Disclosure of Invention
The invention aims to provide a method and a device for growing a cadmium zinc telluride single crystal, which overcome the problems or at least partially solve the problems so as to solve the problems of low growth efficiency and low yield of the existing cadmium zinc telluride melt crystal.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a method for growing a cadmium zinc telluride single crystal, which comprises the following preparation steps:
putting the tellurium-zinc-cadmium melt into a crucible, and putting the crucible into a high-temperature region of a growth furnace;
the cold pole rod penetrates through the hot pole tube, and the hot pole tube and the bottom of the cold pole rod extend into the crucible;
the hot pole tube is electrically connected with an external heat source, the cold pole rod is electrically connected with an external cold source, the temperature of the central area of the growth interface is in a relatively low level through the cold pole rod, new crystals caused by the relatively low temperature of the cold pole rod in the melt are avoided through the hot pole tube, the growth interface is ensured to grow from the center, and the generation of nucleation on the outer wall is reduced;
the temperature of one side of a melt at a growth interface is slightly lower than the central point by the relative displacement generated between the hot electrode tube and the cold electrode rod and the crucible, so that the growth can be ensured to expand from the center to the periphery, and meanwhile, the hot electrode tube keeps the area outside the central point higher than the central point, so that the nucleation at other places is avoided to generate polycrystal;
and after the crystallization is finished, taking the crucible out of the growth furnace, and taking out the tellurium-zinc-cadmium single crystal.
The utility model provides a growth device of tellurium zinc cadmium monocrystal, includes the crucible, the crucible is inside to be provided with keeps the invariable heat polar tube of temperature to tellurium zinc cadmium melt body, it has on the cold pole stick that carries out central cooling to tellurium zinc cadmium melt body to run through on the heat polar tube.
As a further scheme of the invention, the top end of the thermode tube is electrically connected with a heat source device, the heat source device is electrically connected with the PWM controller through a lead, one end of the PWM controller is electrically connected with a temperature sensor, and the temperature sensor is arranged on the thermode tube so as to conveniently control the temperature of the tip end of the thermode tube.
As a further aspect of the present invention, the heat source device is one of a growth furnace and a separate heater.
As a further scheme of the invention, the top end of the cold pole rod is electrically connected with a cold source device, and the cold source device is electrically connected with the PWM controller through a lead, so that the temperature of the tip end of the cold pole rod can be conveniently controlled.
As a further scheme of the invention, the temperature of the tip of the cold electrode rod is 3 ℃ lower than that of the tip of the hot electrode tube, and the cold source device is an independent heater, so that the temperature difference is prevented from being increased, and the crystallization stability of the melt is improved.
As a further scheme of the invention, the bottom surface of the hot electrode tube is higher than the bottom surface of the cold electrode rod, the distance between the bottom surface of the hot electrode tube and the bottom surface of the cold electrode rod is 1-1.5mm, and the distance between the bottom surface of the cold electrode rod and the inner bottom end of the crucible is 1mm, so that the central area of the melt is cooled, the temperature stability of the surrounding area is ensured, and new crystallization is avoided.
As a further scheme of the invention, more than two temperature measuring points are arranged on the periphery of the crucible and are uniformly distributed in the height direction of the periphery of the crucible, the lower limit of the number of the temperature measuring points is one point corresponding to each 10mm of melt, and the characteristic temperature of a growth interface is calculated by using the temperature measuring point data and is used for growth control.
As a further proposal of the invention, the diameter of the cold pole rod is 6mm, which is convenient for the central cooling and crystallization of the tellurium-zinc-cadmium melt in the central area.
The invention provides a method and a device for growing a cadmium zinc telluride single crystal, which have the beneficial effects that: the hot electrode tube and the cold electrode rod are arranged, so that the artificial intervention on the temperature of the growth interface and the melt side is realized, the condition that the central point is slightly lower is formed, the growth can be ensured to expand from the center to the periphery, meanwhile, the hot electrode tube is used for keeping the area outside the central point to be higher than the central point, the formation of nuclei at other places is avoided, and the growth efficiency and the yield of the tellurium-zinc-cadmium crystal are improved.
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.
Example 1
Referring to fig. 1 to 5, a method for growing a cadmium zinc telluride single crystal according to an embodiment of the present invention includes the following steps:
placing a tellurium-zinc-cadmium melt 5 into a crucible 3, placing the crucible 3 into a high-temperature region of a growth furnace 1, and selecting the growth furnace 1 suitable for a vertical gradient solidification method;
the cold pole rod 4 penetrates through the hot pole tube 2, and the bottom of the hot pole tube 2 and the bottom of the cold pole rod 4 extend into the crucible 3;
the hot pole tube 2 is electrically connected with an external independent heater, the cold pole rod 4 is electrically connected with the external independent heater, the temperature of the central area of the growth interface 7 is in a relatively low level through the cold pole rod 4, the relatively low temperature of the cold pole rod 4 is prevented from initiating new crystallization in the melt 5 through the hot pole tube 2, the growth interface 7 is ensured to start to grow from the center, and the generation of nucleation on the outer wall is reduced;
in a growth furnace 1 suitable for a vertical gradient solidification method, a hot electrode tube 2 and a cold electrode rod 4 are connected with an external pulling machine, the hot electrode tube 2 and the cold electrode rod 4 are driven to move by the external pulling machine, so that relative displacement is generated between the hot electrode tube 2 and the cold electrode rod 4 and a crucible 3, artificial intervention on the temperature of the side of a growth interface 7 and a melt 5 is realized, the condition that the central point is slightly lower is formed, growth can be ensured to expand from the center to the periphery, meanwhile, the hot electrode tube 2 is used for keeping the area except the central point higher than the central point, and the phenomenon that nucleation at other places generates polycrystal is avoided;
after the crystallization is completed, the crucible 3 is taken out from the growth furnace 1, and the tellurium-zinc-cadmium single crystal 6 is taken out.
Example 2
Referring to fig. 1 to 5, a method for growing a cadmium zinc telluride single crystal according to an embodiment of the present invention includes the following steps:
placing the tellurium-zinc-cadmium melt 5 into a crucible 3, placing the crucible 3 into a high-temperature region of a growth furnace 1, and selecting the growth furnace 1 suitable for the Bridgman method;
the cold pole rod 4 penetrates through the hot pole tube 2, and the bottom of the hot pole tube 2 and the bottom of the cold pole rod 4 extend into the crucible 3;
the hot pole tube 2 is electrically connected with the inner wall of the high-temperature region of the growth furnace 1, the cold pole rod 4 is electrically connected with an external independent heater, the temperature of the central region of the growth interface 7 is in a relatively low level through the cold pole rod 4, the relatively low temperature of the cold pole rod 4 is prevented from initiating new crystals in the melt 5 through the hot pole tube 2, the growth interface 7 is ensured to grow from the center, and the generation of nucleation on the outer wall is reduced;
in a growth furnace 1 suitable for a Bridgman method, the positions of a hot electrode tube 2 and a cold electrode rod 4 are kept fixed, and a crucible 3 is driven to move downwards through the self function of the growth furnace 1, so that the relative displacement between the hot electrode tube 2 and the cold electrode rod 4 and the crucible 3 is realized, the artificial intervention on the temperature of the growth interface 7 and the melt 5 side is realized, the condition that the central point is slightly lower is formed, the growth can be ensured to expand from the center to the periphery, meanwhile, the hot electrode tube 2 is used for keeping the area outside the central point higher than the central point, and the phenomenon that nucleation at other places generates polycrystal is avoided;
after the crystallization is completed, the crucible 3 is taken out from the growth furnace 1, and the tellurium-zinc-cadmium single crystal 6 is taken out.
Comparative example 1
Referring to fig. 2, the method for growing a cadmium zinc telluride single crystal according to an embodiment of the present invention includes the following steps:
placing a tellurium-zinc-cadmium melt 5 into a crucible 3, placing the crucible 3 with the tellurium-zinc-cadmium melt 5 into a growth furnace 1 suitable for a vertical gradient solidification method, and placing the crucible 3 into a high-temperature region of the growth furnace 1;
the tellurium-zinc-cadmium melt 5 is crystallized into crystal ingots from bottom to top under the condition of temperature change in a high-temperature interval;
after the crystallization is completed, the crucible 3 is taken out from the growth furnace 1, and the tellurium-zinc-cadmium single crystal 6 is taken out.
Comparative example 2
Referring to fig. 2, the method for growing a cadmium zinc telluride single crystal according to an embodiment of the present invention includes the following steps:
placing a tellurium-zinc-cadmium melt 5 into a crucible 3, placing the crucible 3 with the tellurium-zinc-cadmium melt 5 into a growth furnace 1 suitable for the Bridgman method, and placing the crucible 3 into a high-temperature region of the growth furnace 1;
the tellurium-zinc-cadmium melt 5 is crystallized into crystal ingots from bottom to top under the condition of temperature change in a high-temperature interval;
after the crystallization is completed, the crucible 3 is taken out from the growth furnace 1, and the tellurium-zinc-cadmium single crystal 6 is taken out.
4 inch crucible 3 (phi 108mm, h 200mm)
|
Crystallization Rate (mm/h)
|
Yield (%)
|
Example 1
|
0.6
|
76
|
Example 2
|
1.6
|
79
|
Comparative example 1
|
0.4
|
70
|
Comparative example 2
|
1.2
|
65 |
6 inch crucible 3 (phi 151mm, h 250mm)
|
Crystallization Rate (mm/h)
|
Yield (%)
|
Example 1
|
0.5
|
67
|
Example 2
|
1.1
|
58
|
Comparative example 1
|
0.3
|
60
|
Comparative example 2
|
0.8
|
50 |
As shown in fig. 1, 6 and 7, the top end of the thermode tube 2 is electrically connected to a heat source device, and the heat source device is electrically connected to a PWM controller through a wire, one end of the PWM controller is electrically connected to a temperature sensor, and the temperature sensor is disposed on the thermode tube 2.
The heat source equipment is one of the growth furnace 1 and a separate heater.
The top end of the cold pole rod 4 is electrically connected with cold source equipment, and the cold source equipment is electrically connected with the PWM controller through a lead.
The temperature of the tip of the cold pole rod 4 is 3 ℃ lower than that of the tip of the hot pole tube 2, and the cold source device is an independent heater.
The bottom surface of the hot electrode tube 2 is higher than the bottom surface of the cold electrode rod 4, the distance between the bottom surface of the hot electrode tube 2 and the bottom surface of the cold electrode rod 4 is 1-1.5mm, and the distance between the bottom surface of the cold electrode rod 4 and the bottom end of the crucible 3 is 1 mm.
In the using process of the invention, the temperature of the hot pole tube 2 is convenient to detect through the temperature sensor, and the temperatures of the hot pole tube 2 and the cold pole rod 4 are convenient to control through the PWM controller, so that the temperature difference between the hot pole tube 2 and the cold pole rod 4 is controlled to be 3 ℃.
As shown in figure 2, more than two temperature measuring points 8 are arranged on the periphery of the crucible 3, the more than two temperature measuring points 8 are uniformly distributed in the height direction of the periphery of the crucible 3, the lower limit of the number of the temperature measuring points 8 is one point corresponding to each 10 mm-height melt, and the characteristic temperature of a growth interface is calculated by using the temperature measuring point data and used for growth control.
Setting the distance from the central point of the crucible 3 to the temperature measuring point as r, wherein the distance is a fixed value, and all the temperature measuring points 8 are equidistant from the center of the crucible 3, and the unit is mm;
setting the temperature of a temperature measuring point 8 corresponding to a growth interface 7 as t, taking a plane where the growth interface 7 is located, respectively finding the nearest temperature measuring point 8 values above and below the plane, and using the distance between the temperature measuring point 8 and the growth interface 7 as a weight value in a weighted average mode;
calculating the characteristic temperature t' ═ t-r 0.01
Determining cold bar temperature
Setting the crystallization temperature of the tellurium-zinc-cadmium melt as t0, wherein the tellurium-zinc-cadmium crystallization temperatures are different in proportion;
if t ' < t0, the cold source temperature of the cold pole rod 4 is t0, and if t ' > t0, the cold source temperature is (t ' + t 0)/2.
As shown in FIGS. 1 and 3-5, the growth device of the CdZnTe single crystal comprises a crucible 3, a hot pole tube 2 for keeping the CdZnTe melt 5 at a constant temperature is arranged in the crucible 3, the hot pole tube 2 is used for ensuring the temperature in the crucible 3 to be stable and avoiding the initiation of new crystallization, and a cold pole rod 4 for carrying out central temperature reduction on the CdZnTe melt 5 penetrates through the hot pole tube 2 and is used for keeping the temperature of the central area of a growth interface 7 at a lower level.
The diameter of the cold pole 4 is 6 mm.
In the using process of the invention, the lower parts of the hot electrode tube 2 and the cold electrode rod 4 are extended into the crucible 3, the bottom ends of the hot electrode tube 2 and the cold electrode rod 4 are close to the growth interface 7 between the melt 5 and the crystal 6, then in the growth furnace 1, the hot electrode tube 2 and the cold electrode rod 4 and the crucible 3 move relatively, the central area temperature of the growth interface 7 is in a lower level through the cold electrode rod 4, the relative low temperature of the cold electrode rod 4 is prevented from initiating new crystals in the melt 5 through the hot electrode tube 2, the growth interface 7 is ensured to grow from the center, the outer wall of the crucible 3 can also be influenced to a certain degree, the probability of nucleation on the outer wall is reduced, the temperature of the side of the melt 5 at the growth interface 7 can be artificially interfered, the growth interface is ensured to form a condition that the central point is slightly lower, and the growth can be ensured to expand from the center to the periphery with a large probability, meanwhile, the heat pipe is used for keeping the area outside the central point to be higher than the central point, so that the phenomenon that nucleation at other places generates polycrystal is avoided, the structure is simple, the tellurium-zinc-cadmium melt 5 is stable in crystallization, and the growth efficiency is high.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.