CN103060901A - Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method - Google Patents

Preparation process for growing plurality of crystals through edge-defined film-fed crystal growth method Download PDF

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CN103060901A
CN103060901A CN2013100454226A CN201310045422A CN103060901A CN 103060901 A CN103060901 A CN 103060901A CN 2013100454226 A CN2013100454226 A CN 2013100454226A CN 201310045422 A CN201310045422 A CN 201310045422A CN 103060901 A CN103060901 A CN 103060901A
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heating element
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gradient
crystal
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CN103060901B (en
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王静
秦冒晓
黄小卫
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Baoshan Xinlong Electronic Technology Co ltd
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UNIONLIGHT TECHNOLOGY Co Ltd
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Abstract

The invention relates to a preparation process for growing a plurality of crystals through an edge-defined film-fed crystal growth method, which comprises the following steps of: (1) placing a raw material into a crucible of a single crystal growth furnace, and vacuumizing; (2) providing a heating body for a high-temperature environment in the single crystal growth furnace, electrifying and heating until to 100-200 DEG C below the melting point of the raw material, maintaining the temperature, providing a heating body for an upper growth gradient and providing a heating body for a lower growth gradient, increasing the temperature until to 100-300 DEG C above the melting temperature of the raw material, and melting the raw material into a melt; (3) seeding; (4) necking; (5) shouldering; (6) pulling seed crystals, so as to grow multiple crystals with a constant diameter; and (7) stopping pulling until the multiple crystals are completely removed away from the upper surface of a mould under seed crystal pulling, controlling the temperature gradient in the single crystal growth furnace as zero, maintaining a constant temperature, decreasing to room temperature, so as to stop the growth of a chip, thereby obtaining the multiple crystals. The preparation process for growing the plurality of crystals through the edge-defined film-fed crystal growth method disclosed by the invention can simultaneously and independently control the growths of multiple crystals.

Description

The preparation technology of many crystal of guided mode method growth
Technical field
The present invention relates to a kind of preparation technology of crystal, the preparation technology of many crystal of especially a kind of guided mode method growth.
Background technology
The guided mode method is one of method of manually producing from melt monocrystal material, and namely " edge limited film feed growth " technology is called for short the EFG method, the crystal of the specified shape that is mainly used in growing, and in fact it is a kind of distortion of crystal pulling method.The guided mode method is because the crystal such as slice, silk, pipe, rod, plate of directly growing from melt, and crystalline growth velocity is fast, size can accurately be controlled, greatly simplified the work program of crystal, material, time and resource have been saved, reduce production costs, increase economic efficiency, thereby be subject to people's attention.
The principle of work of guided mode method is that raw material is put into the crucible heating and melting, melt rises to die tip along a mould under wicking action, connect the seed crystal lifting melt at the mould top liquid level, make on the interface of seed crystal and melt and constantly carry out rearranging of atom or molecule, solidify gradually and grow the single crystal identical with the die edge shape with cooling.
The speed of growth is one of principal element that affects EFG method crystal mass, if the speed of growth is too high, it is cellular that growth interface can become, and has a large amount of pores or cavity in the crystal, and dislocation desity also will increase.Many crystal of actual growth carry out the seeding growth to multi-mould simultaneously by a seed crystal, often owing to poor synchronization, and cause the crystal orientation of each bar crystal to differ, radial symmetry gradient is inhomogeneous, cause crystal dislocation density high even form crystal boundary, and with larger stress, crystal mass is very undesirable.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the preparation technology of many crystal of a kind of guided mode method growth is provided, reach independently control when can realize many crystal growths.
According to technical scheme provided by the invention, the preparation technology of many crystal of a kind of guided mode method growth, feature is may further comprise the steps:
(1) raw material is packed in the crucible in the monocrystal growing furnace, monocrystal growing furnace is vacuumized, the vacuum tightness in the control monocrystal growing furnace is 1.0 * 10 -3~ 1.0 * 10 -4Pa;
(2) provide heating element, upper growth gradient to provide heating element, lower growth gradient to provide the heating element energising to heat to the hot environment in the monocrystal growing furnace, heat-up rate is 7 ~ 20 ℃/minute; When treating that temperature reaches following 100 ~ 200 ℃ of raw material fusing point, keep hot environment that the temperature of heating element is provided; Provide heating element and lower growth gradient to provide heating element to continue to heat up to upper growth gradient, it is 1 ~ 3 ℃/minute that upper growth gradient provides the heat-up rate of heating element, lower growth gradient provides 2 ~ 7 ℃/minute of the heat-up rates of heating element, is warming up to above 100 ~ 300 ℃ of the fusing point of raw material; Raw material in the crucible is fused into melt, constant temperature 1 ~ 2 hour;
(3) seeding: 3 ~ 5 millimeters places, top that the seed crystal of lifting rod lower end is suspended from every group of mould in the crucible simultaneously bake brilliant, roasting brilliant 30~60 minutes; Behind the roasting crystalline substance seed crystal is dropped on each mould, make the face of weld of seed crystal and the abundant welding of melt on each mould upper surface, realize the seeding of many wafers;
(4) necking down: behind the seeding, seed crystal lifts with 20~60 millimeters/hour speed respectively, and necking down length is finished necking down after 15 ~ 20 millimeters;
(5) expand shoulder: expand shoulder after necking down is finished, expanding the fillet degree is 120 degree, and the rate of pulling is 0~10 millimeter/hour, expands to finish behind 15 ~ 30 millimeters of the shoulder length degree and expands shoulder; The upper growth gradient of cooling rate reduction with 0.5 ~ 1 ℃/minute when expanding shoulder provides heating element and lower growth gradient that the temperature of heating element is provided;
(6) behind the expansion shoulder, lift seed crystal, make many crystal carry out isodiametric growth, in the isodiametric growth process, the rate of pulling is 10~50 millimeters/hour, provides heating element and lower growth gradient that the temperature of heating element is provided with growth gradient in 0.1 ~ 0.6 ℃/minute the cooling rate reduction simultaneously;
(7) until many crystal under the seed crystal lifting fully behind the upper surface of break away from moulds, stop to lift, reducing respectively upper growth gradient with 3 ~ 9 ℃/minute cooling rates provides heating element and lower growth gradient that the temperature of heating element is provided, the temperature that makes growth gradient provide heating element, lower growth gradient that heating element is provided provides the temperature of heating element consistent with hot environment, be that thermograde in the monocrystal growing furnace is zero, and constant temperature 1 ~ 2 hour; Then reducing hot environment with 1 ~ 6 ℃/minute cooling rate provides heating element, upper growth gradient to provide heating element, lower growth gradient that the temperature of heating element is provided, and is cooled to room temperature, and the growth of wafer finishes, and namely obtains many crystal.
In described step (3)~(7), the seed crystal on every group of mould is adjusted respectively the rate of pulling independently, to guarantee the crystal synchronous growth on every group the mould.
Preparation technology of the present invention is in crystal growth and operation, reach independently control when can realize many crystal growths, especially, if unusual phenomenon appears in certain one or more groups mould in crystal growing process, can unusually carry out independent, micro-growth regulating for this group by control device; Both replace conventional guided mode method monolithic growth pattern, improved production efficiency, guaranteed again the synchronism of guided mode fado bar crystal growth, improved crystal mass, reduced energy consumption, saved cost.
Description of drawings
Fig. 1 is the structural representation of growing apparatus of the present invention.
Embodiment
The invention will be further described below in conjunction with concrete accompanying drawing.
As shown in Figure 1: the growing apparatus of many crystal of described guided mode method growth comprises monocrystal growing furnace 1, vacuum extractor 2, crucible bracket 3, crucible 4, heat-preservation cylinder 5, upper stay-warm case 6, lower stay-warm case 7, tubular hot environment provide heating element 8, upper growth gradient to provide heating element 9, lower growth gradient that heating element 10, mould 11, lifting rod 12, control device 13 etc. are provided all around.
As shown in Figure 1, the present invention includes monocrystal growing furnace 1, the furnace chamber of monocrystal growing furnace 1 is connected with vacuum extractor 2, the furnace chamber bottom of monocrystal growing furnace 1 is provided with crucible bracket 3, crucible 4 is set on the crucible bracket 3, heat-preservation cylinder 5 around the outside of crucible 4 is provided with, the top of heat-preservation cylinder 5 arranges stay-warm case 6 all around, the bottom of heat-preservation cylinder 5 arranges lower stay-warm case 7 all around, crucible 4 and all around heat-preservation cylinder 5 between the tubular hot environment is set heating element 8 is provided, be provided with growth gradient at upper stay-warm case 6 heating element 9 is provided, be provided with lower growth gradient at lower stay-warm case 7 heating element 10 is provided, upper growth gradient provides heating element 9 and lower growth gradient to provide heating element 10 to lay respectively at the upper and lower of crucible 4; Be installed with many group moulds 11 in described crucible 4 inside, every group of mould 11 upsides are provided with the lifting rod 12 that can stretch up and down and rotate, and the bottom of lifting rod 12 is provided with seed crystal; Described lifting rod 12 is connected with control device 13, and control device 13 is used for each lifting rod 12 of control and lifts up and down independently respectively and spinning movement;
Described tubular hot environment provide heating element 8, upper growth gradient provide heating element 9, lower growth gradient provide heating element 10 all with crucible 4 coaxial settings;
Described vacuum extractor 2 is vacuum pump etc., the equipment that can vacuumize the furnace chamber of monocrystal growing furnace 1.
Principle of work of the present invention and working process: as shown in Figure 1, in crystal growth and operation, described control device 13 can be controlled lifting rod 12 at the same time or separately, when can realize the growth of many crystal and independent control, guarantees the synchronism that many crystal are grown.
Embodiment one: the preparation technology of many crystal of a kind of guided mode method growth may further comprise the steps:
(1) with purity is high purity aluminium oxide (Al more than 99.999% 2O 3) the powder piece packs into after drying in high temperature oxidation atmosphere in the crucible in the monocrystal growing furnace, and monocrystal growing furnace is vacuumized, the vacuum tightness in the control monocrystal growing furnace is 1.0 * 10 -3Pa;
(2) provide heating element, lower growth gradient to provide heating element and hot environment to provide the heating element cleaning clean monocrystal growing furnace and inner upper growth gradient, to burn and stay-warm case after dust removal process, crucible, mould etc. are placed in the monocrystal growing furnace through high temperature is empty, level is put in requirement, can not occur tilting, and guarantee with one heart; Proofread and correct lifting rod, seed crystal is connected on the lifting rod, and adjusting makes the face of weld of every group of seed crystal perpendicular to the middle of the mould of its below simultaneously;
(3) provide heating element, upper growth gradient to provide heating element, lower growth gradient to provide the heating element energising to heat to the hot environment in the monocrystal growing furnace, heat-up rate is 7 ℃/minute; When treating that temperature reaches 1950 ℃, keep hot environment that the temperature of heating element is provided; Provide heating element and lower growth gradient to provide heating element continue to heat up to upper growth gradient, it is 1 ℃/minute that upper growth gradient provides the heat-up rate of heating element, and lower growth gradient provides 2 ℃/minute of the heat-up rates of heating element, is warming up to 2150 ℃; Raw material in the crucible is fused into melt, constant temperature 1 hour;
(4) seeding: 3 millimeters places, top that the seed crystal of lifting rod lower end is suspended from every group of mould in the crucible simultaneously bake brilliant, roasting brilliant 30 minutes; Behind the roasting crystalline substance seed crystal is dropped on each mould, make the face of weld of seed crystal and the abundant welding of melt on each mould upper surface, realize the seeding of many wafers; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(5) necking down: behind the seeding, seed crystal lifts with 20 millimeters/hour speed respectively, and necking down length is finished necking down after 15 millimeters; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal normal growth on every group the mould;
(6) expand shoulder: expand shoulder after necking down is finished, expanding the fillet degree is 120 degree, expands to finish behind 15 millimeters of the shoulder length degree and expands shoulder; The upper growth gradient of cooling rate reduction with 0.1 ℃/minute when expanding shoulder provides heating element and lower growth gradient that the temperature of heating element is provided; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(7) behind the expansion shoulder, lift seed crystal, make many crystal carry out isodiametric growth, in the isodiametric growth process, the rate of pulling is 10 millimeters/hour, provides heating element and lower growth gradient that the temperature of heating element is provided with growth gradient in 0.1 ℃/minute the cooling rate reduction simultaneously; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(8) until many crystal at the complete upper surface of break away from moulds approximately after 3 millimeters under the seed crystal lifting, stop to lift, reduce upper growth gradient with 6 ℃/minute cooling rates heating element is provided, reduce the temperature that lower growth gradient provides heating element with 9 ℃/minute cooling rates, make growth gradient that heating element is provided, lower growth gradient provides the temperature of heating element to provide the temperature of heating element consistent with hot environment, be that the interior thermograde of monocrystal growing furnace is zero (even upper growth gradient provides heating element, the temperature that lower growth gradient provides heating element and hot environment that heating element is provided is 1950 ℃), and constant temperature 1 hour; Then reducing hot environment with 1 ℃/minute cooling rate provides heating element, upper growth gradient to provide heating element, lower growth gradient that the temperature of heating element is provided, and is cooled to room temperature, and the growth of wafer finishes, and namely obtains many sapphire crystals; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould.
Embodiment two: the preparation technology of many crystal of a kind of guided mode method growth may further comprise the steps:
(1) with purity is high purity aluminium oxide (Al more than 99.999% 2O 3) the powder piece packs into after drying in high temperature oxidation atmosphere in the crucible in the monocrystal growing furnace, and monocrystal growing furnace is vacuumized, the vacuum tightness in the control monocrystal growing furnace is 1.0 * 10 -4Pa;
(2) provide heating element, lower growth gradient to provide heating element and hot environment to provide the heating element cleaning clean monocrystal growing furnace and inner upper growth gradient, to burn and stay-warm case after dust removal process, crucible, mould etc. are placed in the monocrystal growing furnace through high temperature is empty, level is put in requirement, can not occur tilting, and guarantee with one heart; Proofread and correct lifting rod, seed crystal is connected on the lifting rod, and adjusting makes the face of weld of every group of seed crystal perpendicular to the middle of the mould of its below simultaneously;
(3) provide heating element, upper growth gradient to provide heating element, lower growth gradient to provide the heating element energising to heat to the hot environment in the monocrystal growing furnace, heat-up rate is 20 ℃/minute; When treating that temperature reaches 1850 ℃, and keep hot environment that the temperature of heating element is provided; Provide heating element and lower growth gradient to provide heating element continue to heat up to upper growth gradient, it is 3 ℃/minute that upper growth gradient provides the heat-up rate of heating element, and lower growth gradient provides 7 ℃/minute of the heat-up rates of heating element, is warming up to 2350 ℃; Raw material in the crucible is fused into melt, constant temperature 2 hours;
(4) seeding: 5 millimeters places, top that the seed crystal of lifting rod lower end is suspended from every group of mould in the crucible simultaneously bake brilliant, roasting brilliant 60 minutes; Behind the roasting crystalline substance seed crystal is dropped on each mould, make the face of weld of seed crystal and the abundant welding of melt on each mould upper surface, realize the seeding of many wafers; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(5) necking down: behind the seeding, seed crystal lifts with 60 millimeters/hour speed respectively, and necking down length is finished necking down after 20 millimeters; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal normal growth on every group the mould;
(6) expand shoulder: expand shoulder after necking down is finished, expanding the fillet degree is 120 degree, and the rate of pulling is 10 millimeters/hour, expands to finish behind 30 millimeters of the shoulder length degree and expands shoulder; The upper growth gradient of cooling rate reduction with 1 ℃/minute when expanding shoulder provides heating element and lower growth gradient that the temperature of heating element is provided; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(7) behind the expansion shoulder, lift seed crystal, make many crystal carry out isodiametric growth, in the isodiametric growth process, the rate of pulling is 50 millimeters/hour, provides heating element and lower growth gradient that the temperature of heating element is provided with growth gradient in 0.6 ℃/minute the cooling rate reduction simultaneously; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(8) until many crystal at the complete upper surface of break away from moulds approximately after 3 millimeters under the seed crystal lifting, stop to lift, reduce upper growth gradient with 4 ℃/minute cooling rates heating element is provided, reduce the temperature that lower growth gradient provides heating element with 7 ℃/minute cooling rates, make growth gradient that heating element is provided, lower growth gradient provides the temperature of heating element to provide the temperature of heating element consistent with hot environment, be that the interior thermograde of monocrystal growing furnace is zero (even upper growth gradient provides heating element, the temperature that lower growth gradient provides heating element and hot environment that heating element is provided is 1850 ℃), and constant temperature 2 hours; Then reducing hot environment with 6 ℃/minute cooling rate provides heating element, upper growth gradient to provide heating element, lower growth gradient that the temperature of heating element is provided, and is cooled to room temperature, and the growth of wafer finishes, and namely obtains many sapphire crystals; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould.
Embodiment three: the preparation technology of many crystal of a kind of guided mode method growth may further comprise the steps:
(1) with purity is high purity aluminium oxide (Al more than 99.999% 2O 3) the powder piece packs into after drying in high temperature oxidation atmosphere in the crucible in the monocrystal growing furnace, and monocrystal growing furnace is vacuumized, the vacuum tightness in the control monocrystal growing furnace is 5 * 10 -4Pa;
(2) provide heating element, lower growth gradient to provide heating element and hot environment to provide the heating element cleaning clean monocrystal growing furnace and inner upper growth gradient, to burn and stay-warm case after dust removal process, crucible, mould etc. are placed in the monocrystal growing furnace through high temperature is empty, level is put in requirement, can not occur tilting, and guarantee with one heart; Proofread and correct lifting rod, seed crystal is connected on the lifting rod, and adjusting makes the face of weld of every group of seed crystal perpendicular to the middle of the mould of its below simultaneously;
(3) provide heating element, upper growth gradient to provide heating element, lower growth gradient to provide the heating element energising to heat to the hot environment in the monocrystal growing furnace, heat-up rate is 10 ℃/minute; When treating that temperature reaches 1900 ℃, and keep hot environment that the temperature of heating element is provided; Provide heating element and lower growth gradient to provide heating element continue to heat up to upper growth gradient, it is 2 ℃/minute that upper growth gradient provides the heat-up rate of heating element, and lower growth gradient provides 5 ℃/minute of the heat-up rates of heating element, is warming up to 2250 ℃; Raw material in the crucible is fused into melt, constant temperature 1.5 hours;
(4) seeding: 4 millimeters places, top that the seed crystal of lifting rod lower end is suspended from every group of mould in the crucible simultaneously bake brilliant, roasting brilliant 50 minutes; Behind the roasting crystalline substance seed crystal is dropped on each mould, make the face of weld of seed crystal and the abundant welding of melt on each mould upper surface, realize the seeding of many wafers; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(5) necking down: behind the seeding, seed crystal lifts with 30 millimeters/hour speed respectively, and necking down length is finished necking down after 16 millimeters; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal normal growth on every group the mould;
(6) expand shoulder: expand shoulder after necking down is finished, expanding the fillet degree is 120 degree, and the rate of pulling is 5 millimeters/hour, expands to finish behind 20 millimeters of the shoulder length degree and expands shoulder; The upper growth gradient of cooling rate reduction with 0.6 ℃/minute when expanding shoulder provides heating element and lower growth gradient that the temperature of heating element is provided; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(7) behind the expansion shoulder, lift seed crystal, make many crystal carry out isodiametric growth, in the isodiametric growth process, the rate of pulling is 20 millimeters/hour, provides heating element and lower growth gradient that the temperature of heating element is provided with growth gradient in 0.2 ℃/minute the cooling rate reduction simultaneously; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould;
(8) until many crystal at the complete upper surface of break away from moulds approximately after 3 millimeters under the seed crystal lifting, stop to lift, reduce upper growth gradient with 3 ℃/minute cooling rates heating element is provided, reduce the temperature that lower growth gradient provides heating element with 6 ℃/minute cooling rates, make growth gradient that heating element is provided, lower growth gradient provides the temperature of heating element to provide the temperature of heating element consistent with hot environment, be that the interior thermograde of monocrystal growing furnace is zero (even upper growth gradient provides heating element, the temperature that lower growth gradient provides heating element and hot environment that heating element is provided is following 1900 ℃ of raw material fusing point), and constant temperature 1.5 hours; Then reducing hot environment with 3 ℃/minute cooling rate provides heating element, upper growth gradient to provide heating element, lower growth gradient that the temperature of heating element is provided, and is cooled to room temperature, and the growth of wafer finishes, and namely obtains many sapphire crystals; Can adjust independently respectively the rate of pulling to the seed crystal on every group of mould in this step, to guarantee the crystal synchronous growth on every group the mould.

Claims (2)

1. the preparation technology of many crystal of a guided mode method growth is characterized in that, may further comprise the steps:
(1) raw material is packed in the crucible in the monocrystal growing furnace, monocrystal growing furnace is vacuumized, the vacuum tightness in the control monocrystal growing furnace is 1.0 * 10 -3~ 1.0 * 10 -4Pa;
(2) provide heating element, upper growth gradient to provide heating element, lower growth gradient to provide the heating element energising to heat to the hot environment in the monocrystal growing furnace, heat-up rate is 7 ~ 20 ℃/minute; When treating that temperature reaches following 100 ~ 200 ℃ of raw material fusing point, keep hot environment that the temperature of heating element is provided; Provide heating element and lower growth gradient to provide heating element to continue to heat up to upper growth gradient, it is 1 ~ 3 ℃/minute that upper growth gradient provides the heat-up rate of heating element, lower growth gradient provides 2 ~ 7 ℃/minute of the heat-up rates of heating element, is warming up to above 100 ~ 300 ℃ of the fusing point of raw material; Raw material in the crucible is fused into melt, constant temperature 1 ~ 2 hour;
(3) seeding: 3 ~ 5 millimeters places, top that the seed crystal of lifting rod lower end is suspended from every group of mould in the crucible simultaneously bake brilliant, roasting brilliant 30~60 minutes; Behind the roasting crystalline substance seed crystal is dropped on each mould, make the face of weld of seed crystal and the abundant welding of melt on each mould upper surface, realize the seeding of many wafers;
(4) necking down: behind the seeding, seed crystal lifts with 20~60 millimeters/hour speed respectively, and necking down length is finished necking down after 15 ~ 20 millimeters;
(5) expand shoulder: expand shoulder after necking down is finished, expanding the fillet degree is 120 degree, and the rate of pulling is 0~10 millimeter/hour, expands to finish behind 15 ~ 30 millimeters of the shoulder length degree and expands shoulder; The upper growth gradient of cooling rate reduction with 0.5 ~ 1 ℃/minute when expanding shoulder provides heating element and lower growth gradient that the temperature of heating element is provided;
(6) behind the expansion shoulder, lift seed crystal, make many crystal carry out isodiametric growth, in the isodiametric growth process, the rate of pulling is 10~50 millimeters/hour, provides heating element and lower growth gradient that the temperature of heating element is provided with growth gradient in 0.1 ~ 0.6 ℃/minute the cooling rate reduction simultaneously;
(7) until many crystal under the seed crystal lifting fully behind the upper surface of break away from moulds, stop to lift, reducing respectively upper growth gradient with 3 ~ 9 ℃/minute cooling rates provides heating element and lower growth gradient that the temperature of heating element is provided, the temperature that makes growth gradient provide heating element, lower growth gradient that heating element is provided provides the temperature of heating element consistent with hot environment, be that thermograde in the monocrystal growing furnace is zero, and constant temperature 1 ~ 2 hour; Then reducing hot environment with 1 ~ 6 ℃/minute cooling rate provides heating element, upper growth gradient to provide heating element, lower growth gradient that the temperature of heating element is provided, and is cooled to room temperature, and the growth of wafer finishes, and namely obtains many crystal.
2. the growing apparatus of many crystal of guided mode method as claimed in claim 1 growth is characterized in that: in described step (3)~(7), the seed crystal on every group of mould is adjusted respectively the rate of pulling independently, to guarantee the crystal synchronous growth on every group the mould.
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CN103806091A (en) * 2014-02-26 2014-05-21 闽能光电集团有限公司 Automatic control method for sapphire crystals in edge-defined film-fed growth
CN104047049A (en) * 2014-06-30 2014-09-17 南京航空航天大学 Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process
CN104264214A (en) * 2014-09-30 2015-01-07 元亮科技有限公司 Growing device and growing process for growing of terbium gallium garnet crystals by virtue of guided mode method
CN106480494A (en) * 2016-10-13 2017-03-08 中国工程物理研究院化工材料研究所 Condense necking down device and the necking method of the seed crystal of crystal growth for horizontal gradient
CN106498488A (en) * 2016-10-28 2017-03-15 同济大学 Multiple doping CaF are grown simultaneously2The device of crystal and the preparation method based on the device
CN106702481A (en) * 2017-03-20 2017-05-24 宁夏佳晶科技有限公司 Improved multi-flake guide-die artificial sapphire preparation technology
CN107059114A (en) * 2017-03-08 2017-08-18 同济大学 The mould and method of a kind of EFG technique growth crystal optical fibre
CN108570707A (en) * 2017-03-09 2018-09-25 中科钢研节能科技有限公司 EFG technique sapphire crystallization system
CN109576778A (en) * 2018-12-25 2019-04-05 内蒙古中环光伏材料有限公司 A method of reducing the impurity content that CZ method prepares monocrystalline
CN111172588A (en) * 2020-01-20 2020-05-19 江苏双良新能源装备有限公司 Seeding and drawing method for growing large-surface band-shaped silicon

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