CN105568369A - Crystal feeding method for Czochralski method crystal growth and automatic crystal feeding equipment - Google Patents
Crystal feeding method for Czochralski method crystal growth and automatic crystal feeding equipment Download PDFInfo
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- CN105568369A CN105568369A CN201610054686.1A CN201610054686A CN105568369A CN 105568369 A CN105568369 A CN 105568369A CN 201610054686 A CN201610054686 A CN 201610054686A CN 105568369 A CN105568369 A CN 105568369A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a crystal feeding method for Czochralski method crystal growth. The crystal feeding method includes the steps that a crucible is heated, and crystal materials located in the crucible are melted; seed crystals are slowly moved down; when the mass of the seed crystals is changed, the seed crystals continue to be slowly moved down to reach the crystal feeding depth; the mass increase or decrease speed of the seed crystals is monitored, when the mass increase or decrease speed range of the seed crystals is within a threshold value V, the crucible is kept in an original heating state, when the mass increase or decrease speed range of the seed crystals exceeds the threshold value V, the temperature of the crucible is increased or decreased, then the seed crystals are moved up, and crystal feeding is conducted again. According to the crystal feeding method, heat impact caused to the seed crystals by the temperature gradient of a heat insulation system in the crystal feeding process is avoided, and when the phenomena of seed crystal growth overspeed and seed crystal melting happen, crystal descending operation is conducted again by adjusting the crystal feeding temperature. The invention further provides automatic crystal feeding equipment. A control device of the equipment controls the crystal growth process to be automatically conducted, full-automatic crystal feeding is achieved, and manpower is avoided during crystal feeding operation.
Description
Technical field
The present invention relates to method of crystal growth by crystal pulling field, particularly relate to a kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment.
Background technology
Lower crystalline substance operation is the committed step determining quality in crystal growing process.In prior art, the equipment for Czochralski grown crystal is mainly artificial hand and turns down crystal type and automatic lower brilliant function device.Manually lower brilliant major defect is, easily causes the most advanced and sophisticated dislocation accumulation of seed crystal, even seed crystal cracking.And automatic lower brilliant equipment, utilize motor evenly slowly to move down seed crystal and complete lower crystalline substance operation.But, although solve seed temperature in operational process to change too fast problem, but still cannot judge that whether lower crystalline substance is successful.Whether lower crystalline substance success, and the judgement of the faint in the melt changing conditions of seed crystal, all adopts the method for observation " seed crystal aperture " in industry.The main drawback of this method is exactly highly rely on artificial experience, and the observation of different lower brilliant slip-stick artist may obtain diverse judged result.And in the crystal that fusing point is lower, aperture not obvious being even difficult to finds, this just loses the foundation judging that seed crystal changes completely.
Further, when after the lower brilliant success of judgement, just start to enter " necking down stage ", the time length shorter (0.5-2 hour) of this one-phase is also often defined as a part for lower brilliant process.And existing operation, according to human eye viewed seed crystal " aperture " changing conditions lift seed crystal, or adopt fixing necking method, ignore seed crystal changing conditions, specify a set of constant necking down flow process.This just loses the meaning of necking operation completely, often causes " shouldering " overlong time, or does not reach elimination growth interface dislocation object completely.
Thus, lower crystalline substance operation of the prior art, relies on artificial experience completely, adopts the method for observing " seed crystal aperture ", fundamentally cannot solve and how judge lower brilliant success or failure problem.
Summary of the invention
The object of the invention is to overcome shortcoming and defect of the prior art, a kind of lower crystal method for method of crystal growth by crystal pulling is provided.
The present invention is achieved by the following technical solutions: a kind of lower crystal method for method of crystal growth by crystal pulling, comprises the following steps:
(1) to crucible heating, the crystalline material fusing being positioned at crucible is made;
(2) slowly seed crystal is moved down;
(3) when seed crystal quality changes, continue slowly to move down to reach the lower brilliant degree of depth;
(4) monitor seed crystal quality speed of increasing and decrease, when seed crystal quality speed of increasing and decrease scope is in threshold value V, original heated condition is kept to crucible; Exceed threshold value V when seed crystal quality increases or reduces velocity range, raise or reduce the temperature of crucible, then, move seed crystal, perform step (2), again lower brilliant.
Relative to prior art, lower crystal method of the present invention, avoids causing thermal shocking by the thermograde of heat-insulation system to seed crystal in lower brilliant process, when occur seeded growth overrun and seed crystal melting phenomenon time by adjusting lower brilliant temperature, lower brilliant operation again; The speed that can increase according to seed crystal quality or reduce judges lower brilliant success or failure.
Further, described lower crystal method also comprises step (5), according to the speed of seed crystal quality change, selects intensification necking down or constant temperature necking down.
Further, advancing the speed when seed crystal quality is 0.5 ~-2g/h, selects constant temperature necking down; When seed crystal quality is advanced the speed more than 0.5g/h, select intensification necking down.
Further, the speed moving down seed crystal is 100 ~ 150mm/h.
Further, the described lower brilliant degree of depth is 0.5 ~ 1mm.
Present invention also offers a kind of automatically lower brilliant equipment for method of crystal growth by crystal pulling, comprise body of heater, crucible, seed rod, heating unit, upper weight sensor and/or lower weight sensor, control device; Described crucible is arranged in the furnace chamber of body of heater; Described heating unit to be arranged in described furnace chamber and to described crucible heating; Described upper weight sensor is arranged on seed rod and/or described lower weight sensor is arranged at crucible bottom; Described control device is electrically connected with described seed rod, heating unit, upper weight sensor and/or lower weight sensor respectively; Described control device monitoring seed crystal quality speed of increasing and decrease, and control heating unit according to the speed of increasing and decrease of seed crystal and move on the heating of crucible and seed rod, move down or rotate.
Relative to prior art, automatically lower brilliant equipment for method of crystal growth by crystal pulling of the present invention, automatically carrying out of crystal growing process is controlled by control device, and the lower brilliant temperature of adjustment can be judged according to process brilliant under reality, realize full-automatic lower brilliant process, make lower crystalline substance operation depart from artificial, avoid artificial interference.
Further, described control device comprises temperature control module, monitoring module and lift rotation control module; Described lift rotates control module and is electrically connected with temperature control module and monitoring module respectively; Described temperature control module is electrically connected with heating unit, and described monitoring module is electrically connected with upper weight sensor and/or lower weight sensor respectively, and described lift rotates control module and is electrically connected with seed rod; Described temperature control module is measured crucible temperature in real time and is controlled heating unit according to the temperature that crucible is measured; Crystal weight in seed weight and/or crucible on described monitoring module monitoring seed rod; Described lift to rotate on crucible temperature that control module obtains according to temperature control module and the seed rod that monitoring module obtains crystal weight in seed weight and/or crucible, regulates the speed of seed rod lift or rotation.
Further, also comprise one to link the grating scale arranged with seed rod.
Further, described control device monitoring seed crystal quality speed of increasing and decrease, when seed crystal quality speed of increasing and decrease scope is in threshold value V, keeps original heated condition to crucible; Exceed threshold value V when seed crystal quality increases or reduces velocity range, raise or reduce the temperature of crucible, then, move seed crystal, again lower brilliant.
Further, described seed rod drives the speed that moves down of seed crystal to be 100 ~ 150mm/h.
In order to understand better and implement, describe the present invention in detail below in conjunction with accompanying drawing.
Accompanying drawing explanation
Fig. 1 is the block diagram of the present invention for the lower crystal method of method of crystal growth by crystal pulling.
Fig. 2 is the time dependent curve of quality change of lower seed crystal in brilliant process under the present invention.
Fig. 3 is the connection diagram of each module of control device of brilliant equipment under the present invention automatically.
Embodiment
Lower crystal method for method of crystal growth by crystal pulling of the present invention, select suitable lower brilliant opportunity by the temperature of crucible and the state of seed crystal quality change of monitoring splendid attire crystalline material, refer to Fig. 1, specifically comprise the following steps:
(1) to crucible heating, the crystalline material fusing being positioned at crucible is made;
(2) slowly seed crystal is moved down;
Concrete, the speed moving down seed crystal is selected as required.Working efficiency can be affected when moving down seed crystal and crossing slow; Too fast when moving down seed crystal, thermal shocking can be produced to seed crystal, damage is caused to seed crystal.In the present embodiment, the speed moving down seed crystal described in is 100 ~ 150mm/h.But the speed that moves down of seed crystal is not limited to this.
(3) when seed crystal quality changes, continue slowly to move down to reach the lower brilliant degree of depth; Concrete, when the crystalline material of seed crystal contact melting, the crystalline material of seed crystal absorption fusing, seed crystal quality increases.In the present embodiment, the described lower brilliant degree of depth is 0.5 ~ 1mm.But the lower brilliant degree of depth is not limited to this.
(4) monitor seed crystal quality speed of increasing and decrease, when seed crystal quality speed of increasing and decrease scope is in threshold value V, original heated condition is kept to crucible; Exceed threshold value V when seed crystal quality increases or reduces velocity range, raise or reduce the temperature of crucible, then, move seed crystal, perform step (2), again lower brilliant.Refer to Fig. 2, it is the time dependent curve of quality change of lower seed crystal in brilliant process under the present invention.When seed crystal quality decrease or increasing amount are less than the quality change in step (3), brilliant success is described down.When seed crystal quality increases or decrease is greater than quality change in step (3) fast, brilliant failure is described down, again lower brilliant.
Concrete, in step (4), when the seed crystal quality scope of advancing the speed exceedes threshold value V, illustrate down that brilliant temperature is on the low side, the crystalline material of fusing is fast at seed crystal surrounding crystalline.The now temperature of raise crucible, the crystallization around fusing seed crystal, then re-starts lower crystalline substance operation.Exceed threshold value V when seed crystal quality reduces speed range, brilliant temperature drift is described down, seed crystal rapid melting.Now reduce the temperature of crucible, then re-start lower crystalline substance operation.
(5) according to the speed of seed crystal quality change, intensification necking down or constant temperature necking down is selected.Concrete, when seed crystal quality speed of increasing and decrease scope is in threshold value V, brilliant success is described down, now according to the speed of seed crystal quality change, select intensification necking down or constant temperature necking down, on namely accelerating, move the speed of seed crystal, and rotate seed crystal, thus eliminate the extension of original dislocation in seed crystal simultaneously as far as possible.After seed weight is stable, the quality change of seed crystal has three kinds: gently, slowly reduce or slowly increase.Necking operation can reduce the dislocation caused by thermal shocking in seed crystal face in lower brilliant process.Compared to the fixing necking down set pattern generally used, the present invention according to the quality change situation in lower brilliant process, can select suitable necking down mode.Necking operation can classify as seed crystal melting process slowly, by intensification or constant temperature while lift seed crystal, the contact surface of seed crystal and melt is reduced.Concrete, advancing the speed when seed crystal quality is 0.5 ~-2g/h, selects constant temperature necking down.When seed crystal quality is advanced the speed more than 0.5g/h, select intensification necking down.Concrete temperature rise rate and rate of mass change existence function relation.
Based on the above lower crystal method for method of crystal growth by crystal pulling, the invention provides a kind of automatically lower brilliant equipment for method of crystal growth by crystal pulling, comprise body of heater, crucible, seed rod 10, heating unit 20, upper weight sensor 30 and/or lower weight sensor 40, control device 50.Described furnace interior hollow forms furnace chamber.Described crucible is arranged in the furnace chamber of body of heater.Described heating unit 20 to be arranged in described furnace chamber and to described crucible heating.Described upper weight sensor 30 is arranged on seed rod 10 and/or described lower weight sensor 40 is arranged at crucible bottom.Described control device 50 is electrically connected with described seed rod 10, heating unit 20, upper weight sensor 30 and/or lower weight sensor 40 respectively.The quality of seed crystal monitored by described upper weight sensor 30, is upper weighing system.The quality of crystal in crucible monitored by described lower weight sensor 40, under to weigh system control device.Seed crystal quality speed of increasing and decrease monitored by described control device 50, and according to the speed of increasing and decrease of seed crystal control the heating of heating unit 20 pairs of crucibles and seed rod 10 on move, move down or rotate.Described seed rod 10 is linkedly set with grating scale.
Described control device 50 comprises temperature control module 51, monitoring module 52 and lift and rotates control module 53.Refer to Fig. 3, it is the connection diagram of control device 50 modules of automatic lower brilliant equipment of the present invention.Described lift rotates control module 53 and is electrically connected with temperature control module 51 and monitoring module 52 respectively.Described temperature control module 51 is electrically connected with heating unit 20.Described monitoring module 52 is electrically connected with upper weight sensor 30 and/or lower weight sensor 40 respectively.Described lift rotates control module 53 and is electrically connected with seed rod 10.Described temperature control module 51 is measured crucible temperature in real time and is controlled heating unit 20 according to the temperature that crucible is measured.Described monitoring module 52 to monitor on seed rod 10 crystal weight in seed weight and/or crucible.Described lift to rotate on crucible temperature that control module 53 obtains according to temperature control module 51 and the seed rod 10 that monitoring module 52 obtains crystal weight in seed weight and/or crucible, the speed that adjustment seed rod 10 lifts or rotates.
Below in conjunction with the present embodiment, automatic lower brilliant equipment of the present invention is further described:
According to the character of different crystal material, select suitable seed crystal to move down speed, avoid lower brilliant process long or cause damage to seed crystal.
Whether changed by upper weighing system monitoring quality, when quality changes, illustrate that seed crystal enters liquid level.Now control seed crystal and continue the lower brilliant degree of depth moving down 0.5-1mm, then stop moving down.
Monitoring quality changes, when seed crystal quality increases or reduction velocity range exceedes threshold value V, judge that lower brilliant temperature is on the low side or higher, temperature control module 51 controls heating unit 20 and improves or reduce lower brilliant temperature, then lift rotation control module 53 controls seed crystal moves, and restarts lower crystalline substance operation.Be within threshold value V when seed crystal quality increases or reduces velocity range, temperature control module 51 controls heating unit 20 and finely tunes lower brilliant temperature, makes seed crystal quality maintain steadily constant or change by a small margin.When after seed crystal steady quality, steady temperature.Finally, according to the speed that seed crystal increases or reduces, judge and select intensification necking down or constant temperature necking down.
Because in seed crystal quality and crucible, the quality of melt is shifting relation, the step of thus being undertaken by lower weighing system operating can reach same control effects with aforementioned by upper weighing system.
Relative to prior art, lower crystal method of the present invention, avoids causing thermal shocking by the thermograde of heat-insulation system to seed crystal in lower brilliant process, and with the addition of lower brilliant mechanism for correcting errors, when occur seeded growth overrun and seed crystal melting phenomenon time by adjusting lower brilliant temperature, lower brilliant operation again.Automatic lower brilliant equipment of the present invention, realizes full-automatic lower brilliant process, makes lower crystalline substance operation depart from manual operation.
The present invention is not limited to above-mentioned embodiment, if do not depart from the spirit and scope of the present invention to various change of the present invention or distortion, if these are changed and distortion belongs within claim of the present invention and equivalent technologies scope, then the present invention is also intended to comprise these changes and distortion.
Claims (10)
1., for a lower crystal method for method of crystal growth by crystal pulling, it is characterized in that: comprise the following steps:
(1) to crucible heating, the crystalline material fusing being positioned at crucible is made;
(2) slowly seed crystal is moved down;
(3) when seed crystal quality changes, continue slowly to move down to reach the lower brilliant degree of depth;
(4) monitor seed crystal quality speed of increasing and decrease, when seed crystal quality speed of increasing and decrease scope is in threshold value V, original heated condition is kept to crucible; Exceed threshold value V when seed crystal quality increases or reduces velocity range, raise or reduce the temperature of crucible, then, move seed crystal, perform step (2), again lower brilliant.
2. lower crystal method according to claim 1, is characterized in that: also comprise step (5), according to the speed of seed crystal quality change, selects intensification necking down or constant temperature necking down.
3. lower crystal method according to claim 2, is characterized in that: advancing the speed when seed crystal quality is 0.5 ~-2g/h, selects constant temperature necking down; When seed crystal quality is advanced the speed more than 0.5g/h, select intensification necking down.
4. the lower crystal method according to claim arbitrary in claim 1-3, is characterized in that: the speed moving down seed crystal is 100 ~ 150mm/h.
5. lower crystal method according to claim 4, is characterized in that: the described lower brilliant degree of depth is 0.5 ~ 1mm.
6., for an automatically lower brilliant equipment for method of crystal growth by crystal pulling, it is characterized in that: comprise body of heater, crucible, seed rod, heating unit, upper weight sensor and/or lower weight sensor, control device; Described crucible is arranged in the furnace chamber of body of heater; Described heating unit to be arranged in described furnace chamber and to described crucible heating; Described upper weight sensor is arranged on seed rod and/or described lower weight sensor is arranged at crucible bottom; Described control device is electrically connected with described seed rod, heating unit, upper weight sensor and/or lower weight sensor respectively; Described control device monitoring seed crystal quality speed of increasing and decrease, and control heating unit according to the speed of increasing and decrease of seed crystal and move on the heating of crucible and seed rod, move down or rotate.
7. automatic lower brilliant equipment according to claim 6, is characterized in that: described control device comprises temperature control module, monitoring module and lift and rotates control module; Described lift rotates control module and is electrically connected with temperature control module and monitoring module respectively; Described temperature control module is electrically connected with heating unit, and described monitoring module is electrically connected with upper weight sensor and/or lower weight sensor respectively, and described lift rotates control module and is electrically connected with seed rod; Described temperature control module is measured crucible temperature in real time and is controlled heating unit according to the temperature that crucible is measured; Crystal weight in seed weight and/or crucible on described monitoring module monitoring seed rod; Described lift to rotate on crucible temperature that control module obtains according to temperature control module and the seed rod that monitoring module obtains crystal weight in seed weight and/or crucible, regulates the speed of seed rod lift or rotation.
8. automatic lower brilliant equipment according to claim 6, is characterized in that: also comprise one and to link the grating scale arranged with seed rod.
9. automatic lower brilliant equipment according to claim 6, is characterized in that: described control device monitoring seed crystal quality speed of increasing and decrease, when seed crystal quality speed of increasing and decrease scope is in threshold value V, keeps original heated condition to crucible; Exceed threshold value V when seed crystal quality increases or reduces velocity range, raise or reduce the temperature of crucible, then, move seed crystal, again lower brilliant.
10. the automatically lower brilliant equipment according to claim arbitrary in claim 6-9, is characterized in that: described seed rod drives the speed that moves down of seed crystal to be 100 ~ 150mm/h.
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| CN201610054686.1A CN105568369B (en) | 2016-01-26 | 2016-01-26 | A kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment |
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| CN201610054686.1A CN105568369B (en) | 2016-01-26 | 2016-01-26 | A kind of lower crystal method for method of crystal growth by crystal pulling and automatic lower brilliant equipment |
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