CN112853473A

CN112853473A - LiF crystal growth method and device

Info

Publication number: CN112853473A
Application number: CN202110087424.6A
Authority: CN
Inventors: 范庆英; 邱睿; 邱少卿; 崔硕; 刘志; 谢付莹; 孔宝国; 王培君; 石煜; 韩超; 程阳; 邱旭; 杨仪
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-01-22
Filing date: 2021-01-22
Publication date: 2021-05-28

Abstract

The invention relates to the field of lithium fluoride crystal cultivation, and discloses a LiF crystal growth method and a device thereof, it includes the equipment body, the reacting furnace, bell and crucible, the bottom symmetry of bell is fixed with the pull rod that just is located the reacting furnace of two vertical directions, the bottom of two pull rods all is fixed with rather than vertically and be the telescopic connecting rod, it all is fixed with curved cover that presss from both sides to be close to one side on two connecting rods, two press from both sides the cover cooperation and be used for fixed crucible, one side of equipment body is connected with the mounting bracket, it is connected with the bull stick to rotate on the mounting bracket, be fixed with the carousel on the bull stick, be provided with on the mounting bracket and be used for driving the bull stick to carry out pivoted runner assembly, the top of carousel is fixed with the deflector of vertical direction, there is the dead lever of block sliding connection on the deflector on the bell, be. The crucible can be conveniently charged and taken out, and the problem that raw materials or crystals are spilled accidentally during manual taking is avoided.

Description

LiF crystal growth method and device

Technical Field

The invention belongs to the field of cultivation of lithium fluoride crystals, and particularly relates to a LiF crystal growth method and a LiF crystal growth device.

Background

The molecular formula of the lithium fluoride is LiF, and the lithium fluoride belongs to a cubic crystal system. Experiments have shown that when LiF crystals are irradiated with gamma rays, a stable laser output is facilitated. Using (Mg, Cu, P): LiF single crystal can be used for manufacturing detection elements of thermoluminescent detectors and X-ray fluorescence analyzers. In addition, the LiF single crystal also has good ultraviolet transmitting function and fluorine gas erosion resistance, and can be used for manufacturing window materials of fluorine-containing lasers.

In the process of cultivating the lithium fluoride crystal, raw materials need to be put into a crystal growth furnace for cultivating. The crystal growing furnace is a technological test instrument, is mainly suitable for preparing oxides, photonic crystal metals, alloys, compounds and various single crystal samples, and can regulate the atmosphere in the growing process.

However, due to the fact that the reaction furnace of the crystal growth furnace is high due to the fact that the apparatus is used, when the apparatus is used, an operator needs to climb to a high place by means of other tools to open the reaction furnace to put in raw materials or take out cultured crystals, and in the process, the operator is prone to accidentally spill the crystal when the raw materials are put in or the crystals are taken out due to unstable gravity center, and therefore the LiF crystal growth method and the LiF crystal growth device are provided.

Disclosure of Invention

The invention aims to: in order to solve the problems that the reaction furnace of the crystal growth furnace provided by the background technology is high, when in use, an operator needs to climb to a high place by other tools to open the reaction furnace to put in raw materials or take out cultured crystals, and in the process, the operator is easy to accidentally spill the raw materials or the cultured crystals when putting in the raw materials or taking out the crystals due to unstable gravity center, the invention provides the LiF crystal growth method and the LiF crystal growth device.

In order to achieve the above purpose, the invention provides, on one hand, a LiF crystal growth apparatus, which comprises an apparatus body, a reaction furnace, a furnace cover and a crucible, wherein two pull rods which are in the vertical direction and are positioned in the reaction furnace are symmetrically fixed at the bottom end of the furnace cover, telescopic connecting rods which are perpendicular to the pull rods are fixed at the bottom ends of the two pull rods, arc-shaped jackets are fixed at the sides of the two connecting rods which are close to each other, the two jackets are matched for fixing the crucible, a mounting frame is connected at one side of the apparatus body, a rotating rod is rotatably connected at the top end of the mounting frame through a bearing, a rotating disc is fixed at the top end of the rotating rod, a rotating assembly for driving the rotating rod to rotate is arranged on the mounting frame, a guide plate in the vertical direction is fixed at the top end of the rotating disc, and a fixing rod which is clamped, and the turntable is provided with a driving assembly for driving the fixing rod to slide up and down.

Furthermore, a sliding groove in the vertical direction is formed in the guide plate, and a sliding block clamped and slidably connected with the sliding groove is fixed at one end, far away from the furnace cover, of the fixed rod.

Furthermore, the sliding groove is a wedge-shaped groove, and the sliding block is a wedge-shaped block matched with the wedge-shaped groove.

Further, drive assembly is including installing the electronic gear steering ware on the carousel, the top of electronic gear steering ware is rotated and is connected with the lead screw of vertical direction and activity through the deflector bottom, lead screw and slider screw thread through connection and its top are passed through the bearing and are connected with the groove top of spout.

Furthermore, the rotating assembly comprises a motor which is connected to the mounting frame and has an output shaft which is vertically upward, and gears which are meshed with each other are fixed at the top end of the output shaft of the motor and the outer peripheral side of the rotating rod.

Furthermore, two connecting grooves which are vertical and communicated with the top end of the reaction furnace are symmetrically formed in the inner wall of the reaction furnace, each pull rod is located in the corresponding connecting groove, each connecting groove is a T-shaped groove, and each pull rod is a T-shaped rod matched with the T-shaped groove.

Further, every the connecting rod all includes with the fixed hollow rod of the pull rod that corresponds, two the equal slip grafting in one side that is close to each other on the hollow rod has with the fixed inserted bar of the cover that corresponds, be provided with between hollow rod and the inserted bar and be used for the spacing subassembly of injecing the sliding distance of inserted bar.

Further, spacing subassembly is including the stopper of symmetry fixing at every inserted bar top, bottom respectively, every the spacing groove of being connected with the stopper cooperation that corresponds is all seted up to both sides about the inner wall of hollow rod, every the one end that is close to the corresponding hollow rod outside on the spacing groove all communicates with each other with the hollow rod that corresponds.

In another aspect of the present invention, there is provided a method for growing LiF crystal, the method comprising the steps of:

charging raw materials into a crucible;

putting a crucible into the reaction furnace;

filling a heat insulating material into the reaction furnace;

vacuumizing the reaction furnace to 1000 Pa;

the temperature of the reaction furnace is increased to 884-1350 ℃ and kept for 3.5 hours.

Compared with the prior art, the invention has the beneficial effects that:

according to the crucible furnace, the crucible is connected with the furnace cover, the furnace cover is connected to the guide plate in a sliding mode through the fixed rod in a clamping mode, the fixed rod, the furnace cover and the crucible can be driven to move up and down synchronously through the action of the driving assembly, after the crucible rises out of the reaction furnace, the rotating rod drives the rotating disc and the guide plate to rotate through the action of the rotating assembly, so that the crucible is not in contact with the reaction furnace in the vertical direction, then the crucible is moved down through the action of the driving assembly, the crucible can be conveniently charged and taken out, and the problem that raw materials or crystals are spilled due to accidents when the crucible is taken manually is avoided.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is an enlarged view of the structure at A of the present invention;

FIG. 3 is a schematic front view of the present invention;

FIG. 4 is a schematic side view of the present invention;

FIG. 5 is an exploded view of the present invention;

FIG. 6 is an enlarged view of the structure at B of the present invention;

FIG. 7 is an enlarged view of the structure at position C of the present invention;

FIG. 8 is an enlarged view of the structure at D of the present invention;

FIG. 9 is an enlarged view of the structure at E of the present invention;

in the figure: 1. an apparatus body; 2. a reaction furnace; 21. connecting grooves; 3. a furnace cover; 4. a pull rod; 5. a connecting rod; 51. a hollow shaft; 52. inserting a rod; 521. a limiting block; 6. a jacket; 61. a bolt; 7. a crucible; 8. a mounting frame; 81. a rotating rod; 9. a turntable; 10. a rotating assembly; 101. a motor; 102. a gear; 11. a guide plate; 111. a chute; 12. fixing the rod; 121. a slider; 13. a drive assembly; 131. an electric gear steering; 132. and a screw rod.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The LiF crystal growth method and apparatus provided by this embodiment, as shown in fig. 1 and fig. 5, comprises an apparatus body 1, a reaction furnace 2, a furnace cover 3 and a crucible 7, wherein two vertical pull rods 4 are symmetrically fixed at the bottom end of the furnace cover 3, the two pull rods 4 are located in the reaction furnace 2, the bottom ends of the two pull rods 4 are both fixed with connecting rods 5 which are perpendicular to the two pull rods 4 and are telescopic, arc-shaped jackets 6 with inward openings are fixed at the sides of the two connecting rods 5 which are close to each other, the two arc-shaped jackets 6 are connected with each other by bolts 61 to form an annular sleeve for fixing the crucible 7, furthermore, a mounting frame 8 is connected to one side of the apparatus body 1, a rotating rod 81 capable of rotating in situ is rotatably connected to the top end of the mounting frame 8 by a bearing, a rotating disc 9 is fixed to the top end of the rotating rod 81, in addition, a rotating assembly 10 for driving the rotating rod 81 is provided on the mounting frame 8, a guide plate 11 in the vertical direction is fixed at the top end of a rotary table 9, a fixing rod 12 clamped and connected on the guide plate 11 in a sliding manner is fixed on a furnace cover 3, a driving assembly 13 for driving the fixing rod 12 to slide up and down is further arranged on the rotary table 9, when the device is used, firstly, a crucible 7 is taken out from a reaction furnace 2 through the driving assembly 13, then, the crucible 7 is enabled to be relatively deviated from the reaction furnace 2 in the vertical direction through a rotating assembly 10, thus, the crucible 7 is moved down through the driving assembly 13, raw materials for synthesizing lithium fluoride can be conveniently put into the crucible 7, then, the crucible 7 filled with raw materials for synthesizing lithium fluoride is put into the reaction furnace 2 through the steps in the reverse direction, then, the furnace cover 3 is tightly closed, the reaction furnace 2 is vacuumized to 1000 Pa, then, the reaction furnace 2 is heated to 884 ℃, and the raw materials begin to melt, then, the temperature in the reaction furnace 2 needs to be kept between 884 ℃ and 1350 ℃, and after 3.5 hours, the temperature can be reduced and cooled to take out the cultured lithium fluoride crystal.

As shown in fig. 5 and 6, a vertical sliding groove 111 is formed in the guide plate 11, and a sliding block 121 engaged with the sliding groove 111 is fixed at one end of the fixed rod 12 away from the furnace lid 3, where as shown in fig. 6, the sliding groove 111 is a wedge-shaped groove, and the sliding block 121 is a wedge-shaped block adapted to the wedge-shaped groove.

The driving assembly 13 specifically operates as shown in fig. 5, the driving assembly 13 includes an electric gear steering gear 131 installed on the rotary disc 9, a lead screw 132 is rotatably connected to a top end of the electric gear steering gear 131, the lead screw 132 is vertically and movably inserted through a bottom end of the guide plate 11, the lead screw 132 is threadedly inserted into the slider 121, and a top end of the lead screw is connected to a top of the sliding slot 111 through a bearing, so that the lead screw 132 is rotated in place under the driving of the electric gear steering gear 131, and the slider 121, which is threadedly inserted into the lead screw 132 and slidably connected to the sliding slot 111, can move up and down along the sliding slot 111.

The rotating assembly 10 specifically operates as shown in fig. 1 and 2, the rotating assembly 10 includes a motor 101 connected to the mounting frame 8 and having an output shaft extending vertically upward, and gears 102 engaged with each other are fixed to a top end of the output shaft of the motor 101 and an outer peripheral side of the rotating rod 81, so that the two gears 102 and the rotating rod 81 are driven by the motor 101 to rotate synchronously.

In order to maintain the stability of the crucible 7 during moving in the reaction furnace 2, as shown in fig. 5 and 7, two connecting grooves 21 are symmetrically formed in the inner wall of the reaction furnace 2, the connecting grooves 21 are vertically and communicate with the top end of the crucible, each pull rod 4 is located in the corresponding connecting groove 21, each connecting groove 21 is a T-shaped groove, and each pull rod 4 is a T-shaped rod matched with the T-shaped groove.

The reason why the connecting rods 5 are telescopic is as shown in fig. 8 and 9, each connecting rod 5 comprises a hollow rod 51 fixed with the corresponding pull rod 4, the adjacent sides of the two hollow rods 51 are inserted with inserting rods 52 fixed with the corresponding jackets 6 in a sliding manner, a limiting assembly for limiting the sliding distance of the inserting rods 52 so as to prevent the inserting rods 52 from sliding out accidentally is arranged between the hollow rods 51 and the inserting rods 52, the limiting assembly comprises limiting blocks 521 symmetrically fixed at the top end and the bottom end of each inserting rod 52 respectively, the upper side and the lower side of the inner wall of each hollow rod 51 are provided with limiting grooves matched and connected with the corresponding limiting blocks 521, one end of each limiting groove, which is close to the outer side of the corresponding hollow rod 51, is not communicated with the corresponding hollow rod 51, so that when the limiting blocks 521 move to one end of the limiting groove, which is close to the outer side of the corresponding hollow rod 51, the blocking assembly can be, and can no longer move.

In the idle place of the device, all the electric devices and the drivers matched with the electric devices are arranged, and all the driving parts, which refer to the power element, the electric devices and the adaptive power supply, are connected through the conducting wires by the person skilled in the art, and specific connecting means refer to the following expressions that the electric connection is completed among the electric devices in sequence, and the detailed connecting means are well known in the art.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. A growth device of LiF crystals comprises an equipment body (1), a reaction furnace (2), furnace covers (3) and crucibles (7), and is characterized in that two pull rods (4) which are vertical to each other and are positioned in the reaction furnace (2) are symmetrically fixed at the bottom end of each furnace cover (3), two telescopic connecting rods (5) which are vertical to each other are fixed at the bottom ends of the two pull rods (4), arc-shaped clamping sleeves (6) are fixed at one sides of the two connecting rods (5) which are close to each other, the two clamping sleeves (6) are matched for fixing the crucibles (7), one side of the equipment body (1) is connected with an installation frame (8), the top end of the installation frame (8) is rotatably connected with a rotating rod (81) through a bearing, a rotating disc (9) is fixed at the top end of the rotating rod (81), and a rotating assembly (10) for driving the rotating rod (81) to rotate is arranged on the installation frame (8), the top of carousel (9) is fixed with deflector (11) of vertical direction, be fixed with block sliding connection dead lever (12) on deflector (11) on bell (3), be provided with on carousel (9) and be used for driving drive assembly (13) that dead lever (12) slided from top to bottom.

2. The LiF crystal growth apparatus according to claim 1, wherein the guide plate (11) is provided with a vertical sliding groove (111), and a sliding block (121) engaged with the sliding groove (111) and slidably connected is fixed at one end of the fixing rod (12) far away from the furnace cover (3).

3. The LiF crystal growing apparatus according to claim 2, wherein said chute (111) is a wedge-shaped groove, and said slide block (121) is a wedge-shaped block adapted to said wedge-shaped groove.

4. The LiF crystal growing device of claim 3, wherein the driving assembly (13) comprises an electric gear steering gear (131) installed on the rotating disc (9), the top end of the electric gear steering gear (131) is rotatably connected with a lead screw (132) which is vertically and movably penetrates through the bottom end of the guide plate (11), the lead screw (132) is in threaded penetrating connection with the sliding block (121), and the top end of the lead screw is connected with the top of the sliding chute (111) through a bearing.

5. The LiF crystal growing apparatus according to claim 1, wherein said rotating assembly (10) comprises a motor (101) connected to said mounting frame (8) and having an output shaft extending vertically upward, wherein gears (102) engaged with each other are fixed to a top end of said output shaft of said motor (101) and an outer peripheral side of said rotating rod (81).

6. The LiF crystal growing apparatus according to claim 1, wherein two connecting grooves (21) are symmetrically formed on the inner wall of the reactor (2), wherein the two connecting grooves are vertically and communicated with the top end of the reactor, each of the pull rods (4) is respectively located in the corresponding connecting groove (21), each of the connecting grooves (21) is a T-shaped groove, and each of the pull rods (4) is a T-shaped rod matched with the T-shaped groove.

7. The LiF crystal growing apparatus according to claim 1, wherein each of the connecting rods (5) comprises a hollow rod (51) fixed to the corresponding pulling rod (4), an inserting rod (52) fixed to the corresponding jacket (6) is slidably inserted into each of two adjacent sides of the hollow rods (51), and a limiting assembly for limiting a sliding distance of the inserting rod (52) is disposed between the hollow rods (51) and the inserting rod (52).

8. The growth device of LiF crystal according to claim 7, wherein the limiting assembly comprises limiting blocks (521) symmetrically fixed at the top end and the bottom end of each insertion rod (52), the upper and lower sides of the inner wall of each hollow rod (51) are respectively provided with a limiting groove in fit connection with the corresponding limiting block (521), and one end of each limiting groove, which is close to the outer side of the corresponding hollow rod (51), is not communicated with the corresponding hollow rod (51).

9. A method of growing LiF crystals, said method comprising the steps of:

charging raw materials into a crucible (7);

placing a crucible (7) into the reaction furnace (2);

filling a heat insulating material into the reaction furnace (2);

the reaction furnace (2) is vacuumized to 1000 Pa;

the temperature of the reaction furnace (2) is increased to 884-1350 ℃ and kept for 3.5 hours.