Method for growing large-size platy eutectic fluorescent material for weapon motion trail camera shooting

Abstract

The invention discloses a method for growing a large-size platy eutectic fluorescent material for weapon motion trail camera shooting, which comprises the following steps: pulling a crucible to slowly move on a horizontal clamping groove crystal pulling track by using a crystal pulling rod, so that the head of the crucible is close to a heating area; the power is increased to 18.5 kW, and the crucible continues to be moved through the horizontal clamping groove crystal pulling track when the raw materials begin to melt, so that the crucible stably and completely enters a heating area; the power of the growth furnace is continuously increased to 23.5 kW and kept for 5 hours, after material melting operation is completed, the crucible is pulled through a crystal pulling rod, the head of the crucible is moved to the junction of the heating area and the cooling area at the manual pulling speed of 200 mm / h, and crystal pulling is started at the crystal pulling speed of 50 mm / h; and S5, when the tail part of the crucible reaches the junction of the heating area and the cooling area, ending eutectic growth. The invention provides a method for growing a large-size plate-shaped eutectic fluorescent material for weapon motion trail camera shooting, which can effectively ensure that a crucible can move stably after the crystal pulling rate is increased, and prevent the problems of eutectic cracking and the like caused by crucible bumping.

Description

Technical Field

[0001] The present invention relates to the technical field of preparing Al2O3 / YAG:Re eutectic fluorescent materials for weapon motion trajectory photography. More specifically, the present invention relates to a method for growing large-size plate-shaped eutectic fluorescent materials for weapon motion trajectory photography. Background Art

[0002] In the translucent Al2O3 / YAG eutectic material, the YAG phase and Al2O3 grow intertwined with each other, making it exhibit excellent high-temperature stability in high-temperature environments, so it has always been used as a structural material in high-temperature environments. By doping rare earth elements into the Al2O3 / YAG eutectic material, a variety of new and efficient phosphors can be prepared with the Al2O3 / YAG eutectic as the matrix, which has great engineering application prospects and potential economic value. For example, in the field of high-speed photography of the movement trajectory of buried weapons, high-power white light LEDs are needed as light sources for illumination. Using Al2O3 / YAG:Re eutectic as a fluorescent material instead of epoxy resin encapsulated phosphor materials can effectively solve the resin aging problem caused by the heating of high-power white light LED light sources and greatly improve the service life of high-power white light LED devices. In the process of large-size eutectic growth, for large-size plate-shaped Al2O3 / YAG:Re eutectics doped with rare earth elements, a large temperature gradient is generally required to complete the crystallization growth of the eutectic. However, once the eutectic movement is bumpy during the large temperature gradient crystal pulling process, it will cause the eutectic to crack, so a smooth crystal pulling track is required to realize the eutectic pulling process.

[0003] However, the crystal pulling track in the IKAK-2 crystal growth furnace produced by Donetsk Company in Ukraine, which is used in the horizontal directional solidification preparation of large-sized plate-shaped Al2O3 / YAG:Re eutectics, cannot fully meet the production needs. Specifically, when using the IKAK-2 crystal growth furnace for rapid melting and recrystallization of large-sized plate-shaped Al2O3 / YAG:Re eutectics, the original crystal pulling track has no slot components and a small number of rollers. When the crystal pulling rate increases, the crucible shakes left and right, moves abruptly back and forth, etc., which will cause the eutectic to crack or crack inside. More seriously, the internal stress of the eutectic is over-concentrated during the growth process, resulting in the inability of the eutectic to solidify and form, and ultimately causing the preparation to fail. Therefore, a new type of horizontally placed roller crystal pulling track is designed to complete the production. Summary of the invention

[0004] An object of the present invention is to solve at least the above problems and / or disadvantages and to provide at least the advantages which will be described hereinafter.

[0005] In order to achieve these purposes and other advantages of the present invention, a method for growing a large-size plate-shaped eutectic fluorescent material for weapon motion trajectory photography is provided, comprising: S1. Place the boat-shaped molybdenum crucible with raw materials on the horizontal slot crystal pulling track of the growth furnace, seal the furnace and heat it up. During the heating process, the vacuum degree in the furnace needs to be maintained at 5.0×10 -3 Pa or above; S2. Use the crystal pulling rod to pull the crucible to move slowly on the horizontal slot crystal pulling track so that the crucible head is close to the heating zone; increase the power to 18.5kW, and continue to move the crucible through the horizontal slot crystal pulling track when the raw material begins to melt, so that it is stable and enters the heating zone completely; S3, continuously increasing the power of the growth furnace to 23.5 kW and maintaining it for 5 hours to perform a material chemical operation; S4. After the material is quenched, the crucible is pulled by a crystal pulling rod to move the crucible head to the junction of the heating zone and the cooling zone at a manual pulling speed of 200 mm / h, and crystal pulling is started at a crystal pulling speed of 50 mm / h; S5, when the tail of the crucible reaches the junction of the heating zone and the cooling zone, the eutectic growth ends, and the power of the growth furnace is reduced to 21.5 kW at a cooling rate of 0.8 kW / h within 2.5 hours; S6. Reduce the power of the growth furnace to zero at a cooling rate of 0.72 kW / h within 30 hours, and continue to operate circulating cooling water and high vacuum for about 36 hours to reduce the temperature in the furnace to room temperature.

[0006] Preferably, the horizontal slot crystal pulling track is configured to include: At least two groups of roller fixed supports are respectively arranged on the side walls of the bottom of the tunnel corresponding to the heating zone and the cooling zone, and each group of roller fixed supports consists of two roller fixed supports arranged opposite to each other; A roller that is inserted into the fixing holes of each set of roller fixing supports to connect two roller fixing supports that are arranged opposite to each other into an integrated structure; A track group arranged on rollers and spaced at a predetermined distance to support and guide the tray, wherein the track group is composed of an even number of tracks; Track connectors are provided at the two free ends of the track to connect the tracks into an integrated structure; Wherein, a connection hole matching with an external crystal pulling connection rod is provided on one side track connection piece; A convex ring matching the spacing distance of the tracks is arranged in the middle of the roller, and the track group is clamped on the convex ring in a symmetrical manner.

[0007] Preferably, the materials of the rollers, track connectors and track groups are all tungsten-molybdenum rods; The track connector is connected to the track assembly via a fixing hole and a molybdenum wire inserted into the fixing hole.

[0008] Preferably, it further comprises: two L-shaped pallet baffles arranged on the track group to define a pallet placement area; Two stopper posts extending horizontally toward the track connector are respectively provided on each L-shaped tray baffle; The boat-shaped molybdenum crucible is arranged on a tray, and a plurality of heat insulation screens are arranged on one side of the tray.

[0009] The present invention includes at least the following beneficial effects: First, the present invention optimizes the horizontal directional solidification equipment of large-sized plate-like eutectics, and can obtain the largest domestic plate-like eutectics of the size of 100 millimeters, and the quality of the eutectic can be significantly improved.

[0010] Secondly, the present invention designs a novel horizontally placed roller crystal pulling track, by setting 4 rollers, and setting matching annular protrusions at the centers of the rollers, and setting the track to an even number, so that when the center is clamped on the annular protrusion, the central symmetry and the limitation of the annular protrusion are utilized, so that compared with the prior art, it can effectively ensure that the crucible can move smoothly after the crystal pulling rate is increased, and prevent the eutectic from cracking due to the bumps of the crucible. Problems such as the growth and preparation of large-size plate-like Al2O3 / YAG:Re eutectics with better performance can be obtained.

[0011] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 It is a schematic structural diagram of a roller crystal pulling track according to an embodiment of the present invention; Figure 2 for Figure 1 A schematic cross-sectional view of Figure 3 for Figure 1 Schematic diagram of longitudinal section; Figure 4 for Figure 3 A magnified schematic diagram of the middle left part; Figure 5 for Figure 3 A magnified schematic diagram of the middle right part; Among them, tunnel wall A-1, tunnel wall B-2, roller fixed support-3, roller-4, track assembly-5, tray-6, molybdenum wire-7, annular protrusion-8, track-9, stop column-10, L-shaped tray baffle-11, track connector-12, fixing hole-13, connecting hole-14, heat insulation screen-15. DETAILED DESCRIPTION

[0013] The present invention is further described in detail below in conjunction with the accompanying drawings so that those skilled in the art can implement the invention with reference to the description.

[0014] It should be understood that terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0015] It should be noted that in the description of the present invention, the orientation or positional relationship indicated by the term is based on the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention. In addition, the terms "Ⅰ" and "Ⅱ" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0016] In the description of the present invention, it should be noted that, unless otherwise clearly stipulated and limited, the terms "installed", "provided with", "mounted / connected", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection. It can be a mechanical connection or an electrical connection. It can be directly connected or indirectly connected through an intermediate medium. It can be the internal connection of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0017] like Figure 1-Figure 5 The horizontally placed roller crystal pulling track of the present invention includes: tunnel wall A 1, tunnel wall B 2, at least two groups of roller fixing supports 3 arranged in each tunnel wall, multiple rollers 4 placed horizontally for connecting each group of roller fixing supports 3 into an integrated structure, track components 5 arranged on the rollers 4, trays 6 arranged on the track components 5, etc., all of which are made of tungsten-molybdenum rods and fixed by punching and interlacing. The middle part of the four horizontally placed rollers 4 has an annular protrusion 8, which can clamp the track to prevent the tray 6 and the crucible from moving left and right. The increase in the number of horizontally placed rollers 4 can improve the stability of the track when it moves forward and backward. At the same time, according to the size of the growing eutectic, the size of the track tray 6 can be increased or decreased according to actual experimental needs.

[0018] Example 1 This embodiment mainly describes the realization form of the combined structure of the tunnel wall of the horizontally placed roller pulling track and the roller fixed support. Figure 2 As shown, the combined structure of each tunnel wall and the roller fixed support 3 includes: two tunnel walls with square dimensions are respectively installed inside the multi-layer partitioned thermal insulation screen, a heating body installation position is reserved between the two tunnel walls, and an installation groove with a size of 30mm×20mm is opened on the lower wall of the two tunnels for respectively fixing 8 installation roller fixed supports 3.

[0019] Example 2 like Figure 2-Figure 5As shown, this embodiment mainly describes the implementation form of the combined structure of the horizontally placed roller 4, the track assembly 5, and the tray 6, and its specific structure includes: a horizontally placed roller 4 is respectively installed between each two roller fixing supports 3 arranged opposite to each other, a total of 4 pieces, and an annular protrusion 8 for defining the track is arranged in the middle of each roller 4; The track assembly 5 is mainly composed of tungsten rods, including 4 tracks 9, 4 stop columns 10, 2 L-shaped tray baffles 11, and 2 track connectors 12; the 2 track connectors 12 are two tungsten connecting mechanisms at the front and rear ends of the track 9. After the fixing holes 13 are punched in the track 9 and the track connectors 12, the 4 tracks 9 are fixed by the molybdenum wire 7 passing through the fixing holes 13. At the same time, a connecting hole 14 is also provided on one side of the track connector 12 for connecting with an external crystal pulling rod; the rectangular tray 6 is placed in the area defined by the two L-shaped tray baffles 11, and is used to place a boat-shaped molybdenum crucible, multiple heat insulation screens 15 and raw materials that need to be heated and melted.

[0020] The specific shapes and sizes of each component are as follows: The tunnel wall A1 is a rectangular cavity of 300×120×2 mm, 357 mm in height, with four 30×20 mm roller 4 mounting slots at the bottom; The tunnel wall B 2 is a rectangular cavity of 300×120×2 mm, 307 mm in height, and has four 30×20 mm mounting slots for rollers 4 at the bottom; The roller fixing support 3 is a rectangular block with a bottom of 40×20×1.5 mm, a boss with a size of 40×20×22 mm on the top, and a round hole with a diameter of 10 mm in the middle; Four horizontally placed rollers 4: 22mm diameter cylinder, 10mm diameter round hole in the middle, 18×88mm diameter slots on both sides 3mm away from the end face; The four rails 9 are all made of 290×10mm cylinders; The four stopper posts 10 are all 30×10 mm cylinders; The two L-shaped tray baffles 11 are both made of 38×20×3mm angle iron, with a width of 216×176, and 15×15mm slots on both sides are used to reserve installation positions for the stopper columns 10; The two rail connectors 12 are both 216×10×5mm long strips with four circular fixing holes of 3mm in diameter in the middle; The tray 6 is a rectangular tray of 290×226×38 mm, and has a groove of 284×220×30 mm inside.

[0021] Example 3 The original crystal pulling track in the IKAK-2 type crystal growth furnace is only suitable for single crystal growth, with a low temperature gradient, slow crystal pulling speed, and no large bumps, but it is difficult to meet the needs of fast melting and recrystallization of large-sized plate-shaped Al2O3 / YAG:Re eutectics. This embodiment uses the horizontal roller crystal pulling track of Example 2 to grow large-sized plate-shaped Al2O3 / YAG:Re eutectics in the IKAK-2 type growth furnace produced by Donets Company in Ukraine. The operation process is as follows: 10 kg of dense raw material is loaded into the processed boat-shaped molybdenum crucible (referred to as crucible or boat-shaped crucible) and placed on this horizontal slot crystal pulling track and then loaded into the furnace to seal the furnace. Turn on the cooling circulation system, mechanical pump and diffusion pump, and turn on the power for heating. The vacuum degree must be maintained at 5.0×10 -3 Pa, use the crystal pulling rod to pull the crucible to move slowly on the horizontal card slot crystal pulling track, so that the crucible head is close to the heating zone; increase the power to 18.5kW, the raw material begins to melt, and the vacuum degree will fluctuate slightly at this time. Continue to move the crucible on the horizontal card slot crystal pulling track to make it stable and all enter the heating zone. At this time, continue to increase the power to 23.5kW and keep it for 5 hours to achieve the purpose of fully melting the material. Slowly move the crucible head to the junction of the heating zone and the cooling zone. Because the horizontal card slot crystal pulling track can reduce the bumps of the crucible during the crystal pulling process, the crystal pulling rate can be greatly increased. Therefore, pull the crystal at a pulling speed of 50mm / h. When the tail of the crucible reaches the junction of the heating zone and the cooling zone, the crucible enters the cooling zone, and the eutectic growth ends. The power was reduced to 21.5 kW in 2.5 hours (the cooling rate was about 0.8 kW / h); then the power was reduced to zero in 30 hours (the cooling rate was about 0.72 kW / h); finally, circulating cooling water and high vacuum were maintained for about 36 hours to reduce the temperature in the furnace to room temperature.

[0022] The super-large plate-shaped Al2O3 / YAG:Re eutectic grown using this horizontal slot crystal pulling track has no visible bubbles or cracks, and is of good quality. The size is about 220mm×200mm×35mm, and this experiment is over. Through this experiment, it can be seen that the horizontal roller crystal pulling track designed by the present invention effectively solves the problem of rapid movement and bumping of the material boat by adding a slot in the middle of the track roller, so that during the eutectic growth, the horizontal slot crystal pulling track enables the boat-shaped molybdenum crucible to move stably at a speed of 50mm / h during the eutectic growth, which is significantly improved compared to the movement rate of 1mm / h in the original single crystal growth. In addition, the improvement this time adopts a purely physical structure design to ensure stability. Compared with other electronic designs, it can better adapt to the dual requirements of high temperature environment and stability during eutectic growth.

[0023] The above solution is only an illustration of a preferred embodiment, but is not limited thereto. When implementing the present invention, appropriate replacement and / or modification can be performed according to user needs.

[0024] The number of devices and processing scales described here are used to simplify the description of the present invention. Applications, modifications and variations of the present invention will be obvious to those skilled in the art.

[0025] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and the embodiments. It can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily realized. Therefore, without departing from the general concept defined by the claims and equivalent scope, the present invention is not limited to the specific details and the illustrations shown and described here.

Claims

1. A method for growing large-size plate-shaped eutectic fluorescent materials for weapon motion trajectory photography, characterized in that: include: S1. Place the boat-shaped molybdenum crucible with raw materials on the horizontal slot crystal pulling track of the growth furnace, seal the furnace and heat it up. During the heating process, the vacuum degree in the furnace needs to be maintained at 5.0×10 -3 Pa or above; S2. Use the crystal pulling rod to pull the crucible to move slowly on the horizontal slot crystal pulling track so that the crucible head is close to the heating zone; increase the power to 18.5kW, and continue to move the crucible through the horizontal slot crystal pulling track when the raw material begins to melt, so that it is stable and enters the heating zone completely; S3, continuously increasing the power of the growth furnace to 23.5 kW and maintaining it for 5 hours to perform a material chemical operation; S4. After the material is quenched, the crucible is pulled by a crystal pulling rod to move the crucible head to the junction of the heating zone and the cooling zone at a manual pulling speed of 200 mm / h, and crystal pulling is started at a crystal pulling speed of 50 mm / h; S5, when the tail of the crucible reaches the junction of the heating zone and the cooling zone, the eutectic growth ends, and the power of the growth furnace is reduced to 21.5 kW at a cooling rate of 0.8 kW / h within 2.5 hours; S6. Reduce the power of the growth furnace to zero at a cooling rate of 0.72 kW / h within 30 hours, and continue to operate circulating cooling water and high vacuum for about 36 hours to reduce the temperature in the furnace to room temperature.

2. The method for growing a large-size plate-shaped eutectic fluorescent material for weapon motion trajectory photography as claimed in claim 1, characterized in that: The horizontal slot crystal pulling track is configured to include: At least two groups of roller fixed supports are respectively arranged on the side walls of the bottom of the tunnel corresponding to the heating zone and the cooling zone, and each group of roller fixed supports consists of two roller fixed supports arranged opposite to each other; A roller that is inserted into the fixing holes of each set of roller fixing supports to connect two roller fixing supports that are arranged opposite to each other into an integrated structure; A track group arranged on rollers and spaced at a predetermined distance to support and guide the tray, wherein the track group is composed of an even number of tracks; Track connectors are provided at the two free ends of the track to connect the tracks into an integrated structure; Wherein, a connection hole matching with an external crystal pulling connection rod is provided on one side track connection piece; A convex ring matching the spacing distance of the tracks is arranged in the middle of the roller, and the track group is clamped on the convex ring in a symmetrical manner.

3. The method for growing a large-size plate-shaped eutectic fluorescent material for weapon motion trajectory photography as claimed in claim 2, characterized in that: The materials of the rollers, track connectors and track groups are all tungsten-molybdenum rods; The track connector is connected to the track assembly via a fixing hole and a molybdenum wire inserted into the fixing hole.

4. The method for growing a large-size plate-shaped eutectic fluorescent material for weapon motion trajectory photography as claimed in claim 2, characterized in that: The invention also includes: two L-shaped pallet baffles arranged on the track group to define a pallet placement area; Two stopper posts extending horizontally toward the track connector are respectively provided on each L-shaped tray baffle; The boat-shaped molybdenum crucible is arranged on a tray, and a plurality of heat insulation screens are arranged on one side of the tray.

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