CN117448939A - Crystal furnace and crystal growth control method - Google Patents
Crystal furnace and crystal growth control method Download PDFInfo
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- CN117448939A CN117448939A CN202311430391.6A CN202311430391A CN117448939A CN 117448939 A CN117448939 A CN 117448939A CN 202311430391 A CN202311430391 A CN 202311430391A CN 117448939 A CN117448939 A CN 117448939A
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- 239000013078 crystal Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000010453 quartz Substances 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 230000008859 change Effects 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims description 13
- 229910052793 cadmium Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 238000003491 array Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QWUZMTJBRUASOW-UHFFFAOYSA-N cadmium tellanylidenezinc Chemical compound [Zn].[Cd].[Te] QWUZMTJBRUASOW-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
-
- 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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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 provides a crystal furnace and a crystal growth control method, which comprise a quartz container, wherein a growth container is arranged in the quartz container, a heater is arranged around the outer side of the quartz container, a plurality of temperature sensors are uniformly distributed on the inner top of the growth container, and the temperature sensors can move up and down along the growth container. The added temperature gradient of the external heating field in the center and the edge area of the crucible is beneficial to the diffusion of the accumulated phase change latent heat in the center area of the crucible to the edge of the crucible, and the process can also play a role in homogenizing the melt substances; by accurately measuring the temperature at the solid-liquid interface, the temperature at the solid-liquid interface is conveniently controlled, so that the edge of the solid-liquid interface is periodically above Tm, nucleation and crystal growth originating near the crucible-melt interface area are inhibited, and the single crystal rate can be greatly improved.
Description
Technical Field
The invention relates to the technical field of tellurium-zinc-cadmium production, in particular to a crystal furnace and a crystal growth control method.
Background
Cadmium zinc telluride (CdZnTe), hereinafter referred to as CZT, is a compound semiconductor material. At present, the CZT single crystal has two main functions, namely, a tellurium-cadmium-Mercury (MCT) detector (a middle-high-end infrared detector which is mainstream at present) is prepared by serving as a substrate slice, and the CZT single crystal is used as a room-temperature nuclear radiation detector material.
Cadmium telluride (CdTe) is added with a certain amount of zinc element (Zn) and can be regarded as a ternary compound formed by partially replacing Cd with Zn. CdTe as a group II-VI compound has strong bonding ionic property, so that the energy barriers of vacancies, dislocation, twin crystals, stacking faults and the like are relatively low, and defects are easy to generate. During the growth of single crystals, the thermal conductivity is also low and the heat transfer at the solid-liquid interface is very difficult. In the context of the increasing demands for single crystal sizes, the problem of heat transport in the central region of the crystal is more pronounced. Such physical properties cause difficulty in single crystal production.
In the prior art, the CZT single crystal growth adopts the principle of solidifying liquid into solid, namely, growing the CZT crystal in a high-temperature furnace by a melt method, and the principle is that the slow growth of the single crystal is realized by the temperature gradient in the furnace body. The main methods for growing CZT crystals by the melt method are Bridgman method (Bridgman) and vertical gradient solidification method (Vertical Gradient Freeze, VGF) and the like. Due to the physical characteristics of CZT crystals, the existing method for growing the CZT crystals by a melt method has the problems of low single crystal rate and excessively high defect density (concentration); zn element fluctuations are also an important issue for the finished substrate or radiation detection crystal.
Disclosure of Invention
The present invention aims to provide a crystal furnace and a crystal growth control method that overcome or at least partially solve the above problems.
In order to achieve the above purpose, the technical scheme of the invention is specifically realized as follows:
the invention provides a crystal growth control method, which comprises the following steps:
s1, putting seed crystals in a seed crystal area of a crucible, then putting a tellurium-zinc-cadmium polycrystal composite material with the purity of 7N into a pyrolytic boron nitride crucible, then putting the crucible into a closed quartz container, vacuumizing the quartz container, and putting the quartz container into a crystal furnace to start crystal growth;
s2, raising the temperature of the h1 area and the h2 area until the tellurium-zinc-cadmium polycrystal is completely melted, and starting to grow, wherein a solid-liquid interface is arranged at the juncture of the h2 area and the h3 area and is set to be 0 in height;
s3, starting growth by changing temperature field distribution, wherein the temperature gradient is selected to be G=0.3 ℃/mm, the temperature field change rate, namely the cooling rate, is 0.1 ℃/h, the growth rate is 0.3mm/h, after one period, the solid-liquid interface is pushed upwards by 1.7mm, at the moment, the theta=0.8 DEG is started to be adjusted, meanwhile, the temperature field is started to be rotated, and in the subsequent growth, the inclination center is adjusted upwards according to the speed of 0.3mm/h, and meanwhile, the rotation is kept;
s4, after the diameter of the solid-liquid interface reaches a certain degree, starting to monitor the readings of the center temperature T0 and the edge temperature Tedge through a temperature sensor, and calculating the average value T of the pi/2 sector edge of the lowest temperature area, wherein when the average value T is 1.2 ℃ lower than T0, the average value is maintained to be theta=0.8 DEG due to the inclination of the temperature field, namely
θ＝(0.8-(T0-T-1.2))°
When T0-T >1.6 ℃, θ=0.4°
When T0-T <0.8 ℃, θ=1.2°
And S5, continuing to grow until the growth is finished.
As a further aspect of the present invention, in the step S1, the inner diameter of the region h1 of the crucible is 104mm.
As a further aspect of the present invention, in the step S3, the rotation speed of the rotation temperature field is 2 to 5RPM.
As a further aspect of the present invention, in the step S4, the solid-liquid interface diameter reaches a level of half the diameter of the crystal growth vessel or the solid-liquid interface rises from the initial height to a height of 0.5×h2.
The crystal furnace comprises a quartz container, wherein a growth container is arranged in the quartz container, a heater is arranged around the outer side of the quartz container, a plurality of temperature sensors are uniformly distributed on the inner top of the growth container, and the temperature sensors can move up and down along the growth container.
As a further scheme of the invention, a servo motor is arranged below the quartz container, an output shaft on the servo motor is fixedly connected with the bottom end of the heater, and the heater is driven to rotate through the operation of the servo motor.
As a further scheme of the invention, five temperature sensors are arranged, one temperature sensor is arranged at the middle position of the growth container, the other four temperature sensors are arranged around the middle temperature sensor in an annular array, and the included angle between every two adjacent temperature sensors and the middle temperature sensor is 90 degrees.
As a further scheme of the invention, a plurality of temperature sensors are arranged, one temperature sensor is arranged at the middle position of the growth container, the other temperature sensors are arranged around the middle temperature sensor in a plurality of groups of annular arrays, and the included angle between two adjacent temperature sensors in the same array and the middle temperature sensor is 45 degrees.
As a further scheme of the invention, the heater is arranged in an inclined state, and the included angle between the central axis of the heater and the central axis of the growth container is 0.4-1.2 degrees.
As a further scheme of the invention, the top of the growth container is fixedly connected with an electric lifting assembly, a distribution plate is fixedly connected to a telescopic rod at the bottom of the electric lifting assembly, and a plurality of temperature sensors are uniformly fixed on the distribution plate.
The invention provides a crystal furnace and a crystal growth control method, which have the beneficial effects that:
1. the added temperature gradient of the external heating field in the center and the edge area of the crucible is beneficial to the diffusion of the accumulated phase change latent heat in the center area of the crucible to the edge of the crucible, and the process can also play a role in homogenizing the melt substance;
2. by accurately measuring the temperature at the solid-liquid interface, the temperature at the solid-liquid interface is convenient to control, so that the edge of the solid-liquid interface is periodically above Tm, nucleation and crystal growth originating near a crucible-melt interface area are inhibited, the single crystal rate can be greatly improved, and the problem that the yield of CZT single crystal production is low and Zn elements are unevenly distributed in the same growth plane is solved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the method of the present invention.
Fig. 2 is a schematic structural view of the present invention.
Fig. 3 is a schematic diagram illustrating the operation of the structure of the present invention.
FIG. 4 is a schematic diagram of a minimum number of temperature sensors according to the present invention.
FIG. 5 is a schematic diagram of an ideal number configuration of temperature sensors in the present invention.
FIG. 6 is a schematic diagram of the test parameters of the present invention.
Fig. 7 is a schematic view showing the inclination of the heater during the growth process according to the present invention.
In the figure: 1. a heater; 2. a quartz container; 3. a growth vessel; 4. a temperature sensor.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
Referring to fig. 1-7, the crystal growth control method provided by the embodiment of the invention comprises the following steps:
s1, putting seed crystals in a seed crystal area of a crucible, then putting a tellurium-zinc-cadmium polycrystal composite material with the purity of 7N into a pyrolytic boron nitride crucible, wherein the inner diameter of an h1 area of the crucible is 104mm, then putting the crucible into a closed quartz container 2, vacuumizing the quartz container 2, and putting the quartz container into a crystal furnace to start crystal growth;
s2, raising the temperature of the h1 area and the h2 area until the tellurium-zinc-cadmium polycrystal is completely melted, and starting to grow, wherein a solid-liquid interface is arranged at the juncture of the h2 area and the h3 area and is set to be 0 in height;
depending on the growth conditions, a suitable interface melt temperature Tm is chosen. Since the CZT melting point varies with composition, there are different composition designs in practice for adjusting the crystal growth process and various indices of the crystal finished product, and this work is not innovative here, and Tm selection is not limited here, as appropriate values obtained in practice are in order.
S3, starting growth by changing temperature field distribution, wherein the temperature gradient is selected to be G=0.3 ℃/mm, the temperature field change rate, namely the cooling rate is 0.1 ℃/h, the growth rate is 0.3mm/h at the moment, after 5.67 hours, the solid-liquid interface is pushed upwards by 1.7mm, at the moment, the theta=0.8 DEG is started to be adjusted, meanwhile, the temperature field is started to be rotated, the rotation speed is 2-5 RPM, and in the subsequent growth, the inclination center is adjusted upwards according to the speed of 0.3mm/h, and meanwhile, the rotation is kept;
s4, the solid-liquid interface diameter reaches the degree that when the solid-liquid interface reaches half of the diameter of the crystal growth container 3 or the solid-liquid interface rises to the height of 0.5 h2 from the initial height, the temperature sensor 4 starts to monitor the readings of the center temperature T0 and the edge temperature Tedge, due to the inclination of the temperature field, one half of the area is higher than Tm, one half of the area is lower than Tm, the average value T of the pi/2 sector edge of the lowest temperature area is calculated, and when the average value T is 1.2 ℃ lower than T0, the average value T is maintained to be theta=0.8 DEG, namely
θ＝(0.8-(T0-T-1.2))°
When T0-T >1.6 ℃, θ=0.4°
When T0-T <0.8 ℃, θ=1.2°
And S5, continuing to grow until the growth is finished.
Supplementary explanation for the distribution of the temperature sensors 4. The more the temperature sensor 4 is, the more the temperature distribution condition on the solid-liquid interface can be accurately known. Sensors distributed in the middle region, e.g., 0.5r,0.8r, etc., the readings of which can be used to correct the edge temperature. With the intermediate area sensor, a linear temperature profile should be obtained for the readings by linear fitting, and T should be calculated from the fitted profile.
Referring to fig. 2-7, a crystal furnace comprises a quartz container 2, wherein a growth container 3 is arranged in the quartz container 2, a heater 1 is arranged around the outer side of the quartz container 2, a plurality of temperature sensors 4 are uniformly distributed on the top of the growth container 3, and the temperature sensors 4 can move up and down along the growth container 3.
A servo motor is arranged below the quartz container 2, an output shaft on the servo motor is fixedly connected with the bottom end of the heater 3, and the heater 3 is driven to rotate through the operation of the servo motor.
The top of the growth container 3 is fixedly connected with an electric lifting assembly, a distribution plate is fixedly connected to a telescopic rod at the bottom of the electric lifting assembly, a plurality of temperature sensors 4 are uniformly fixed on the distribution plate, and the electric lifting assembly operates to drive the distribution plate and the temperature sensors 4 to move up and down so as to keep the temperature sensors 4 at a position 1.2-1.5 mm above a solid-liquid interface all the time.
The temperature sensors 4 are five, one of the temperature sensors 4 is arranged in the middle of the growth container 3, the other four temperature sensors 4 are arranged around the middle temperature sensor 4 in a ring-shaped array, and the included angle between two adjacent temperature sensors 4 and the middle temperature sensor 4 is 90 degrees.
The temperature sensors 4 are arranged in a plurality, one temperature sensor 4 is arranged at the middle position of the growth container 3, the other temperature sensors 4 are arranged around the middle temperature sensor 4 in a plurality of groups of annular arrays, and the included angle between two adjacent temperature sensors 4 in the same array and the middle position temperature sensor 4 is 45 degrees.
The heater 3 is arranged in an inclined state, and the included angle between the central axis of the heater 3 and the central axis of the growth container 3 is 0.4-1.2 degrees.
The present invention adopts the basic principle of the VGF method, which is to control the output power of the heater 3 to manufacture a temperature gradient during use. The technical principle is shown in figure 2. The temperature sensor 4 is arranged in the crystal growth container 3, the sensor is uniformly distributed on the whole cross section, the measuring object of the sensor is melt temperature distribution of a horizontal plane 1.2-1.5 mm above the solid-liquid interface, and the sensor can move up and down to keep the measuring area at the target area all the time. The number of sensors can be self-containedThe minimum number of rows should be 5, and more sensors can obtain more accurate measurement results. Taking fig. 5 as an example, the circular section of the melt is cut along the axes with 4 radiuses, the included angle between every two adjacent axes is 45 degrees, and the parameters required to be obtained are the temperature T of the central area 0 Edge temperature e.g. T a ，T D Etc., and center region temperature, e.g., T 0-a-0.5r 。
Fig. 3 illustrates the other parameters that the crystal growth vessel 3 is divided into three parts: part h1 is the crystal growth zone where the crystals are the final product; h3 is a seed crystal area, and seed crystals of a determined crystal face are placed; h2 is a shoulder region, and the crystal diameter of the region is gradually increased from r1 which is the same as that of the seed crystal region to r. The temperature monitoring is also required in this area, the temperature distribution of the growth vessel 3 can be monitored by the independent expansion and contraction of thermocouples according to the arrangement mode shown in fig. 3 or fig. 4, the temperature distribution of the growth vessel 3 can also be measured by using only the thermocouple at the center, other thermocouples adopt an external mode, and the measured temperature value of the external thermocouple is different according to the different aspects of vessel materials, crystal furnace design and the like and needs to be calibrated through experiments in advance.
The temperature fields herein are of symmetrical design, i.e. AB and AB are coincident in the initial state. θ is the angle between AB and AB during crystal growth. In the growth process, the whole thermal field needs to be inclined, and the inclination center is the intersection point of the crystallization temperature surface of the isothermal surface of the crystal growth and the solid-liquid interface. In practice, since CZT growth is very slow, the solid-liquid interface location and the location of the temperature field are typically relatively fixed, and no special sensors need to be arranged to confirm the solid-liquid interface location. After the start of growth, the entire temperature is first tilted by θ and then rotated along the axis ab while varying the temperature field according to the conventional VGF method for crystal growth.
The rotating temperature field achieves the following effects:
1. the increased temperature gradient of the external heating field in the center and edge regions of the crucible is beneficial to the diffusion of the accumulated phase change latent heat in the center region of the crucible to the edge of the crucible. The process can also play a role in homogenizing the melt substance;
2. the edge of the solid-liquid interface is periodically above Tm, so that nucleation and crystal growth originating from the vicinity of the crucible-melt interface area are inhibited, and the single crystal rate can be greatly improved.
In many cases, the growth vessel 3 (e.g., pyrolytic boron nitride crucible) is entirely enclosed in the quartz vessel 2, and then crystal growth is performed. No matter how the external sealing is performed, or the technical details of manufacturing element atmosphere adjusting partial pressure and the like, the method for designing and controlling the growth equipment can be suitable, and the non-important details are not described additionally.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and changes may be made to the present application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc. which are within the spirit and principles of the present application are intended to be included within the scope of the claims of the present application.
Claims (8)
1. A crystal growth control method, characterized by comprising the steps of:
s1, putting seed crystals in a seed crystal area of a crucible, then putting a tellurium-zinc-cadmium polycrystal composite material with the purity of 7N into a pyrolytic boron nitride crucible, then putting the crucible into a closed quartz container (2), vacuumizing the quartz container (2), and putting the quartz container into a crystal furnace to start crystal growth;
s2, raising the temperature of the h1 area and the h2 area until the tellurium-zinc-cadmium polycrystal is completely melted, and starting to grow, wherein a solid-liquid interface is arranged at the juncture of the h2 area and the h3 area and is set to be 0 in height;
s3, starting growth by changing temperature field distribution, wherein the temperature gradient is selected to be G=0.3 ℃/mm, the temperature field change rate, namely the cooling rate, is 0.1 ℃/h, the growth rate is 0.3mm/h, after one period, the solid-liquid interface is pushed upwards by 1.7mm, at the moment, the theta=0.8 DEG is started to be adjusted, meanwhile, the temperature field is started to be rotated, and in the subsequent growth, the inclination center is adjusted upwards according to the speed of 0.3mm/h, and meanwhile, the rotation is kept;
s4, after the diameter of the solid-liquid interface reaches a certain degree, starting to monitor the readings of the center temperature T0 and the edge temperature Tedge through a temperature sensor (4), and calculating the average value T of the pi/2 sector edge of the lowest temperature area, wherein the average value T is 1.2 ℃ lower than the T0, and the angle of theta=0.8 DEG is maintained when the average value T is 1.2 DEG, namely
θ＝(0.8-(T0-T-1.2))°
When T0-T >1.6 ℃, θ=0.4°
When T0-T <0.8 ℃, θ=1.2°
And S5, continuing to grow until the growth is finished.
2. The method according to claim 1, wherein in the step S1, the inner diameter of the region h1 of the crucible is 104mm.
3. The crystal growth control method according to claim 1, wherein in the step S3, the rotational speed of the rotational temperature field is 2 to 5RPM.
4. A crystal growth control method according to claim 1, characterized in that in step S4 the solid-liquid interface diameter is reached to such an extent that half the diameter of the crystal growth vessel (3) is reached or the solid-liquid interface rises from an initial height to a height of 0.5 x h 2.
5. The utility model provides a crystal furnace, its characterized in that includes quartz container (2), quartz container (2) inside is provided with growth container (3), and is provided with heater (1) around the outside of quartz container (2), the top evenly distributed has a plurality of temperature sensor (4) in growth container (3), and temperature sensor (4) can reciprocate along growth container (3).
6. A crystal furnace according to claim 5, characterized in that the temperature sensors (4) are provided in five, one of the temperature sensors (4) is provided in the middle position of the growth vessel (3), the other four temperature sensors (4) are provided in an annular array around the middle temperature sensor (4), and the angle between two adjacent temperature sensors (4) and the middle position temperature sensor (4) is 90 °.
7. A crystal furnace according to claim 5, characterized in that the temperature sensors (4) are provided in plural, one of the temperature sensors (4) is provided at the middle position of the growth vessel (3), the other plurality of temperature sensors (4) are provided in plural sets of annular arrays around the middle temperature sensor (4), and the angle between two adjacent temperature sensors (4) of the same array to the middle position temperature sensor (4) is 45 °.
8. The crystal growing furnace according to claim 5, wherein the heater (3) is arranged in an inclined state, and an included angle between a central axis of the heater (3) and a central axis of the growth container (3) is 0.4 ° to 1.2 °.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311430391.6A CN117448939A (en) | 2023-10-31 | 2023-10-31 | Crystal furnace and crystal growth control method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311430391.6A CN117448939A (en) | 2023-10-31 | 2023-10-31 | Crystal furnace and crystal growth control method |
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| Publication Number | Publication Date |
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| CN117448939A true CN117448939A (en) | 2024-01-26 |
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| CN202311430391.6A Pending CN117448939A (en) | 2023-10-31 | 2023-10-31 | Crystal furnace and crystal growth control method |
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| Country | Link |
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- 2023-10-31 CN CN202311430391.6A patent/CN117448939A/en active Pending
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