressive improvement of crucible pressure difference.
Background
The arsenic germanium cadmium single crystal is a chalcopyrite semiconductor crystal, the nonlinear coefficient of the arsenic germanium cadmium single crystal is the highest in the semiconductor, meanwhile, the arsenic germanium cadmium crystal has a wide light transmission wavelength range and a proper birefringence gradient and is an excellent candidate material for a frequency conversion crystal, but the crystal is subject to the factors of the crystal growth quality and develops very slowly.
Firstly, when the arsenic-germanium-cadmium polycrystal raw material is synthesized, the single-substance elements of Cd, Ge and As are adopted, wherein the elements of Cd and As are toxic and volatile, so that the excessive vapor pressure in a crucible is easily caused during the synthesis of the raw material, and the explosion of a tube is caused to generate danger; secondly, when the single crystal grows, Cd and As in the polycrystalline raw material volatilize, so that the difference of components of each part of the crystal is caused, the steam pressure in a crucible is high during the growth, and the danger of tube explosion is easily caused; and because the difference of the thermal expansion coefficients of the crystal is large, the difference of the thermal expansion coefficients of the a axis and the c axis can reach more than 15 times, so that the crystal is easy to crack when cooled, and the integrity of the grown single crystal is difficult to ensure.
Although various research groups have adopted various methods to grow the cadmium arsenic germanium crystal, the growth of cadmium arsenic germanium single crystal is still immature, and the cadmium arsenic germanium single crystal with large size and good integrity is difficult to grow out with high repetition rate, but the excellent nonlinear performance of the cadmium arsenic germanium single crystal attracts researchers to research the application of the cadmium arsenic germanium single crystal. The arsenic germanium cadmium monocrystal can realize frequency doubling, optical parametric and optical oscillation parametric output laser. Kildal et al use 10.6um laser pumping arsenic germanium cadmium single crystal to achieve frequency doubling output of 5.3um laser. The Vodopyanov subject group realizes optical parametric and optical parametric oscillation by pumping arsenic germanium cadmium single crystal between 2002 and 2003, and respectively realizes output of medium-long wave infrared laser of 6.8-20.1 um and 7 um-16 um.
So far, the relevant reports about the application of the cadmium arsenic germanium single crystal are very limited, and the practical application of the cadmium arsenic germanium crystal is severely limited by the size and the crystallization quality of the cadmium arsenic germanium crystal. Cd and As volatilize during the synthesis of arsenic germanium cadmium raw materials and the growth of single crystals, so that the crucible is easy to crack during the growth of the crystals, and certain danger exists.
Disclosure of Invention
The invention aims to solve the problem of danger caused by cracking of a crucible due to volatilization of Cd and As elements during synthesis of an arsenic-germanium-cadmium polycrystal material and growth of a single crystal, and provides an effective and progressive method for relieving pressure difference between the inside and the outside of the crucible during synthesis of the arsenic-germanium-cadmium raw material and growth of the single crystal.
The method comprises the steps of correspondingly placing arsenic, germanium, cadmium or arsenic-germanium-cadmium raw materials into a first layer crucible for raw material synthesis or single crystal growth, then placing the first layer crucible into a second layer crucible, calculating the space volume between the first layer crucible and the second layer crucible, calculating according to a formula PV = nRT, and placing a proper mass of a Cd simple substance between the first layer crucible and the second layer crucible. According to the same method, the second layer of crucible is placed into the third layer of crucible, a proper amount of Cd simple substance is taken and placed, the pressure difference between the crucibles is gradually reduced, and the experimental safety is ensured.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for synthesizing arsenic germanium cadmium raw materials by improving crucible pressure difference in a progressive mode is characterized by comprising the following steps:
firstly, a quartz crucible is cleaned and dried by deionized water and is taken as a first layer raw material synthesis crucible, and elemental elements of arsenic, germanium and cadmium are put into the first layer raw material synthesis crucible.
Secondly, taking a quartz crucible which is larger than the first layer of raw material synthesis crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the first layer of raw material synthesis crucible, and taking the quartz crucible as a second layer of raw material synthesis crucible; firstly, calculating the void volume V between a first layer of raw material synthesis crucible and a second layer of raw material synthesis crucible; then according to the calculation formula: PV = nRT- - - - - (1) calculating the amount of substance n of Cd required in units: and mol, further calculating the mass of the required Cd in unit: g; in equation (1): p is the pressure of the gas in the gap between the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible, unit: pa; r is gas constant, unit: pa.m3V (mol.k); t is the temperature of the gas, unit: DEG C; the temperature T of the gas is 93 when the raw materials are synthesized0 ℃ to 970 ℃, when the pressure P of the gap gas between the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible is calculated to be equal to 1.0 multiplied by 105Pa～1.7×105When Pa is needed, calculating the mass of the needed Cd according to the formula (1), and putting the Cd between the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible; and vacuumizing and sealing the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible.
Thirdly, taking a quartz crucible which is larger than the second layer of raw material synthesis crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the second layer of raw material synthesis crucible, and taking the quartz crucible as a third layer of raw material synthesis crucible; firstly, calculating the void volume V between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible1(ii) a Then according to the calculation formula: p1V1=n1RT1Calculating the amount of Cd needed, n1The unit: and mol, further calculating the mass of the needed Cd, unit: g; in equation (2): p1The pressure of the gas in the gap between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible is as follows: pa; r is a gas constant, T1Is the temperature of the gas, in units: DEG C; temperature T of gas1Taking 930-970 ℃, and calculating the pressure P of the gap gas between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible1Is equal to 0.3X 105Pa～1.0×105When Pa is needed, the mass of the Cd obtained by calculation is put between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible according to the formula (2); and vacuumizing and sealing the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible.
And fourthly, putting the sealed first layer of raw material synthesis crucible, the sealed second layer of raw material synthesis crucible and the sealed third layer of raw material synthesis crucible into a synthesis furnace for raw material synthesis.
A method for growing arsenic germanium cadmium single crystal by improving crucible pressure difference in a progressive manner is characterized by comprising the following steps:
firstly, a quartz crucible is cleaned and dried by deionized water and is used as a first layer crystal growth crucible, and arsenic germanium cadmium raw material is put into the first layer crystal growth crucible.
Secondly, taking a quartz crucible which is larger than the first layer of crystal growth crucible, cleaning the quartz crucible by deionized water, drying the quartz crucible, sleeving the quartz crucible outside the first layer of crystal growth crucible, and taking the quartz crucible as a second layer of crystal growth crucible; firstly, calculating the void volume V between the first layer of crystal growth crucible and the second layer of crystal growth crucible2(ii) a Then according to the calculation formula: p2V2=n2RT2-calculating the mass n of Cd required2The unit: and mol, further calculating the mass of the needed Cd, unit: g; in equation (3): p2Is the pressure of the gas in the gap between the first layer of crystal growth crucible and the second layer of crystal growth crucible, unit: pa; r is a gas constant, T2Is the temperature of the gas between the first layer crystal growth crucible and the second layer crystal growth crucible, in units of: DEG C; temperature T of gas2Taking 670-780 ℃, and calculating the pressure P of the gap gas between the first layer of crystal growth crucible and the second layer of crystal growth crucible2Is equal to 0.8X 105Pa～1.7×105When Pa is needed, putting the calculated mass of Cd between a first layer of crystal growth crucible and a second layer of crystal growth crucible according to a formula (3); and vacuumizing and sealing the first layer of crystal growth crucible and the second layer of crystal growth crucible.
Thirdly, taking a quartz crucible which is larger than the second layer of crystal growth crucible, cleaning the quartz crucible by deionized water, drying the quartz crucible, and sleeving the quartz crucible outside the second layer of crystal growth crucible to serve as a third layer of crystal growth crucible; firstly, calculating the void volume V between the second layer of crystal growth crucible and the third layer of crystal growth crucible3(ii) a Then according to the calculation formula: p3V3=n3RT3-calculating the mass n of Cd required3The unit: and mol, further calculating the mass of the needed Cd, unit: g; in equation (4): p3Is the pressure of the gas in the gap between the second layer of crystal growth crucible and the third layer of crystal growth crucible, unit: pa; r is a gas constant, T3For the temperature of the gas between the first and second crystal growth cruciblesBit: DEG C; temperature T of gas3Taking 670-780 ℃, and calculating the pressure P of the gap gas between the second layer of crystal growth crucible and the third layer of crystal growth crucible3Is equal to 0.3X 105Pa～0.8×105When Pa is needed, putting the calculated mass of Cd between a second layer crystal growth crucible and a third layer crystal growth crucible according to a formula (4); and vacuumizing and sealing the second layer of crystal growth crucible and the third layer of crystal growth crucible.
And fourthly, putting the sealed first layer of crystal growth crucible, the sealed second layer of crystal growth crucible and the sealed third layer of crystal growth crucible into a single crystal growth furnace for crystal growth.
The invention has the beneficial effects that: through the design, the pressure of a growth crucible can be relieved in a segmented mode during synthesis of arsenic, germanium and cadmium raw materials or crystal growth, the risk of the experimental process is reduced, and the safety factor is improved. The method can ensure the safety of the operation of the arsenic germanium cadmium raw material synthesis and the single crystal growth.
Drawings
FIG. 1 is a schematic view of a crucible assembly for synthesizing arsenic-germanium-cadmium crystal raw materials according to the present invention;
FIG. 2 is a schematic view of the crucible assembly for arsenic germanium cadmium crystal growth of the present invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
example (b):
1. the method for synthesizing the arsenic, germanium and cadmium raw material for gradually improving the internal and external pressure difference of growth is completed according to the following steps:
firstly, a quartz crucible is cleaned and dried by deionized water and is used as a first layer raw material synthesis crucible, and elemental elements of arsenic, germanium and cadmium are put into the first layer raw material synthesis crucible, as shown in figure 1.
And secondly, taking a quartz crucible which is larger than the first layer of raw material synthesis crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the first layer of raw material synthesis crucible, and taking the quartz crucible as a second layer of raw material synthesis crucible, wherein the second layer of raw material synthesis crucible is shown in figure 1. Comparing the volumes of the two crucibles, the volume between the two crucibles can be knownVoid volume, noted V, void volume V is 2.48X 10-3m3. PV = nRT according to the formula (1), where P is the pressure of the gas in the space between the two crucibles, n is the quantity to be calculated and is the quantity of the substance in the space between the two crucibles, R is a gas constant with a value of 8.31 Pa.m3V (mol.K), T is the temperature of the gas. When the raw materials are synthesized, T is 950 ℃, and P is calculated to be equal to 1.2 multiplied by 105The amount n of Cd required at Pa is 2.95X 10-2And (3) mol, combining the molar mass of Cd steam with 112.4g/mol, calculating the mass of the required Cd to be 3.32g, and putting the Cd between the first layer of raw material synthesis and the second layer of crucible. And vacuumizing and sealing the first layer crucible and the second layer crucible.
And thirdly, taking a quartz crucible which is larger than the second layer of raw material synthesis crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the second layer of raw material synthesis crucible, and taking the quartz crucible as a third layer of raw material synthesis crucible as shown in figure 1. Calculating the void volume V between the two crucibles1Is 3.55 multiplied by 10-3m3. According to the formula (2) P1V1=n1RT1In which P is1Is the pressure of the gas in the space between the second and third layer of raw material synthesis crucibles, n1The amount to be calculated is the amount of the gaseous substance in the space between the two crucibles, R is a gas constant with a value of 8.31 Pa.m3/(mol•K)，T1Is the temperature of the gas. Wherein T is1Taking 950 ℃ and calculating P1Equal to 0.5X 105Amount n of Cd substance required at Pa1Is 1.76X 10-2And (3) mol, calculating the mass of the required Cd to be 1.98g by combining the molar mass of the Cd steam to be 112.4g/mol, and putting the Cd between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible. And vacuumizing and sealing the crucibles for synthesizing the second layer of raw materials and the third layer of raw materials.
And fourthly, putting the sealed raw material synthesis crucible into a synthesis furnace for raw material synthesis.
2. The arsenic germanium cadmium single crystal growth method for gradually improving the internal and external pressure difference comprises the following steps:
firstly, a quartz crucible is cleaned and dried by deionized water and is used as a first layer crystal growth crucible, and arsenic germanium cadmium raw material is put into the first layer crystal growth crucible, as shown in figure 2.
And secondly, taking a quartz crucible which is larger than the first layer of crystal growth crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the first layer of crystal growth crucible, and taking the quartz crucible as a second layer of crystal growth crucible, wherein the second layer of crystal growth crucible is shown in figure 2. Comparing the volumes of the two crucibles, the void volume between the two crucibles is known and is denoted V2Void volume V2Is 3.83X 10-4m3. According to the formula (3) P2V2=n2RT2In which P is2Is the pressure of the gas in the space between the two crystal growth crucibles, n2The amount to be calculated is the amount of the gaseous substance in the space between the two crystal growth crucibles, R is a gas constant and has a value of 8.31 Pa.m3/(mol•K)，T2Is the temperature of the gas between the two crystal growth crucibles. T is2Taking 740 ℃, calculating P2Is equal to 1.0 × 105Pa, the amount of Cd needed for the synthesis of the starting material n2Is 4.6X 10-3And (3) mol, combining the molar mass of Cd steam with 112.4g/mol, calculating the mass of the required Cd to be 0.52g, and putting the Cd between the first layer of crystal growth crucible and the second layer of crystal growth crucible. And vacuumizing and sealing the first layer of crystal growth crucible and the second layer of crystal growth crucible.
And thirdly, taking a quartz crucible which is larger than the second layer of crystal growth crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the second layer of crystal growth crucible, and taking the quartz crucible as a third layer of crystal growth crucible as shown in figure 2. Calculating the void volume V between the two crucibles3Void volume V3Is 5.87X 10-4m3. According to the formula (4) P3V3=n3RT3In which P is3Is the pressure of the gas in the space between the second and third crystal growth crucibles, n3The amount to be calculated is the amount of the gaseous substance in the space between the two crystal growth crucibles, R is a gas constant and has a value of 8.31 Pa.m3/(mol•K)，T3Is the temperature of the gas between the two crystal growth crucibles. Wherein T is3Taking 740 ℃, and measuringCalculate P3Equal to 0.5X 105Amount n of Cd substance required at Pa33.5mol, the molar mass of Cd combined with the molar mass of 112.4g/mol, the mass of Cd required was calculated to be 0.40g, and placed between the second and third layer of crystal growth crucibles. And vacuumizing and sealing the second layer crystal growth crucible and the third layer crystal growth crucible.
And fourthly, putting the sealed crystal growth crucible into a single crystal growth furnace for crystal growth.

Claims (2)

1. A method for synthesizing arsenic germanium cadmium raw materials by improving crucible pressure difference in a progressive mode is characterized by comprising the following steps:
step one, cleaning and drying a quartz crucible by using deionized water, taking the quartz crucible as a first layer raw material synthesis crucible, and putting elemental elements of arsenic, germanium and cadmium into the first layer raw material synthesis crucible;
secondly, taking a quartz crucible which is larger than the first layer of raw material synthesis crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the first layer of raw material synthesis crucible, and taking the quartz crucible as a second layer of raw material synthesis crucible; firstly, calculating the void volume V between a first layer of raw material synthesis crucible and a second layer of raw material synthesis crucible; then according to the calculation formula: PV = nRT- - - - - (1) calculating the amount of substance n of Cd required in units: and mol, further calculating the mass of the required Cd in unit: g;
in equation (1): p is the pressure of the gas in the gap between the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible, unit: pa; r is gas constant, unit: pa.m3V (mol.k); t is the temperature of the gas, unit: DEG C;
when the raw materials are synthesized, the temperature T of the gas is 930-970 ℃, and when the pressure P of the gas in the gap between the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible is calculated to be equal to 1.0 multiplied by 105Pa～1.7×105When Pa is needed, calculating the mass of the needed Cd according to the formula (1), and putting the Cd between the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible; vacuumizing and sealing the first layer of raw material synthesis crucible and the second layer of raw material synthesis crucible;
thirdly, taking a quartz crucible which is larger than the second layer of raw material synthesis crucible, cleaning the quartz crucible by using deionized water, drying the quartz crucible, sleeving the quartz crucible outside the second layer of raw material synthesis crucible, and taking the quartz crucible as a third layer of raw material synthesis crucible; firstly, calculating the void volume V between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible1(ii) a Then according to the calculation formula: p1V1=n1RT1Calculating the amount of Cd needed, n1The unit: and mol, further calculating the mass of the needed Cd, unit: g;
in equation (2): p1The pressure of the gas in the gap between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible is as follows: pa; r is a gas constant, T1Is the temperature of the gas, in units: DEG C;
temperature T of gas1Taking 930-970 ℃, and calculating the pressure P of the gap gas between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible1Is equal to 0.3X 105Pa～1.0×105When Pa is needed, the mass of the Cd obtained by calculation is put between the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible according to the formula (2); vacuumizing and sealing the second layer of raw material synthesis crucible and the third layer of raw material synthesis crucible;
and fourthly, putting the sealed first layer of raw material synthesis crucible, the sealed second layer of raw material synthesis crucible and the sealed third layer of raw material synthesis crucible into a synthesis furnace for raw material synthesis.
2. A method for growing arsenic germanium cadmium single crystal by improving crucible pressure difference in a progressive manner is characterized by comprising the following steps:
step one, cleaning and drying a quartz crucible by using deionized water, taking the quartz crucible as a first layer of crystal growth crucible, and putting an arsenic-germanium-cadmium raw material into the first layer of crystal growth crucible;
secondly, taking a quartz crucible which is larger than the first layer of crystal growth crucible, cleaning the quartz crucible by deionized water, drying the quartz crucible, sleeving the quartz crucible outside the first layer of crystal growth crucible, and taking the quartz crucible as a second layer of crystal growth crucible; first, calculate the first layer crystalVoid volume V between the bulk growth crucible and the second layer crystal growth crucible2(ii) a Then according to the calculation formula: p2V2=n2RT2-calculating the mass n of Cd required2The unit: and mol, further calculating the mass of the needed Cd, unit: g;
in equation (3): p2Is the pressure of the gas in the gap between the first layer of crystal growth crucible and the second layer of crystal growth crucible, unit: pa; r is a gas constant, T2Is the temperature of the gas between the first layer crystal growth crucible and the second layer crystal growth crucible, in units of: DEG C;
temperature T of gas2Taking 670-780 ℃, and calculating the pressure P of the gap gas between the first layer of crystal growth crucible and the second layer of crystal growth crucible2Is equal to 0.8X 105Pa～1.7×105When Pa is needed, putting the calculated mass of Cd between a first layer of crystal growth crucible and a second layer of crystal growth crucible according to a formula (3); vacuumizing and sealing the first layer of crystal growth crucible and the second layer of crystal growth crucible;
thirdly, taking a quartz crucible which is larger than the second layer of crystal growth crucible, cleaning the quartz crucible by deionized water, drying the quartz crucible, and sleeving the quartz crucible outside the second layer of crystal growth crucible to serve as a third layer of crystal growth crucible; firstly, calculating the void volume V between the second layer of crystal growth crucible and the third layer of crystal growth crucible3(ii) a Then according to the calculation formula: p3V3=n3RT3-calculating the mass n of Cd required3The unit: and mol, further calculating the mass of the needed Cd, unit: g;
in equation (4): p3Is the pressure of the gas in the gap between the second layer of crystal growth crucible and the third layer of crystal growth crucible, unit: pa; r is a gas constant, T3Is the temperature of the gas between the first layer crystal growth crucible and the second layer crystal growth crucible, in units of: DEG C;
temperature T of gas3Taking 670-780 ℃, and calculating the gas in the gap between the second layer crystal growth crucible and the third layer crystal growth cruciblePressure P of body3Is equal to 0.3X 105Pa～0.8×105When Pa is needed, putting the calculated mass of Cd between a second layer crystal growth crucible and a third layer crystal growth crucible according to a formula (4); vacuumizing and sealing the second layer of crystal growth crucible and the third layer of crystal growth crucible;
and fourthly, putting the sealed first layer of crystal growth crucible, the sealed second layer of crystal growth crucible and the sealed third layer of crystal growth crucible into a single crystal growth furnace for crystal growth.
CN202010783301.1A 2020-08-06 2020-08-06 Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference Pending CN111893575A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010783301.1A CN111893575A (en) 2020-08-06 2020-08-06 Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010783301.1A CN111893575A (en) 2020-08-06 2020-08-06 Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference

Publications (1)

Publication Number Publication Date
CN111893575A true CN111893575A (en) 2020-11-06

Family

ID=73245537

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010783301.1A Pending CN111893575A (en) 2020-08-06 2020-08-06 Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference

Country Status (1)

Country Link
CN (1) CN111893575A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07300385A (en) * 1994-03-11 1995-11-14 Sumitomo Electric Ind Ltd Production of compound semiconductor crystal and crucible therefor
CN102344126A (en) * 2011-06-21 2012-02-08 四川大学 Synthesis method and synthesis container of phosphorus-silicon-cadmium polycrystal
CN202849591U (en) * 2012-09-25 2013-04-03 四川大学 Quartz explosionproof container for single crystal growth
CN104047047A (en) * 2014-06-09 2014-09-17 北京雷生强式科技有限责任公司 Horizontal growth device and growth method of phosphorus silicon cadmium mono-crystal
CN109110810A (en) * 2018-09-29 2019-01-01 中国电子科技集团公司第四十六研究所 A kind of current stabilization synthetic method of arsenic germanium cadmium crystal growth raw material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07300385A (en) * 1994-03-11 1995-11-14 Sumitomo Electric Ind Ltd Production of compound semiconductor crystal and crucible therefor
CN102344126A (en) * 2011-06-21 2012-02-08 四川大学 Synthesis method and synthesis container of phosphorus-silicon-cadmium polycrystal
CN202849591U (en) * 2012-09-25 2013-04-03 四川大学 Quartz explosionproof container for single crystal growth
CN104047047A (en) * 2014-06-09 2014-09-17 北京雷生强式科技有限责任公司 Horizontal growth device and growth method of phosphorus silicon cadmium mono-crystal
CN109110810A (en) * 2018-09-29 2019-01-01 中国电子科技集团公司第四十六研究所 A kind of current stabilization synthetic method of arsenic germanium cadmium crystal growth raw material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李金鹏主编: "《新编普通化学 第2版》", 31 August 2017, 河南医科大学出版社 *

Similar Documents

Publication Publication Date Title
Schunemann et al. Ultralow gradient HGF-grown ZnGeP2 and CdGeAs2 and their optical properties
CN110144624B (en) Synthesis method of selenium-germanium-gallium-barium polycrystal and growth method of selenium-germanium-gallium-barium monocrystal
CN106149046A (en) The polycrystal synthesis method of gallium selenide and method for monocrystal growth
CN103060904A (en) Method for realizing growth of AlN monocrystals by growth mode regulation
CN115010103A (en) Preparation method of purple phosphorus nanobelt material
CN111893575A (en) Arsenic germanium cadmium raw material synthesis and single crystal growth method for progressively improving crucible pressure difference
CN109930203B (en) BaGa4Se7Apparatus and method for synthesizing polycrystal
CN109137080B (en) Method for growing selenium-gallium-barium crystal
CN102296366B (en) Synthetic method of LiGaS2 polycrystalline
CN106978630B (en) Selenium copper silicon barium and selenium copper silicon barium mid and far infrared nonlinear optical crystal and preparation method and purposes
CN101962810B (en) Single crystal LiGa3Te5 as well as preparation method and application thereof
CN1367275A (en) Preparation method of block silicone carbide monocrystal growth
JPH1121197A (en) Seed crystal for crystal growth and fluoride crystal
JP2013047159A (en) Method of producing silicon carbide single crystal, silicon carbide single crystal ingot, and silicon carbide single crystal substrate
JP3659377B2 (en) Method for producing fluoride crystals
CN1477239A (en) Method for growing compound laser crystal
CN113293429B (en) Preparation method of monoclinic phase Ga2S3 single crystal
CN108166063A (en) A kind of selenizing Cd monocrystal method of vapor-phase growing of top seed crystal heat conduction
CN105586638A (en) Preparation method of potassium and lead niobate piezoelectric monocrystal
CN111211041B (en) Method for preparing large-area beta-phase indium selenide single crystal film
Singh et al. Growth and characterization of thallium arsenic selenide crystals for nonlinear optical applications
CN104451859B (en) A kind of method and its device for growing fluoro boron potassjum beryllate crystal
CN115182050B (en) Vapor balance growth BaGa 2 GeSe 6 Method for producing single crystals
JP3724870B2 (en) Pyrolytic boron nitride crucible
CN111197181B (en) Preparation method of high-purity ultrathin silicon carbide substrate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20201106

WD01 Invention patent application deemed withdrawn after publication