CN210262080U - Device for growing ZnTe monocrystal in gas phase - Google Patents
Device for growing ZnTe monocrystal in gas phase Download PDFInfo
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- CN210262080U CN210262080U CN201920733278.8U CN201920733278U CN210262080U CN 210262080 U CN210262080 U CN 210262080U CN 201920733278 U CN201920733278 U CN 201920733278U CN 210262080 U CN210262080 U CN 210262080U
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Abstract
The utility model discloses a device and a method for growing ZnTe monocrystal by gas phase, the device comprises: the heating furnace sequentially comprises a constant temperature area and a linear cooling area along the axial direction, and is provided with a furnace chamber which penetrates through the two temperature areas; the quartz tube is arranged in the furnace chamber of the heating furnace and can relatively move along the axial direction of the furnace chamber; the combined quartz boat consists of main boat, material boat and crystal growing casing. The device has a first working state and a second working state, wherein in the first working state, the main boat is separated from the crystal growth sleeve, and the air pressure in the quartz tube is pumped to 10‑5Pa is then flushed with argon. In the second working state, the main boat and the crystal growth sleeve are connected by the quartz frosting, a closed space is formed in the main boat, the material boat is heated to a target temperature, and the heating furnace is controlled to axially move along the furnace chamber at a constant speed matched with the crystal growth rate, so that the solid-gas interface of the ZnTe crystal is always kept in a constant growth temperature field environment in the crystal growth process, and the stable growth of the ZnTe single crystal is realized.
Description
Technical Field
The utility model belongs to the field of single crystal material preparation, in particular to a device and a method for growing ZnTe single crystal in gas phase.
Background
The ZnTe crystal is a II-VI group compound semiconductor material, has a face-centered cubic structure and a forbidden band width of 2.26ev, can be properly improved and changed along with heavy doping, and is an excellent luminescent material for manufacturing solar cells and high-brightness LEDs. Particularly, because the ZnTe crystal has very obvious nonlinear optical properties and excellent light transmission characteristics, the ZnTe crystal has attracted much attention as a material for terahertz wave emitting and receiving devices in the period of high importance and development and application of the current terahertz technology. The melting point of the ZnTe crystal material reaches 1300 ℃, which makes the growth and preparation of the material difficult. In addition, growth of the ZnTe bulk crystal becomes very difficult due to factors such as increased vapor pressure of the crystal, difficulty in controlling impurities and defects, and easy deformation of the quartz crucible for evaporation. Compared with melt growth, Physical Vapor Transport (PVT) is an effective technology for growing ZnTe single crystals at present, and the technology has the advantages of low crystal growth temperature, complete crystals, good performance and the like.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a device and a method for growing ZnTe single crystal in gas phase, which can keep the constant growth environment of the solid-gas interface of the ZnTe single crystal and realize the stable growth of the ZnTe single crystal.
The utility model adopts the technical scheme as follows:
an apparatus for vapor-phase growing a ZnTe single crystal, comprising:
the heating furnace comprises a constant temperature area and a linear cooling area, and is provided with a furnace chamber penetrating through the two temperature areas;
the quartz tube is inserted in the furnace chamber of the heating furnace and can move relatively along the axial direction of the furnace chamber, and the quartz tube is provided with an inner cavity, one end of the quartz tube is sealed, the other end of the quartz tube is opened, and the quartz tube can be vacuumized.
The combined quartz boat is formed by combining a main boat, a material boat and a crystal growth sleeve, and the main boat, the material boat and the crystal growth sleeve can be separated. The material boat is an open quartz boat and is used for placing ZnTe polycrystalline particles; the main boat is a quartz boat with one closed end and a frosted opening at one end, the closed end is used for placing the material boat, and the open end is used for connecting the crystal growth sleeve. The long brilliant sleeve pipe is for having the combination quartz piece of dull polish mouth and a quartz stick, and its dull polish mouth can be connected sealedly with main boat dull polish mouth, and the department that meets with quartz stick of dull polish mouth is most advanced form.
The flange can be arranged at the open end of the quartz tube, an air exhaust hole and a closed piston port are formed in the flange, and a quartz rod of the crystal growth sleeve penetrates through the piston port and can axially and horizontally move under the condition of keeping closed.
Furthermore, the heating furnace is driven by a driving device to move relative to the quartz tube, and the constant temperature area and the linear cooling area are sequentially arranged along the axial direction of the furnace chamber. The range of the constant temperature area of the heating furnace is larger than the maximum range of relative movement of the material boat, namely, the material boat is always positioned in the constant temperature area in the crystal growth process.
Furthermore, the device also comprises a temperature measurement galvanic couple arranged at the bottom of the material boat and the tip of the crystal growth sleeve, and the quartz rod in the crystal growth sleeve plays a role in temperature guiding, so that a temperature concave point is formed at the tip of the quartz rod, and the growth of crystals is facilitated. The device also comprises a controller which is electrically connected with the temperature measuring couple and the driving device and is used for acquiring inner cavity temperature data detected by the temperature measuring couple and sending a control signal for adjusting the speed or stopping the movement to the driving device according to the acquired inner cavity temperature data so as to control the movement of the heating furnace relative to the quartz tube. In addition, the heating furnace can adopt an electric heating furnace. And can be horizontally arranged or vertically arranged.
Further, the quartz tube may be evacuated, preferably 10-5Pa or less.
Furthermore, the quartz tube is provided with a scavenging port which is communicated with the inner cavity and is used for filling argon after vacuumizing, the quartz tube can be filled with argon, and the pressure of the argon can be adjusted so as to adjust the growth speed of the single crystal.
The device has a first working state and a second working state, wherein in the first working state, the main boat is separated from the crystal growth sleeve, and the air pressure in the quartz tube is pumped to 10-5Pa, then flushing argon; and in the second working state, the main boat is connected with the crystal growth sleeve through the frosted opening, a closed space is formed in the main boat, the material boat is heated to a target temperature, and the heating furnace moves axially at a constant speed.
The utility model also provides a method for utilizing above-mentioned device vapor growth ZnTe single crystal, including following step:
a) putting ZnTe polycrystal granular materials into a material boat, and sealing an outer quartz tube;
b) vacuum pumping is carried out to 10-5Pa below;
c) filling argon into the quartz tube to reach the required pressure;
d) pushing the quartz rod of the crystal growth sleeve to enable the grinding opening of the crystal growth sleeve and the grinding opening of the main boat to be combined to form a closed space;
e) raising the temperature of the furnace to the required temperature;
f) after entering a stable working state, axially moving the heating furnace at a speed of 5-10 mm/day, keeping the operation of the furnace stable and free from shaking, and keeping the temperature of a long crystal face solid/gas interface constant in the moving process of the furnace body;
g) and (5) continuing for 2-3 days to finish the crystal growth process.
The utility model has the advantages that: the utility model discloses a unique structural design, the solid gas interface keeps invariable growing environment when can making the ZnTe crystal growth, is favorable to realizing the stable growth of ZnTe single crystal.
Drawings
FIG. 1 is a schematic structural diagram of a vapor phase growth ZnTe single crystal apparatus of the present invention.
FIG. 2 is a schematic view of the temperature zone of the heating furnace in the apparatus for vapor-phase growth of ZnTe single crystal of the present invention.
The reference numbers in the figures are: 1. heating furnace; 2. a quartz tube; 3. a main boat; 4. a material boat; ZnTe polycrystalline granules; 6. growing a crystal sleeve; 7. a flange; 8. a constant temperature region; 9. a linear cooling region.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the invention can be more easily understood by those skilled in the art. As used in this specification and the appended claims, the terms "comprises" and "comprising" are intended to only encompass the steps and elements that are expressly identified, but not to constitute an exclusive list, and that a method or apparatus may include other steps or elements.
The directional words mentioned in the present invention are defined for convenience of description and according to the viewing angle of the conventional observation, and do not define specific directions, for example, "upper", "lower", "left" and "right" correspond to the upper side, lower side, left side and right side of the paper surface in fig. 1, respectively.
The embodiment provides a device for growing ZnTe single crystals in a gas phase, in particular to a device for growing ZnTe single crystals in a gas phase by moving a horizontal thermal field. Referring to fig. 1, the apparatus includes:
the heating furnace 1 comprises a constant temperature area 8 and a linear cooling area 9 along the horizontal direction, the two temperature areas are divided according to the furnace temperature, and the heating furnace 1 is provided with a furnace chamber which penetrates through the two temperatures;
the quartz tube 2 is inserted into the furnace chamber of the heating furnace 1 and can relatively move along the horizontal direction, one end of the quartz tube 2 is open, the other end of the quartz tube is closed, and the quartz tube is provided with an inner cavity;
the combined quartz boat is formed by combining a main boat 3, a material boat 4 and a crystal growth sleeve 6. The combined quartz boat is arranged in the inner cavity of the quartz tube 2. The main boat 3 is a quartz tube with one open end and one closed end and is provided with an inner cavity and a frosted opening; the material boat 4 is used for containing ZnTe polycrystalline granular materials 5 and is placed in the main boat 3; the crystal growth sleeve 6 is composed of a quartz rod and a quartz piece with a frosted opening. The main boat 3 and the crystal growth sleeve 6 can be connected by a frosted opening.
The growth device has a first working state and a second working state, wherein in the first working state, the main boat 3 is separated from the crystal growth sleeve 6, and the air pressure in the quartz tube 2 is pumped to 10-5Pa is then flushed with argon. In the second working state, the main boat 3 is connected with the crystal growth sleeve 6 through the frosted opening, a closed space is formed in the main boat 3, the material boat 4 is heated to a target temperature, and the heating furnace 1 moves horizontally at a constant speed.
Specifically, in the present embodiment, the apparatus is an apparatus for vapor-phase growth of ZnTe single crystal, and the furnace chamber of the heating furnace 1 is horizontally disposed and has a shape matching the shape of the quartz tube 2 so as to be able to accommodate the quartz tube 2. Relative to the quartz tube, the heating furnace 1 is movably arranged along the horizontal direction, and the constant temperature zone 8 and the linear cooling zone 9 are arranged from left to right in sequence. During growth of the ZnTe single crystal, the heating furnace 1 is gradually moved from left to right. That is, initially, the material boat 4 in the main boat 3 is located at the left side of the constant temperature region 8, and the tip of the long-crystal casing 6 is located at a certain point in the linear cooling region. Along with the growth of the ZnTe single crystal, the solid-gas interface of the crystal is changed, the heating furnace 1 slowly moves from left to right, the moving speed is kept to be the same as the growth speed of the crystal, and the growth environment of the growth interface of the ZnTe single crystal can be kept to be completely consistent.
The heating furnace 1 is driven by a driving device to move left and right. This drive arrangement can select for use the drive arrangement known in the prior art, if drive heating furnace 1 through motor and transmission and remove, and transmission can select synchronous belt drive system or chain drive system, converts the moment of torsion of motor into the linear motion of hold-in range or material strip, then drives heating furnace 1 through linear motion's hold-in range or chain and removes. And will not be described herein.
The quartz tube 2 is in a cylindrical shape which is horizontally arranged, and the inner cavity is correspondingly in a cylindrical shape. The main boat 3 is fixedly arranged in the cylindrical inner cavity, the left end of the main boat 3 is closed, the right end of the main boat 3 is open, and the open end of the main boat is provided with a frosted opening. The material boat 4 is arranged at the left end of the cylindrical inner cavity of the main boat 3, and ZnTe polycrystalline granules are contained in the material boat for serving as a ZnTe steam source. The connection part of the frosted opening and the quartz rod in the crystal growth sleeve 6 is in a tip shape, the crystal growth sleeve and the main boat are connected by the frosted opening, the quartz rod of the crystal growth sleeve 6 plays a role in temperature conduction, so that a temperature low point is formed at the tip of the crystal growth sleeve 6, and crystal growth is facilitated.
And a temperature measuring couple is also arranged at the bottom of the quartz tube 2 and used for measuring the temperature at the bottom of the material boat 4. The temperature measuring couple is connected with a lead and used for transmitting measured temperature data. The apparatus further comprises: and the controller is electrically connected with the temperature measuring couple and is used for acquiring the temperature data detected by the temperature measuring couple.
When ZnTe single crystal is grown, the inner cavity of the quartz tube 2 is filled with argon. The open end of the quartz tube 2 is provided with a flange 7. The flange 7 is provided with a scavenging port which is communicated with the inner cavity and is used for filling argon after vacuumizing. The flange 7 is also provided with a closed piston port, and the quartz rod of the crystal growth sleeve 6 passes through the piston port and can horizontally move under the condition of keeping the sealing.
The method for growing a ZnTe single crystal using the growth apparatus of the present embodiment is described below, and comprises the steps of:
a, putting 5 g of ZnTe polycrystalline granular material into a material boat 4, putting the material boat 4 into a main boat 3, and sealing a quartz tube 2;
b, vacuumizing the air in the quartz tube 2 to 10 DEG-5Pa below;
c, filling argon into the quartz tube 2 to 0.8 at;
d, pushing the crystal growth sleeve 6 to combine with the main boat 3 to form a closed space;
e, setting the furnace temperature of a constant temperature area of the heating furnace to 950 ℃ and setting a linear cooling area to 950-550 ℃;
after the F enters a stable working state, moving the furnace from left to right at the speed of 5 mm/day, keeping the operation of the furnace stable and free from shaking, and keeping the temperature of the long crystal face solid/gas interface constant in the moving process of the furnace body;
g lasts for 3 days, and the crystal growth process is completed.
The utility model discloses a design idea that horizontal thermal field removed through the removal rate of control thermal field, keeps growth condition uniformity such as temperature, atmosphere of ZnTe crystal growth solid/gas interface. The method has the advantages of good crystallization quality of the obtained ZnTe monocrystal and stable crystal quality.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are preferred embodiments, which are intended to enable persons skilled in the art to understand the contents of the present invention and to implement the present invention, and thus, the protection scope of the present invention cannot be limited thereby. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. An apparatus for vapor-phase growth of a ZnTe single crystal, comprising:
the heating furnace sequentially comprises a constant temperature area and a linear cooling area, and is provided with a furnace chamber which penetrates through the two temperature areas;
the quartz tube is arranged in a furnace chamber of the heating furnace and can relatively move along the axial direction of the furnace chamber, the quartz tube is provided with an inner cavity, and one end of the quartz tube is closed and the other end of the quartz tube is open;
the combined quartz boat consists of a main boat, a material boat and a crystal growth sleeve;
the main boat is a quartz boat with one closed end and a frosted opening at the other end, the material boat is placed at the closed end, and the opened end is used for connecting a crystal growth sleeve;
the material boat is an open quartz boat, is arranged at one closed end in the main boat and is used for containing ZnTe polycrystalline particles;
the crystal growth sleeve is a combined quartz piece provided with a grinding opening and a quartz rod, the grinding opening can be connected and sealed with the main boat grinding opening, and the joint of the grinding opening and the quartz rod is in a tip shape;
the flange can be arranged at the open end of the quartz tube, an air exhaust hole and a closed piston port are formed in the flange, and a quartz rod of the crystal growth sleeve penetrates through the piston port and can axially move under the condition of keeping closed.
2. An apparatus for growing a ZnTe single crystal according to claim 1, wherein the heating furnace is driven by a driving means to move relative to the quartz tube, and the constant temperature zone and the linear cooling zone are arranged in order in an axial direction of the furnace chamber.
3. An apparatus for growing ZnTe single crystal according to claim 1, further comprising a thermocouple for measuring temperature provided at the bottom of said boat and at the tip of said growth sleeve.
4. An apparatus for vapor-growing a ZnTe single crystal according to claim 1, further comprising:
and the controller is electrically connected with the temperature measuring couple and the driving device and is used for acquiring inner cavity temperature data detected by the temperature measuring couple and sending a control signal for adjusting the speed or stopping movement to the driving device according to the acquired inner cavity temperature data so as to control the movement of the heating furnace relative to the quartz tube.
5. An apparatus for vapor growing a ZnTe single crystal according to claim 1, wherein the heating furnace may be horizontally disposed or vertically disposed.
6. An apparatus for growing a ZnTe single crystal according to claim 1, wherein the quartz tube is provided with a vent for introducing argon gas after evacuation which is communicated with the inside chamber.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920733278.8U CN210262080U (en) | 2019-05-21 | 2019-05-21 | Device for growing ZnTe monocrystal in gas phase |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920733278.8U CN210262080U (en) | 2019-05-21 | 2019-05-21 | Device for growing ZnTe monocrystal in gas phase |
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| CN210262080U true CN210262080U (en) | 2020-04-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093667A (en) * | 2019-05-21 | 2019-08-06 | 浙江森尼克半导体有限公司 | A kind of device and method of vapor phase growth ZnTe monocrystal |
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- 2019-05-21 CN CN201920733278.8U patent/CN210262080U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093667A (en) * | 2019-05-21 | 2019-08-06 | 浙江森尼克半导体有限公司 | A kind of device and method of vapor phase growth ZnTe monocrystal |
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