前苏联专利SU1433420A3 Cold crucible

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专利摘要:
Kalter Tiegel für die Durchführung des skull-melting-Verfahrens mit Induktionsspulen, über die Hochfrequenz- . Energie in den Tiegelinhalt einkoppelbar ist und innerhalb des Tiegels mit einem Körper aus einem gegenüber einer in dem Tiegel befindlichen Schmelze inerten, elektrisch leitfähigen Material und einen Behälter aus einem gegenüber der Schmelze inerten Material, wobei der Behälter zur offenen Seite des Tiegels hin offen ist und die Schmelze hindurchlassende Öffnungen aufweist.
公开号:SU1433420A3
申请号:SU843741047
申请日:1984-05-03
公开日:1988-10-23
发明作者:Матейка Дитер；Лауриен Рольф
申请人:Н.В.Филипс Глоэлампенфабрикен (Фирма)；
IPC主号:

专利说明:

The invention relates to a cold (needle for melting and crystallization of inorganic compounds by the method of decanter melting.
The purpose of the invention is to increase the size of single crystals.
FIG. 1 shows a crucible, a common, n section; in fig. 2 - container installed in the crucible with holes in the bottom, slit; Fig. 3 is the same, with holes in the side walls: 1 bottom. .
The crucible is made of coarse metal, with double walls, preferably copper, which are cooled by flowing medium (water) and that are bent at a right angle and arranged in a circle. Narzgzhny tubes 1; mec1T has a clearance of 0.3 mm and a bottom seal. The surface of the tubes 1 must be protected against oxidation. Copper tubes protect the layer of silicon, which is A / 6 microns thick. The bottom 2 of the crucible, through which the cooling medium flows, is formed by a plate 3 of a dielectric material that is inert to the melt, for example, from quartz 1 Plate 3 is fixed with the help of i4 elements From a heat-resistant systematic resin and ring 5 made from 1 and an electric material, for example | alumina. This ensures the stability of the crucible wall consisting of tubes 1. A conductive element b inert to melt, for example, made of iridium, is mounted on plate 3 by means of supports 7. A crucible wall formed by tubes 1 surrounds the tube made of heat resistant material, for example quartz (not posazano), and an annular induction coil 8, which is connected to a high frequency generator (not shown), whose operating frequency is 1-7 MHz. A second induction coil 9 is provided under the bottom of the crucible, through which energy with a frequency lower than that supplied to the contents of the crucible through the first induction coil 8 can be introduced into the contents of the crucible. An additional induction coil 9 is connected to a generator (not shown) J which has a working frequency in the range of 7-10 generators can be activated independently of one another. The block 10 is made of heat-resistant material, for example, oxide ceramics, and is designed to reduce heat losses “Container 11, made of material that is inert to the melt, for example iridium, is set-. flax inside the crucible and has a bottom in the form of a reverse cone 12. Through the rod
13 container connected to the mechanism
14 vertically moving. The detector 15 is connected together with one of the rods 13 to an electrical circuit and is designed to determine the melt cell in the crucible. The detector 15 is also filled with a material that is inert to the melt, such as iridium.
The cone 12 of the container has a central opening 16. In this case, the around-G-hole has a diameter of 8 1 F1, an internal diameter of the container of 76 mm, a height of a cylindrical wall of 20 mm and a wall thickness of 2 mm.
The cone is connected to the wall of the container 11 in such a way that a ridge of 2–3 mm is formed by an edge 17, the arrows in FIG. Figures 2 and 3 show the direction of the convection currents in the melt, depending on the arrangement of the holes in the container. ,
The device works as follows.
The crucible is filled with the initial garnet powder, for example, NdjGajO. Generators, excitation induction coils 8 and 9, turn on simultaneously. Preferably, the energy is first applied to the element 6 through the induction coil 9 and heated it to a temperature above the melting point of the garnet material - 1550 s. After a sufficient volume of melt has been formed in the lower part of the crucible, energy is supplied through the induction coil 8 until the material is completely melted. In the course of the process, element 6 performs the function of independent controlled heating. On the inner wall of the crucible and its bottom a sintered layer is formed - a skull. The thickness of this layer can be controlled using both induction coils 8 and 9. In this way, the melting process is stabilized. Neither experiment has reached a critical volume of the melt. Element 6 can be disc-shaped, solid or with holes in the form. holes, slots.
During the heating process, the container 11 is above the contents in the crucible. After melting, the container is lowered using mechanism 1A so that the upper edge of the container protrudes 2-5 mm from the surface of the melt. The container is filled with melt through the holes in the bottom and walls. The container is designed to control the radial temperature distribution with a minimum temperature in the center of the surface of the melt.
For growing, the seed crystal contacts the surface of the melt after a period of stabilization for 15 minutes. Then the crystal is pulled while it is rotating. By slowly lowering the power of the generator connected to the induction coil 8, the diameter of the growing crystal is increased to the desired final diameter. The power of the generator is adjusted so that the crystal continues to grow at a constant diameter and constant height of the melt. The change in the melt level is transmitted by the detector 15, the signal of which controls the mechanism 14.
After the growth is complete, the crystal is separated from the residual melt by a rapid rise. The container 11 is then removed from the melt and the crystal is cooled to room temperature by reducing the power of the generators connected to the induction coils 8 and 9. Pulling the NdijGa O crystal out of the load of 6 kg on the seed Ncl GasOi, rotated at a speed of 14, at a drawing rate 4 mm / h Get single crystals Nd.GajO ,. with a diameter of 40 mm and a length of 60 mm with low voltages.
The method can be varied so that the level of the melt is kept constant by feeding the non-melting material into the space between the crucible wall and the container 11 from an additional device controlled by the detector 15.
Similarly, NaCl crystals are grown at a rotational speed of 20 minutes and a speedy stretch of 18 km / h. Single crystals with a diameter of 55 mm and a length of 190 mm are obtained.
Inventions

权利要求:
Claims (3)
[1]
1. A cold crucible for melting and crystallization of inorganic compounds, made in the form of metal tubes cooled from the inside, forming the walls of the crucibles around which the induction coil is located, and having a cooled bottom made of dielectric material, in order to increase the size of the single crystals, the crucible is provided installed inside it coaxially with a container with an opening having a volume of not more than 25% of the total volume of the crucible, an electrically conductive element inert to the melt, mounted above the bottom of the crucible and Optional independent induction coil located under the bottom of the crucible.
[2]
2. A crucible according to claim 1, about tl and h a-yu and with the fact that the container is made in the form of a hollow cylinder, the wall of which is parallel to the wall of the crucible with the bottom in the form of a reverse cone.
[3]
3. A crucible according to claim 1 or 2, such that the holes in the container are made in the wall of the cylinder and / or in the cone.
I
about OCJOQ I
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/ 3
FIG. 3

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同族专利:

公开号 | 公开日

DE3468130D1|1988-01-28|

EP0124938A3|1985-11-27|

JPH0416702B2|1992-03-24|

DE3316547A1|1984-11-08|

CA1234531A|1988-03-29|

EP0124938B1|1987-12-16|

US4609425A|1986-09-02|

DE3316547C2|1985-05-30|

AT31433T|1988-01-15|

JPS602876A|1985-01-09|

EP0124938A2|1984-11-14|

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US3025191A|1953-07-13|1962-03-13|Raytheon Co|Crystal-growing apparatus and methods|

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DE2245250A1|1972-09-15|1974-03-21|Philips Patentverwaltung|Growing crystals esp garnet monocrystals - in inner chamber partitioned from outer chamber by perforated dividing wall|

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US4246064A|1979-07-02|1981-01-20|Western Electric Company, Inc.|Double crucible crystal growing process|JPH0559874B2|1985-09-11|1993-09-01|Sumitomo Electric Industries|

US4911893A|1987-06-11|1990-03-27|Amoco Corporation|Floating recycle pan for ebullated bed reactors|

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JP2755588B2|1988-02-22|1998-05-20|株式会社東芝|Crystal pulling method|

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

DE3316547A|DE3316547C2|1983-05-06|1983-05-06|Cold crucible for melting non-metallic inorganic compounds|

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