CN104790025A - Preparation device and preparation technology for magnesium fluoride single crystal coating material - Google Patents
Preparation device and preparation technology for magnesium fluoride single crystal coating material Download PDFInfo
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- CN104790025A CN104790025A CN201510174361.2A CN201510174361A CN104790025A CN 104790025 A CN104790025 A CN 104790025A CN 201510174361 A CN201510174361 A CN 201510174361A CN 104790025 A CN104790025 A CN 104790025A
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Abstract
The invention provides a p reparation device and preparation technology for a magnesium fluoride single crystal coating material. On one hand, a graphite heating body is designed to be a trapezoid cylinder (of which the lower base angle is 85.5-86.5 degrees) to form the temperature field gradient distribution (0-135 DEG C/m) in which the temperature at the upper end is high, and the temperature at the lower end is low; on the other hand, a heat-insulating sleeve on the inner wall of a bell jar is designed in a manner that the upper end is thick and the lower end is thin, so as to form the same temperature field gradient distribution (0-135 DEG C/m). Through the adoption of the preparation technology researched and developed through the combination of the structure and innovation, the single crystal ratio of the product is up to about 65%, the produced magnesium fluoride single crystal coating material can avoid the production of magnesium oxide, so that the requirement for no collapse point is met; besides, the yield of single crystal magnesium fluoride produced by the technology is 6-7 times of single-furnace yield of single crystal magnesium fluoride produced by a down-draw process, and the time is shortened by 70%.
Description
Technical field
The present invention relates to preparation facilities and the preparation technology of magnesium fluoride monocrystalline Coating Materials.
Background technology
At present, most of magnesium fluoride optical filming material mode of production mostly is hot pressed multicrystal, dissolves polycrystalline and pull-down single crystal form, and Problems existing is: although polymorphic Coating Materials output is large, price is low, quality can not reach high-end customer requirement; Although pull-down monocrystalline quality is high, require strict to working condition, therefore cause yielding poorly, price is high, finally cannot realize mass market.
Summary of the invention
For above deficiency, the object of this invention is to provide a kind of preparation facilities and preparation technology of magnesium fluoride monocrystalline Coating Materials, the monocrystalline shape magnesium fluoride of high quality, high yield can be produced at short notice.
Concrete technical scheme: the preparation facilities of magnesium fluoride monocrystalline Coating Materials, comprise crucible, graphite heating body and cooling system, wherein the top of crucible is covered with top cover, upwards caves in the place of bottom centre of crucible, cave in place's formation trapezoidal cylinder shape, is covered with bell jar in the outside of crucible; Described graphite heating body is connected with external power source by copper electrode, and the profile of graphite heating body is consistent with trapezoidal cylinder shape; Described cooling system comprises water-in and water outlet and circulation waterway, and described circulation waterway is positioned at bell jar inside.
The inwall of described bell jar is with muff, and described muff adopts the gradient design that upper end is thick, lower end is thin.
Be equipped with thermal insulation layer in the bottom of crucible, the surrounding of thermal insulation layer is provided with auxiliary heating body.
Ring-shaped platform is provided with in the bottom of crucible.
The preparation technology of magnesium fluoride monocrystalline Coating Materials, have employed described preparation facilities, adopts following steps:
1) loaded in crucible by the magnesium fluoride raw material of MgF2 content >=99.9%, top cover, puts down bell jar;
2) opening water-in and water outlet makes water coolant start circulation, and cooler-water temperature keeps≤35 DEG C;
3) open vacuum pump, crucible inside is evacuated to vacuum tightness and is greater than 5 × 10
-3pa;
4) by regulating the temperature of graphite heating body and auxiliary heating body to make the warm field gradient of preparation facilities remain on 0-135 DEG C/m, namely every meter of temperature variation is 0-135 DEG C;
5) after furnace temperature rises to 1380-1400 DEG C from room temperature, again through constant temperature, cooling, cooling, monocrystalline shape magnesium fluoride is finally obtained.
Furnace temperature is set with 3 process nodes when room temperature rises to 1380-1400 DEG C, and first process node is 440-450 DEG C, second process node 490-500 DEG C, and the 3rd process node is 890-900 DEG C.Wherein, from room temperature to the first process node, the time is 7.5-8.5h, evenly heats up; From first process node to the second process node, the time is 4-5h, evenly heats up and dewaters; From second process node to the 3rd process node, the time is 6-7h, evenly heats up and carries out deoxygenation; From the 3rd process node to target temperature 1380-1400 DEG C, the time is 11.5-12.5h, evenly heats up.
Described thermostatic process is: thermostat temperature keeps 14.5-15.5h within the scope of 1380-1400 DEG C, gets rid of gas simultaneously.
Described cooling and process of cooling set 2 process nodes altogether, and as the 4th and the 5th process node, wherein the 4th process node is 1190-1200 DEG C, and the 5th process node is 1040-1050 DEG C.Wherein, from thermostat temperature to the 4th process node, time 4.5-5.5h, uniform decrease in temperature; From the 4th process node to the 5th process node, the time is 22-24h, closes auxiliary heating body, uniform decrease in temperature; From the 5th process node to room temperature, close graphite heating body and vacuum pump, more than naturally cooling 24h.
Technique effect of the present invention: graphite heating body is designed to trapezoidal cylinder (lower base angle is 86o ± 0.5) by (1) one aspect of the present invention, form warm field gradient distribution (0-135 DEG C/m) that upper end is high, lower end is low, on the other hand bell jar inwall muff is designed to that upper end is thick, lower end is thin, make muff to form the warm field gradient distribution of (0-135 DEG C/m) equally, so just the fixing two gradient crystallization method of innovation realization prepares magnesium fluoride monocrystalline Coating Materials; (2) preparation facilities of the present invention and preparation technology is adopted, product monocrystalline rate is up to about 65%, and the magnesium fluoride monocrystalline Coating Materials of output can avoid magnesium oxide to generate, and reaches without collapsing a technical requirements, and output monocrystalline magnesium fluoride of the present invention is glass tube down-drawing list furnace output 6-7 times, time decreased 70%; (3) auxiliary heating body be provided with outside crucible, makes the material inner warm field of crucible more balanced (during single crystal growing, auxiliary heating body is closed) when heating, insulation; (4) 20x10mm ring-shaped platform being installed for collecting volatile matter at crucible bottom, being conducive to material recycle, reduce vacuum apparatus and suck too much impurity environmental pollution simultaneously.
Accompanying drawing explanation
Fig. 1 is the structural representation of magnesium fluoride monocrystalline Coating Materials preparation facilities in the present invention.
Embodiment
embodiment one
As shown in Figure 1, the preparation facilities of magnesium fluoride monocrystalline Coating Materials, comprises crucible 10, graphite heating body 9 and cooling system, wherein the top of crucible 10 is covered with top cover 11, upwards cave in the place of bottom centre of crucible 10, place of caving in forms trapezoidal cylinder shape, is covered with bell jar 1 in the outside of crucible 10; Described graphite heating body 9 is connected with external power source by copper electrode 8, and the profile of graphite heating body 9 is consistent with trapezoidal cylinder shape; Described cooling system comprises water-in 6 and water outlet 5 and circulation waterway, and it is inner that described circulation waterway is positioned at bell jar 1.The inwall of described bell jar 1 is with muff 2, and described muff 2 adopts the gradient design that upper end is thick, lower end is thin.Be equipped with thermal insulation layer 3 in the bottom of crucible 10, the surrounding of thermal insulation layer 3 is provided with auxiliary heating body 4.Ring-shaped platform 7 is provided with in the bottom of crucible 10.
The preparation technology of magnesium fluoride monocrystalline Coating Materials, have employed above-mentioned preparation facilities, adopts following steps:
1) loaded in crucible 10 by magnesium fluoride raw material, top cover 11, puts down bell jar 1;
2) opening water-in 6 and water outlet 5 makes water coolant start circulation, and cooler-water temperature keeps≤35 DEG C;
3) open vacuum pump, crucible 10 inside is evacuated to vacuum tightness and is greater than 5 × 10
-3pa, vacuum pump kind should select oil diffusion pump, best effort scope 5 × 10
-2~ 5 × 10
-4pa, pumping speed V>=70L/S;
4) by regulating the temperature of graphite heating body 9 and auxiliary heating body 4 to make the warm field gradient of preparation facilities remain on 0-135 DEG C/m;
5) after furnace temperature rises to 1380 DEG C from room temperature, again through constant temperature, cooling, cooling, monocrystalline shape magnesium fluoride is finally obtained.
Furnace temperature is set with 3 process nodes when room temperature rises to 1380 DEG C, and first process node is 440 DEG C, and second process node 490 DEG C, the 3rd process node is 890 DEG C.
From room temperature to the first process node, the time is 7.5h, evenly heats up; From first process node to the second process node, the time is 4h, evenly heats up and dewaters; From second process node to the 3rd process node, the time is 6h, evenly heats up and carries out deoxygenation; From the 3rd process node to target temperature 1380 DEG C, the time is 11.5h, evenly heats up.
Described thermostatic process is: thermostat temperature keeps 14.5h within the scope of 1380 DEG C, closes auxiliary heating body 4, gets rid of gas simultaneously.
Described cooling and process of cooling set 2 process nodes altogether, and as the 4th and the 5th process node, wherein the 4th process node is 1190 DEG C, and the 5th process node is 1040 DEG C.
From thermostat temperature to the 4th process node, time 4.5h, uniform decrease in temperature; From the 4th process node to the 5th process node, the time is 22h, closes auxiliary heating body 4, uniform decrease in temperature; From the 5th process node to room temperature, close graphite heating body 9 and vacuum pump, more than naturally cooling 24h.
embodiment two
As shown in Figure 1, the preparation facilities of magnesium fluoride monocrystalline Coating Materials, comprises crucible 10, graphite heating body 9 and cooling system, wherein the top of crucible 10 is covered with top cover 11, upwards cave in the place of bottom centre of crucible 10, place of caving in forms trapezoidal cylinder shape, is covered with bell jar 1 in the outside of crucible 10; Described graphite heating body 9 is connected with external power source by copper electrode 8, and the profile of graphite heating body 9 is consistent with trapezoidal cylinder shape; Described cooling system comprises water-in 6 and water outlet 5 and circulation waterway, and it is inner that described circulation waterway is positioned at bell jar 1.The inwall of described bell jar 1 is with muff 2, and described muff 2 adopts the gradient design that upper end is thick, lower end is thin.Be equipped with thermal insulation layer 3 in the bottom of crucible 10, the surrounding of thermal insulation layer 3 is provided with auxiliary heating body 4.Ring-shaped platform 7 is provided with in the bottom of crucible 10.
The preparation technology of magnesium fluoride monocrystalline Coating Materials, have employed above-mentioned preparation facilities, adopts following steps:
1) loaded in crucible 10 by magnesium fluoride raw material, top cover 11, puts down bell jar 1;
2) opening water-in 6 and water outlet 5 makes water coolant start circulation, and cooler-water temperature keeps≤35 DEG C;
3) open vacuum pump, crucible 10 inside is evacuated to vacuum tightness and is greater than 5 × 10
-3pa, vacuum pump kind should select oil diffusion pump, best effort scope 5 × 10
-2~ 5 × 10
-4pa, pumping speed V>=70L/S;
4) by regulating the temperature of graphite heating body 9 and auxiliary heating body 4 to make the warm field gradient of preparation facilities remain on 0-135 DEG C/m;
5) after furnace temperature rises to 1390 DEG C from room temperature, again through constant temperature, cooling, cooling, monocrystalline shape magnesium fluoride is finally obtained.
Furnace temperature is set with 3 process nodes when room temperature rises to 1390 DEG C, and first process node is 445 DEG C, and second process node 495 DEG C, the 3rd process node is 895 DEG C.
From room temperature to the first process node, the time is 8.h, evenly heats up; From first process node to the second process node, the time is 4.5h, evenly heats up and dewaters; From second process node to the 3rd process node, the time is 6.5h, evenly heats up and carries out deoxygenation; From the 3rd process node to target temperature 1390 DEG C, the time is 12h, evenly heats up.
Described thermostatic process is: thermostat temperature keeps 15.h within the scope of 1390 DEG C, closes auxiliary heating body 4, gets rid of gas simultaneously.
Described cooling and process of cooling set 2 process nodes altogether, and as the 4th and the 5th process node, wherein the 4th process node is 1195 DEG C, and the 5th process node is 1045 DEG C.
From thermostat temperature to the 4th process node, time 5.h, uniform decrease in temperature; From the 4th process node to the 5th process node, the time is 23h, closes auxiliary heating body 4, uniform decrease in temperature; From the 5th process node to room temperature, close graphite heating body 9 and vacuum pump, more than naturally cooling 24h.
embodiment three
As shown in Figure 1, the preparation facilities of magnesium fluoride monocrystalline Coating Materials, comprises crucible 10, graphite heating body 9 and cooling system, wherein the top of crucible 10 is covered with top cover 11, upwards cave in the place of bottom centre of crucible 10, place of caving in forms trapezoidal cylinder shape, is covered with bell jar 1 in the outside of crucible 10; Described graphite heating body 9 is connected with external power source by copper electrode 8, and the profile of graphite heating body 9 is consistent with trapezoidal cylinder shape; Described cooling system comprises water-in 6 and water outlet 5 and circulation waterway, and it is inner that described circulation waterway is positioned at bell jar 1.The inwall of described bell jar 1 is with muff 2, and described muff 2 adopts the gradient design that upper end is thick, lower end is thin.Be equipped with thermal insulation layer 3 in the bottom of crucible 10, the surrounding of thermal insulation layer 3 is provided with auxiliary heating body 4.Ring-shaped platform 7 is provided with in the bottom of crucible 10.
The preparation technology of magnesium fluoride monocrystalline Coating Materials, have employed above-mentioned preparation facilities, adopts following steps:
1) loaded in crucible 10 by magnesium fluoride raw material, top cover 11, puts down bell jar 1;
2) opening water-in 6 and water outlet 5 makes water coolant start circulation, and cooler-water temperature keeps≤35 DEG C;
3) open vacuum pump, crucible 10 inside is evacuated to vacuum tightness and is greater than 5 × 10
-3pa, vacuum pump kind should select oil diffusion pump, best effort scope 5 × 10
-2~ 5 × 10
-4pa, pumping speed V>=70L/S;
4) by regulating the temperature of graphite heating body 9 and auxiliary heating body 4 to make the warm field gradient of preparation facilities remain on 0-135 DEG C/m;
5) after furnace temperature rises to 1400 DEG C from room temperature, again through constant temperature, cooling, cooling, monocrystalline shape magnesium fluoride is finally obtained.
Furnace temperature is set with 3 process nodes when room temperature rises to 1400 DEG C, and first process node is 450 DEG C, and second process node 500 DEG C, the 3rd process node is 900 DEG C.
From room temperature to the first process node, the time is 8.5h, evenly heats up; From first process node to the second process node, the time is 5h, evenly heats up and dewaters; From second process node to the 3rd process node, the time is 7h, evenly heats up and carries out deoxygenation; From the 3rd process node to target temperature 1400 DEG C, the time is 12.5h, evenly heats up.
Described thermostatic process is: thermostat temperature keeps 15.5h within the scope of 1400 DEG C, closes auxiliary heating body 4, gets rid of gas simultaneously.
Described cooling and process of cooling set 2 process nodes altogether, and as the 4th and the 5th process node, wherein the 4th process node is 1200 DEG C, and the 5th process node is 1050 DEG C.
From thermostat temperature to the 4th process node, time 5.5h, uniform decrease in temperature; From the 4th process node to the 5th process node, the time is 24h, closes auxiliary heating body 4, uniform decrease in temperature; From the 5th process node to room temperature, close graphite heating body 9 and vacuum pump, more than naturally cooling 24h.
Claims (10)
1. the preparation facilities of magnesium fluoride monocrystalline Coating Materials, it is characterized in that: comprise crucible (10), graphite heating body (9) and cooling system, wherein the top of crucible (10) is covered with top cover (11), upwards cave in the place of bottom centre of crucible (10), cave in place's formation trapezoidal cylinder shape, is covered with bell jar (1) in the outside of crucible (10); Described graphite heating body (9) is connected with external power source by copper electrode (8), and the profile of graphite heating body (9) is consistent with trapezoidal cylinder shape; Described cooling system comprises water-in (6) and water outlet (5) and circulation waterway, and it is inner that described circulation waterway is positioned at bell jar (1).
2. the preparation facilities of magnesium fluoride monocrystalline Coating Materials as claimed in claim 1, is characterized in that: the inwall of described bell jar (1) is with muff (2), and described muff (2) adopts the gradient design that upper end is thick, lower end is thin.
3. the preparation facilities of magnesium fluoride monocrystalline Coating Materials as claimed in claim 1 or 2, it is characterized in that: be equipped with thermal insulation layer (3) in the bottom of crucible (10), the surrounding of thermal insulation layer (3) is provided with auxiliary heating body (4).
4. the preparation facilities of magnesium fluoride monocrystalline Coating Materials as claimed in claim 1, is characterized in that: be provided with ring-shaped platform (7) in the bottom of crucible (10).
5. the preparation technology of magnesium fluoride monocrystalline Coating Materials, have employed as arbitrary in claim 1-4 as described in preparation facilities, it is characterized in that adopt following steps:
1) loaded in crucible (10) by magnesium fluoride raw material, top cover (11), puts down bell jar (1);
2) opening water-in (6) and water outlet (5) makes water coolant start circulation, and cooler-water temperature keeps≤35 DEG C;
3) open vacuum pump, crucible (10) inside is evacuated to vacuum tightness and is greater than 5 × 10
-3pa;
4) by regulating the temperature of graphite heating body (9) and auxiliary heating body (4) to make the warm field gradient of preparation facilities remain on 0-135 DEG C/m;
5) after furnace temperature rises to 1380-1400 DEG C from room temperature, again through constant temperature, cooling, cooling, monocrystalline shape magnesium fluoride is finally obtained.
6. the preparation technology of magnesium fluoride monocrystalline Coating Materials as claimed in claim 5, it is characterized in that: furnace temperature is set with 3 process nodes when room temperature rises to 1380-1400 DEG C, first process node is 440-450 DEG C, second process node 490-500 DEG C, the 3rd process node is 890-900 DEG C.
7. the preparation technology of magnesium fluoride monocrystalline Coating Materials as claimed in claim 6, is characterized in that: from room temperature to the first process node, the time is 7.5-8.5h, evenly heats up; From first process node to the second process node, the time is 4-5h, evenly heats up and dewaters; From second process node to the 3rd process node, the time is 6-7h, evenly heats up and carries out deoxygenation; From the 3rd process node to target temperature 1380-1400 DEG C, the time is 11.5-12.5h, evenly heats up.
8. the preparation technology of magnesium fluoride monocrystalline Coating Materials as claimed in claim 5, is characterized in that described thermostatic process is: thermostat temperature keeps 14.5-15.5h within the scope of 1380-1400 DEG C, closes auxiliary heating body (4), gets rid of gas simultaneously.
9. the preparation technology of magnesium fluoride monocrystalline Coating Materials as claimed in claim 5, it is characterized in that: described cooling and process of cooling set 2 process nodes altogether, as the 4th and the 5th process node, wherein the 4th process node is 1190-1200 DEG C, and the 5th process node is 1040-1050 DEG C.
10. the preparation technology of magnesium fluoride monocrystalline Coating Materials as claimed in claim 8 or 9, is characterized in that: from thermostat temperature to the 4th process node, time 4.5-5.5h, uniform decrease in temperature; From the 4th process node to the 5th process node, the time is 22-24h, closes auxiliary heating body (4), uniform decrease in temperature; From the 5th process node to room temperature, close graphite heating body (9) and vacuum pump, more than naturally cooling 24h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093660A (en) * | 2019-05-18 | 2019-08-06 | 惠磊光电科技(上海)有限公司 | It is a kind of can be with the grower and technique of high-speed rapid growth bubble-free crystalline material |
| RU2765962C1 (en) * | 2021-08-20 | 2022-02-07 | федеральное государственное автономное образовательное учреждение высшего образования «Казанский (Приволжский) федеральный университет» (ФГАОУ ВО КФУ) | Method of forming a temperature gradient in a thermal unit of a furnace for growing fluoride crystals and a device for its implementation |
| CN115852484A (en) * | 2023-02-27 | 2023-03-28 | 杭州天桴光电技术有限公司 | Device and method for efficiently preparing magnesium fluoride polycrystalline optical coating material |
| CN115852483A (en) * | 2023-02-27 | 2023-03-28 | 杭州天桴光电技术有限公司 | Device and method for preparing round cake-shaped magnesium fluoride crystal coating material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110093660A (en) * | 2019-05-18 | 2019-08-06 | 惠磊光电科技(上海)有限公司 | It is a kind of can be with the grower and technique of high-speed rapid growth bubble-free crystalline material |
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| RU2765962C1 (en) * | 2021-08-20 | 2022-02-07 | федеральное государственное автономное образовательное учреждение высшего образования «Казанский (Приволжский) федеральный университет» (ФГАОУ ВО КФУ) | Method of forming a temperature gradient in a thermal unit of a furnace for growing fluoride crystals and a device for its implementation |
| CN115852484A (en) * | 2023-02-27 | 2023-03-28 | 杭州天桴光电技术有限公司 | Device and method for efficiently preparing magnesium fluoride polycrystalline optical coating material |
| CN115852483A (en) * | 2023-02-27 | 2023-03-28 | 杭州天桴光电技术有限公司 | Device and method for preparing round cake-shaped magnesium fluoride crystal coating material |
| CN115852483B (en) * | 2023-02-27 | 2023-05-16 | 杭州天桴光电技术有限公司 | Device and method for preparing cake-shaped magnesium fluoride crystal coating material |
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