JPS62176990A - Device for producing compound semiconductor single crystal - Google Patents

Abstract

PURPOSE:To obtain the titled device for producing single crystal which is free from deformation and easy in operation and inexpensive in production cost by providing the heat resistant upper and lower jigs and a crucible housing a raw material in the specified quarts vessel and arranging a sealing medium to seal these. CONSTITUTION:After introducing a raw material 13 for a compd. having high dissociation pressure in a crucible 10 consisting of Al2N2 or the like and fitting seed crystal 15 to the lower end part of a rotary pulling-up shaft 5, an upper jig 3 an a lower jig 4 consisting of a heat resistant material (i.e. molybdenum) are inserted into a groove 9. Then a sealing medium (B2O3)7 is heated and melted by a subheater 11 and a main heater 12 to seal the spaces among the jig 3, the shaft 5 and the jig 4 and thereafter the raw material 13 incorporated in the crucible 10 is heated and melted by the main heater 12 and the shaft 5 is descended while rotating the shaft 5 and a rotary shaft 8 and after bringing seed crystal 15 of the lower end part into contact with the raw material 13, single crystal 16 is grown by ascending the shaft 5. Then the produced compd. semiconductor single crystal 16 is taken out and also the raw material 13 remaining in the crucible 10 is easily taken out by separating the upper and lower jigs 1, 2.

Description

[Detailed Description of the Invention] [Industrial Field of Application] The present invention relates to a compound semiconductor single crystal manufacturing device, and in particular to a compound semiconductor single crystal manufacturing device.
The present invention relates to a single crystal manufacturing apparatus for high dissociation pressure compound semiconductors such as As and InP.

[Prior Art] The configuration of a conventional compound semiconductor single crystal manufacturing apparatus is shown in FIG. A rotating pulling shaft 45 contains a high dissociation pressure compound 43 such as GaAs or InP as a raw material in a quartz container 42 fixed on a rotating shaft 41, and a seed crystal 44 is attached to the tip thereof.
is inserted into the quartz container 42 from the top. Furthermore, after a fitting lid 47 made of quartz containing sealing boron oxide 46 is fitted onto the upper part of the quartz container 42, the inside of the bottom container 48 is evacuated. Next, an inert gas such as argon or nitrogen is fed into the full-flexure container 48, and the sealing boron oxide 46 is heated and softened using the sub-heater 49.
A seal is formed between the fitting lid 47 and the rotational pull-up shaft 45. Thereafter, the main heater 50 heats the inside of the quartz container 42 to melt the high wI 11 pressure compound 43, and the rotating pulling shaft 4
5 and rotation @41 in the same direction or in the opposite direction, the rotational pull-up shaft 45 is lowered. In this way, the seed crystal 44 attached to the lower end of the rotary pulling shaft 45 is brought into contact with the melt of the high dissociation pressure compound 43, and then the single crystal 51 is grown by raising the rotary pulling shaft 45. .

In this production apparatus, the high-resolution 1IiIt pressure compound 439 seed 44 and single crystal 51 are sealed in the quartz container 42 by the sealing boron oxide 46, so that they are not exposed to an inert gas atmosphere at high temperatures. For this reason, 8s from the surface of the high dissociation pressure compound 431 seed crystal 44 and single crystal 510
, the dissociation of the volatile components of P'@ is suppressed, and a single crystal having a stoichiometric composition and a good surface condition can be obtained.

[Problems to be Solved by the Invention] However, since the quartz container 42 has a vertically long pot shape, it is difficult to remove the high dissociation pressure compound 43 remaining at the bottom of the quartz container 42 after single crystal growth. Met.

Further, the quartz container 42 and the fitting lid 47 are exposed to high temperatures for a long time, so they are forced to deform.

As a result, in the past, the quartz container 42 and the one-piece lid 47 could not be used repeatedly, and had to be damaged after one single crystal growth.

SUMMARY OF THE INVENTION It is therefore an object of the present invention to provide a compound semiconductor single crystal manufacturing apparatus that can solve the problems of the prior art described above and can extend the life of the container.

[Means for Solving the Problems] In order to achieve the above object, the compound semiconductor single crystal manufacturing apparatus of the present invention divides a quartz container for heating and melting raw materials into an upper container and a lower container. A heat-resistant upper jig and a lower jig are installed around the outer peripheries of the container and the lower container, respectively, and a crucible containing raw materials is placed in the lower container, and the upper jig and the lower A sealing material is used to seal between the upper jig and the rotational pulling shaft having a seed crystal at its lower end.

Function] By providing a heat-resistant upper jig and a lower jig on the outer periphery of the quartz container divided into an upper container and a lower container in this way, deformation of the quartz container when exposed to high temperature conditions is prevented. be done.

Furthermore, by dividing the quartz container into upper and lower parts, it is possible to easily take out the raw material remaining at the bottom of the container after single crystal growth.

[Example] Embodiments of the present invention will be described below with reference to the accompanying drawings.

FIG. 1 is a block diagram of a compound semiconductor single crystal production Q apparatus according to an embodiment of the present invention. In the figure, reference numerals 1 and 2 are an upper container and a lower container made of quartz, and an upper jig 3 and a lower jig 4 made of graphite are provided on the outer peripheries of the containers so as to surround them, respectively. A rotating lifting shaft 5 vertically passes through the upper surfaces of the upper container 1 and the upper jig 3, and four parts are formed on the upper end surface of the upper jig 3 so as to surround the outer periphery of the rotating lifting shaft 5. 6 is formed, and a sealing material 7 made of boron oxide is accommodated within this recess 6. Further, the lower jig 4 is fixed to a rotating shaft 8-H, and a groove 9 is formed along the circumferential direction in the upper edge thereof into which the lower edge of the upper jig 3 is inserted. Also accommodated is a sealing material 7 made of boron oxide. Furthermore, a crucible 10 made of bilolytic boron nitride is placed in the lower container 2.

Further, 11 and 12 denote the sealing material 7 accommodated in the recess 6 of the upper jig 3, the sealing material 7 accommodated in the groove 9 of the lower jig 4, and the raw material 13 in the crucible 10, respectively. A sub-heater and a main heater are used for heating, and each of the above-mentioned members including these are housed in a metal container 14 connected to a vacuum pump (not shown).

Next, a process for producing a single crystal using the apparatus of this example will be described.

First, a high dissociation pressure compound that will become the raw material 13 is stored in the crucible 10, and a seed crystal 15 is attached to the lower end of the rotating pulling shaft 5. Insert into 9. Roughly speaking, the inside of the metal container 14 is evacuated using a vacuum pump, and then an inert gas such as argon or nitrogen is sent into the metal container 14.

Then, the sub-heater 11 and the main heater 12 heat and melt the sealing material 7 accommodated in the recess 6 of the upper jig 3 and the groove 9 of the lower jig 4, and the upper jig 3 and the rotational lifting shaft 5 are separated. After sealing the space between the upper jig 3 and the lower jig 4,
Furthermore, the raw material 13 in the crucible 10 is heated by the main heater 12.
is heated and melted, and the rotary pull-up shaft 5 is lowered while rotating the rotary pull-up shaft 5 and the rotary shaft 8 in the same or opposite directions. In this manner, the seed crystal 15 attached to the lower end of the rotary pulling shaft 5 is brought into contact with the original r1113, and then the single crystal 16 is grown by raising the rotary pulling shaft 5.

After the growth is completed, the upper container 1 and the lower container 2 are separated, and the obtained single crystal 16 can be taken out and the raw material 13 remaining in the crucible 10 can be scraped out.

Incidentally, the divided portions of the upper container 1 and the lower container 2 are not limited to those shown in FIG. 1, and there is no problem in changing their positions as in the portion Δ in FIG. 2 or 3.

Further, the material of the upper jig 3 and the lower jig 4 may be any material as long as it has excellent heat resistance, and in addition to graphite, molybdenum, alumina, etc. can be used.

Further, in the above embodiment, the crucible 10 is made of birolytic boron nitride, but it is not limited to this, and aluminum nitride or the like may be used.

[Effects of the Invention] As explained above, according to the present invention, the following excellent effects are exhibited.

(1) Because they are reinforced by heat-resistant upper and lower jigs, the quartz upper and lower containers do not deform even if exposed to high temperatures for a long time.

(21) Since the quartz container is divided into upper and lower parts, the raw material remaining at the bottom of the container after single crystal growth can be easily removed.

(3) Therefore, the lifespan of the upper and lower containers can be extended. Therefore, the manufacturing cost of single crystals is reduced.

[BRIEF DESCRIPTION OF THE DRAWINGS] FIG. 1 is a configuration diagram of a compound semiconductor single crystal manufacturing apparatus according to an embodiment of the present invention, and FIGS. 2 and 3 are divided parts of an upper container and a lower container in other embodiments. FIG. 4 is a configuration diagram of a conventional example. In the figure, 1 is an upper container, 2 is a lower container, 3 is an upper jig, 4
1 is a lower jig, 5 is a rotating shaft and a pulling shaft, 7 is a sealing material, 10 is a crucible, 13 is a raw material, 15 is a seed crystal, and 16 is a single crystal.

Claims (4)

[Claims] (1) In a compound semiconductor single crystal production apparatus that grows a single crystal at the lower end of the seed crystal by heating and melting the raw material in a quartz container and raising the seed crystal in contact with the raw material with a rotating pulling shaft, An upper container and a lower container formed by dividing a quartz container into upper and lower parts, and a heat-resistant upper jig and a lower jig provided on the outer periphery of the upper container and the lower container so as to surround them, respectively; A crucible containing the raw material and placed in the lower container, interposed between the upper jig and the lower jig, and between the upper jig and the rotational pulling shaft, respectively. A compound semiconductor single crystal manufacturing device comprising: a sealing material for sealing. (2) The upper jig and the lower jig are made of graphite;
The manufacturing apparatus according to claim 1, characterized in that it is made of either molybdenum or alumina. (3) The manufacturing apparatus according to claim 1 or 2, wherein the crucible is made of bilolytic boron nitride or aluminum nitride. (4) Any one of claims 1 to 3, wherein the sealing material is made of boron oxide.
Manufacturing equipment as described in section.