CN105648520A - Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof - Google Patents
Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof Download PDFInfo
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- CN105648520A CN105648520A CN201610155283.6A CN201610155283A CN105648520A CN 105648520 A CN105648520 A CN 105648520A CN 201610155283 A CN201610155283 A CN 201610155283A CN 105648520 A CN105648520 A CN 105648520A
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
Abstract
The invention relates to a seed crystal capable of reinforcing seeding temperature signals. The seed crystal is applied to directional crystal growth from bottom to top. The section area of an upper half part of the seed crystal is greater than that of a lower half part of the seed crystal, so that the side of the upper half part of the seed crystal is in close fit with a seed crystal hole when the seed crystal is placed in the seed crystal hole; at least one gap is formed in a vertical direction between the side of the lower half part of the seed crystal and the side of the seed crystal hole; the at least one gap forms a flow guide gap structure; the top end of a flow guide gap is not communicated with the upper end surface of the seed crystal; and the flow guide gap structure between the side of the seed crystal and the side of the seed crystal hole is used for reinforcing the seeding temperature signals to finish seeding. The seed crystal has the advantages that the seeding polycrystals can be reduced, the seeding temperature signals can be reinforced, and a seeding method of the seed crystal is capable of effectively improving the seeding quality and the yield of crystals.
Description
Technical field
The invention belongs to technical field of crystal growth, in particular to a kind of seed crystal strengthening seeding temperature signal, also relate to the seeding methods of this seed crystal a kind of.
Background technology
By crystal raw material is fused into melt, and make melt under the induction of seed crystal gradually directional solidification growth go out the basic characteristics that the crystal consistent with seed crystal lattice is the growth of melt growth method crystal. And to carry out directional freeze from bottom to top be the method the most generally used in melt growth method, common are falling crucible method (VB), Vertical Gradient Freeze (VGF) method (VGF), directional solidification method (DS), heat-exchanging method (HEM) etc. One of critical process of this kind of growing method is to draw brilliant technique, draws brilliant quality and success or failure are directly connected to the final finished rate of crystal growth.
From bottom to top in molten not crystal growth, owing to seed crystal is placed in the seed crystal hole of crucible bottom so that crystal cannot directly be observed. Draw crystalline substance and require that seed portion melts, in actual mechanical process, the feedback information of seed crystal state is lacked during owing to drawing crystalline substance, production process often exists do not melt, that excess molten (seed crystal all melts or only has a small amount of residual) or seed crystal draw brilliant process is steady not, cause final crystal formation polycrystalline or there is a large amount of dislocations.
Temperature survey near seed crystal is a kind of the most general method judging whether seed crystal melts. When temperature near seed crystal is close to fusing point, it is possible to judge that seed crystal has started fusing according to this. But in the process of growth of high-melting-point crystal, when temperature is greater than 2000 �� of C, High Accuracy Thermocouple Temperature and Thermistor Temperature Measurement meter under prior art all exceed use temperature and cannot directly measure. Another kind surveys the infrared flash ranging temperature that temperature scheme is noncontact formula. And the impact of the series of factors such as the easy flowing by the pollution of body of heater view port, body of heater internal gas of infrared flash ranging temperature and blackness change, testee surface characteristic, the absolute value of measured temperature is often lack of consistency and reliability.
For above-mentioned phenomenon, from the profile design of seed crystal, it is proposed to the signal feedback of seed crystal melted state when crystalline substance is drawn in a kind of acquisition.
In addition, being greater than in the ultrahigh-temperature crystal melt growth method of 2000 �� of C carrying out fusing point, high-temperature fusant crucible used is main high temperature material manufacture by tungsten material usually, and tungsten is the noble metal of high rigidity difficulty processing. Therefore, from the precision of processing, economy with facilitate the angle that crystal grow, the seed crystal hole of placement seed crystal adopts cylindrical hole usually, and the position of cylindrical hole is in the bottom center of crucible (as shown in Figure 1). When seed crystal is placed in seed crystal hole, upper part and the seed crystal hole of seed crystal closely cooperate, and in order to form the space, water conservancy diversion gap of seed crystal hole and seed crystal lower part, seed crystal processing is reserved gap by the method for most convenient.
Gap between seed crystal and seed crystal hole is more big, and when drawing crystalline substance, rise in temperature signal is more obvious, reduces the probability of operator's erroneous judgement; But gap too big time, in gap the crystalline material of crystallization again due to crystallization time short, be easy to form the crystal orientation different from seed crystal.
According to the ultimate principle of crystal along the normal growth at interface, solid-liquid phase interface at seed crystal place is in when solid phase is protruded to liquid phase that (this type of interface claims Raised key axis below, otherwise claim recessed interface), in wide arc gap the crystal of different crystal orientations draw crystalline substance complete after long brilliant process in be difficult to eliminate and form polycrystalline (as shown in Figure 2); In small?gap suture, the crystal of different crystal orientations is then easily eliminated in long brilliant process, makes final crystal product still keep monocrystalline state (as shown in Figure 3); During disadvantageous situation under the crystal growing state at recessed interface, no matter gap size, once form the situation of different crystal orientations, final crystal product all has very big probability to become polycrystalline (as shown in Figure 4).
For this reason, in order to make crystal product keep monocrystalline, the gap between seed crystal and seed crystal hole is the smaller the better, but small?gap suture draws brilliant signal by obviously weakening.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of can reduce draw brilliant become polycrystalline and strengthening seeding temperature signal seed crystal, a kind of seeding methods that can effectively improve the yield rate drawing brilliant quality and crystal is also provided.
For solving the problems of the technologies described above, the technical scheme of the present invention is: a kind of seed crystal strengthening seeding temperature signal, for carrying out directed crystal growth from bottom to top, its innovative point is: the sectional area of described seed crystal upper part is greater than the sectional area of seed crystal lower part, when seed crystal is placed in seed crystal hole, seed crystal upper part side and seed crystal hole closely cooperate, and sectional area remains unchanged; And seed crystal lower part sectional area reduces downwards gradually from upper so that the gap formed between seed crystal and seed crystal hole becomes big gradually, described gap forms gap structure between water conservancy diversion, and the upper surface of the most Xiang Duanyu seed crystal in water conservancy diversion gap is not through.
Further, described seed crystal is made up of a cylinder and an inverted trapezoidal circular cone, and wherein cylinder forms upper part of seed crystal, and inverted trapezoidal circular cone forms lower part of seed crystal, and the maximum diameter of inverted trapezoidal circular cone equals the diameter of upper part column structure.
Further, the cone angle scope of described inverted trapezoidal circular cone is 2��30 ��.
Further, described seed crystal is processed by cylindrical seed crystal, and wherein upper part of seed crystal keeps not processing, and lower part of seed crystal removes the formation of part material to tilt the angle level cutting of 1��15 ��, and the cut surface of seed crystal is plane.
Further, described cut surface can be one or more.
With a seeding methods for the seed crystal of above-mentioned strengthening seeding temperature signal, its innovative point is: described seeding methods comprises the steps:
(1) seed crystal is placed in the seed crystal hole of crucible bottom, and seed crystal has the part of cut surface to be placed on bottom cylindrical seed crystal hole so that between seed crystal lower part side and side, seed crystal hole, form gap, and this gap forms gap structure between water conservancy diversion;
(2) crystal raw material being placed on crucible inside, by progressively promoting heater power, melt to the crystal raw material in crucible, solid-liquid phase interface passes seed crystal upper surface;
(3) by continuing to promote heating power, solid-liquid phase interface is moved downwards, all melts to seed crystal upper surface;
(4) when solid-liquid phase interface moves down into the upper end in space, water conservancy diversion gap, high temperature solution flows into space, water conservancy diversion gap, now, monitors seed crystal bottom surface temperature with infrared light;
(5) when observing strong rise in temperature signal, stop at once promoting heater power, or reduce heating power 0-5KW;
(6), after waiting that solid-liquid phase interface is stable, draw crystalline substance and complete, enter crystal growth technique.
It is an advantage of the current invention that:
(1) the present invention strengthens the seed crystal of seeding temperature signal, when seed crystal is placed in seed crystal hole, seed crystal upper part side and seed crystal hole closely cooperate, and between seed crystal lower part side and side, hole, seed crystal hole, form the gap becoming big gradually, such gap becomes big structure gradually, gap can being made just to be bigger than the liquid film stagnation point of surface-tension energy support, can obtain obvious seeding temperature signal, simultaneously little as far as possible polycrystalline generates district and decreases the possibility drawing brilliant one-tenth polycrystalline;
(2) seeding methods of the present invention, it is possible to draw brilliant signal drawing to obtain in brilliant process, can conveniently judge whether seed crystal melts and put in place; This kind of judgment mode does not need the measurement of temperature absolute value very accurately, because this reducing the use cost of metering facility, and improves the yield rate of production.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 crucible and seed crystal hole modes of emplacement schematic diagram.
Fig. 2-4 is that quality product is affected schematic diagram by gap and solid-liquid interface shape.
Fig. 5 is the structural representation of the seed crystal implementing 1 strengthening seeding temperature signal in the present invention.
Fig. 6 is the structural representation of the seed crystal implementing 2 strengthening seeding temperature signals in the present invention.
Fig. 7 is the structural representation of the seed crystal implementing 3 strengthening seeding temperature signals in the present invention.
Fig. 8 is seeding methods of the present invention temperature feedback signal illustrated example when drawing crystalline substance.
Embodiment
The following examples can make professional and technical personnel more fully understand the present invention, but does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
As shown in Figure 1, cylindrical seed crystal hole 2 it is provided with bottom the crucible 1 that the present embodiment adopts; The seed crystal of the present embodiment strengthening seeding temperature signal, as shown in Figure 5, the diameter of cylindrical seed crystal 3 is 25mm, cylindrical seed crystal 3 total length is 80mm, in lower part 40mm eminence of cylindrical seed crystal 3, being processed with 4 angles of inclination by the mode of machining is 5 �� of cut surfaces 4, and forms gap between cut surface 4 and cylindrical seed crystal hole 2 lower part.
The present embodiment adopts the seeding methods of HEM method growing sapphire crystal, and this seeding methods comprises the steps:
(1) as shown in Figure 1, seed crystal is placed in the cylindrical seed crystal hole 2 bottom crucible 1, and seed crystal has the part of cut surface 4 to be placed on bottom cylindrical seed crystal hole 2 so that form gap between seed crystal lower part side and side, cylindrical seed crystal hole 2, and gap structure between this gap formation water conservancy diversion;
(2) crystal raw material is placed on crucible 1 inner, by progressively promoting heater power, crystal raw material in crucible 1 is melted, solid-liquid phase interface passes seed crystal upper surface, bottom crucible 1 below seed crystal hole and by infrared flash ranging temperature, now, the state that the temperature bottom crucible 1 is in steady rising always, does not almost fluctuate, as shown in the stage in Fig. 8 one;
(3) by continuing to promote heating power, solid-liquid phase interface is moved downwards, seed crystal upper surface is all melted;
(4) when solid-liquid phase interface moves down into the upper end in space, water conservancy diversion gap, high temperature solution flows into space, water conservancy diversion gap, and now, infrared light monitoring seed crystal bottom surface temperature ramp de is sudden change, and as shown in the stage in Fig. 8 two, and signal is strong;
(5) when observing strong rise in temperature signal, stop at once promoting heater power;
(6), after waiting that solid-liquid phase interface is stable, draw crystalline substance and complete, enter crystal growth technique.
Table 1 is the contrast table that embodiment 1 seeding methods and tradition HEM method draw each performance of crystal that crystals growth goes out.
Table 1 embodiment 1 seeding methods draws the contrast of each performance of crystal that crystals growth goes out with tradition HEM method
As can be seen from the above table, the present embodiment 1 seeding methods is compared with tradition HEM method, and the crystal crystal forming rate grown improves greatly, can reach 85%; The product proportion of 100% monocrystalline also promotes greatly, can reach 75%; But the dislocation desity of crystal reduces greatly, and it is at 1500��3600/cm2Between.
Embodiment 2
As shown in Figure 1, cylindrical seed crystal hole 2 it is provided with bottom the crucible 1 that the present embodiment adopts; The seed crystal of the present embodiment strengthening seeding temperature signal, as shown in Figure 6, the diameter of cylindrical seed crystal 3 is 25mm, cylindrical seed crystal 1 total length is 80mm, in lower part 40mm eminence of cylindrical seed crystal 1, being processed with 1 angle of inclination by the mode of machining is 5 �� of cut surfaces 5, and forms gap between cut surface 5 and cylindrical seed crystal hole 2 lower part.
The present embodiment adopts the seeding methods of falling crucible method (VB method) growing sapphire crystal, and this seeding methods comprises the steps:
(1) as shown in Figure 1, seed crystal is placed in the cylindrical seed crystal hole 2 bottom crucible 1, and seed crystal has the part of cut surface 5 to be placed on bottom cylindrical seed crystal hole 2 so that form gap between seed crystal lower part side and side, cylindrical seed crystal hole 2, and gap structure between this gap formation water conservancy diversion;
(2) crystal raw material is placed on crucible 1 inner, by progressively promoting heater power, crystal raw material in crucible 1 is melted, solid-liquid phase interface passes seed crystal upper surface, bottom crucible 1 below seed crystal hole and by infrared flash ranging temperature, now, the state that the temperature bottom crucible 1 is in steady rising always, does not almost fluctuate, as shown in the stage in Fig. 8 one;
(3) by continuing to promote heating power, solid-liquid phase interface is moved downwards, seed crystal upper surface is all melted;
(4) when solid-liquid phase interface moves down into the upper end in space, water conservancy diversion gap, high temperature solution flows into space, water conservancy diversion gap, and now, infrared light monitoring seed crystal bottom surface temperature ramp de is sudden change, and as shown in the stage in Fig. 8 two, and signal is strong;
(5) when observing strong rise in temperature signal, heating power 3-5KW is reduced at once;
(6), after waiting that solid-liquid phase interface is stable, draw crystalline substance and complete, enter crystal growth technique.
Embodiment 3
As shown in Figure 1, cylindrical seed crystal hole 2 it is provided with bottom the crucible 1 that the present embodiment adopts; The seed crystal of the present embodiment strengthening seeding temperature signal, as shown in Figure 7, seed crystal is made up of a cylinder 6 and an inverted trapezoidal circular cone 7, wherein, cylinder 6 forms upper part of seed crystal, inverted trapezoidal circular cone 7 forms lower part of seed crystal, and the maximum diameter of inverted trapezoidal circular cone 7 is identical with the diameter of upper part cylinder 6, and the cone angle of inverted trapezoidal circular cone 7 is 5 ��.
The present embodiment adopts the seeding methods of falling crucible method (VB method) growing sapphire crystal, and this seeding methods comprises the steps:
(1) as shown in Figure 1, seed crystal is placed in the cylindrical seed crystal hole 2 bottom crucible 1, and seed crystal has the part of cut surface 5 to be placed on bottom cylindrical seed crystal hole 2 so that form gap between seed crystal lower part side and side, cylindrical seed crystal hole 2, and gap structure between this gap formation water conservancy diversion;
(2) crystal raw material is placed on crucible 1 inner, by progressively promoting heater power, crystal raw material in crucible 1 is melted, solid-liquid phase interface passes seed crystal upper surface, bottom crucible 1 below seed crystal hole and by infrared flash ranging temperature, now, the state that the temperature bottom crucible 1 is in steady rising always, does not almost fluctuate, as shown in the stage in Fig. 8 one;
(3) by continuing to promote heating power, solid-liquid phase interface is moved downwards, seed crystal upper surface is all melted;
(4) when solid-liquid phase interface moves down into the upper end in space, water conservancy diversion gap, high temperature solution flows into space, water conservancy diversion gap, and now, infrared light monitoring seed crystal bottom surface temperature ramp de is sudden change, and as shown in the stage in Fig. 8 two, and signal is strong;
(5) when observing strong rise in temperature signal, heating power 3-5KW is reduced at once;
(6), after waiting that solid-liquid phase interface is stable, draw crystalline substance and complete, enter crystal growth technique.
Table 2 is the contrast table that embodiment 2-3 seeding methods and tradition VB method draw each performance of crystal that crystals growth goes out.
Table 2 embodiment 2-3 seeding methods draws the contrast of each performance of crystal that crystals growth goes out with tradition VB method
As can be seen from the above table, embodiment 2-3 seeding methods is compared with tradition VB method, and the crystal crystal forming rate grown improves greatly, can reach more than 85%; The product proportion of 100% monocrystalline also promotes greatly, can reach more than 75%; But the dislocation desity of crystal reduces greatly, and it is at 1000��2000/cm2Between.
The contrast table of each performance of crystal that table 3 grows for embodiment 1-3 seeding methods.
The contrast of each performance of crystal that table 3 embodiment 1-3 seeding methods grows
As can be seen from the above table, embodiment 1-3 seeding methods contrasts mutually, each performance of comprehensive crystal, and embodiment 3 is most preferred embodiment; And then, the seed crystal structure that the present invention proposes and the seeding methods of sapphire crystal, the crystal mass grown is excellent, dislocation desity is low, perfection of crystal and yield rate height, it is possible to reduces costs, and is easy to industrialization.
More than show and describe the ultimate principle of the present invention and the advantage of main feature and the present invention. The technician of the industry should understand; the present invention is not restricted to the described embodiments; the principle that the present invention is just described described in above-described embodiment and specification sheets; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention. The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (6)
1. strengthen the seed crystal of seeding temperature signal for one kind, for carrying out directed crystal growth from bottom to top, it is characterized in that: the sectional area of described seed crystal upper part is greater than the sectional area of seed crystal lower part, when seed crystal is placed in seed crystal hole, seed crystal upper part side and seed crystal hole closely cooperate, and sectional area remains unchanged; And seed crystal lower part sectional area reduces downwards gradually from upper so that the gap formed between seed crystal and seed crystal hole becomes big gradually, described gap forms gap structure between water conservancy diversion, and the upper surface of the most Xiang Duanyu seed crystal in water conservancy diversion gap is not through.
2. the seed crystal of strengthening seeding temperature signal according to claim 1, it is characterized in that: described seed crystal is made up of a cylinder and an inverted trapezoidal circular cone, wherein cylinder forms upper part of seed crystal, inverted trapezoidal circular cone forms lower part of seed crystal, and the maximum diameter of inverted trapezoidal circular cone equals the diameter of upper part column structure.
3. the seed crystal of strengthening seeding temperature signal according to claim 2, it is characterised in that: the cone angle scope of described inverted trapezoidal circular cone is 2��30 ��.
4. the seed crystal of strengthening seeding temperature signal according to claim 1, it is characterized in that: described seed crystal is processed by cylindrical seed crystal, wherein upper part of seed crystal keeps not processing, and lower part of seed crystal is formed to tilt the angle level cutting removal part material of 1��15 ��, and the cut surface of seed crystal is plane.
5. the seed crystal of strengthening seeding temperature signal according to claim 4, it is characterised in that: described cut surface can be one or more.
6. strengthen the seeding methods of the seed crystal of seeding temperature signal by claim 1 for one kind, it is characterised in that: described seeding methods comprises the steps:
(1) seed crystal is placed in the seed crystal hole of crucible bottom, and seed crystal has the part of cut surface to be placed on bottom cylindrical seed crystal hole so that between seed crystal lower part side and side, seed crystal hole, form gap, and this gap forms gap structure between water conservancy diversion;
(2) crystal raw material being placed on crucible inside, by progressively promoting heater power, melt to the crystal raw material in crucible, solid-liquid phase interface passes seed crystal upper surface;
(3) by continuing to promote heating power, solid-liquid phase interface is moved downwards, all melts to seed crystal upper surface;
(4) when solid-liquid phase interface moves down into the upper end in space, water conservancy diversion gap, high temperature solution flows into space, water conservancy diversion gap, now, monitors seed crystal bottom surface temperature with infrared light;
(5) when observing strong rise in temperature signal, stop at once promoting heater power, or reduce heating power 0-5KW;
(6), after waiting that solid-liquid phase interface is stable, draw crystalline substance and complete, enter crystal growth technique.
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