JP5499888B2 - Gallium nitride crystal manufacturing apparatus gallium supply method and apparatus - Google Patents

Description

  The present invention relates to a gallium supply method and apparatus for a gallium nitride crystal manufacturing apparatus in which a gallium nitride crystal is manufactured by reacting gallium and nitrogen using a sodium flux.

As one method for producing a gallium nitride-based material used as a light-emitting device or a semiconductor device, a method for producing a gallium nitride (GaN) crystal using sodium (Na) flux and nitrogen gas (N ₂ ) as a nitrogen source Has been proposed.

  A gallium nitride crystal manufacturing apparatus used for manufacturing this type of gallium nitride crystal includes a gallium (Ga) melt (melted liquid) and a sodium (Na) melt (hereinafter referred to as a flux) in the pressure vessel. A reaction vessel for containing (reserving) a gallium melt (liquid Ga) and a sodium melt (liquid Na) is provided, and the pressure vessel is equipped with a heater for heating the reaction vessel. is there.

  Furthermore, a nitrogen gas supply pipe for supplying nitrogen gas into the pressure vessel is provided.

  When producing a gallium nitride crystal using the gallium nitride crystal production apparatus, the inside of the pressure vessel is set to 5-10 MPa in a state where nitrogen gas is supplied from the nitrogen gas supply pipe into the pressure vessel, and A reaction vessel containing liquid Ga and liquid Na is heated with a heater and maintained at a reaction condition of 600 to 1000 ° C. to react the gallium and nitrogen gas, and is provided in advance on the inner bottom of the reaction vessel. A gallium nitride crystal is grown with a certain seed crystal as a nucleus.

  When the gallium nitride crystal is grown as described above, the liquid Ga in the reaction vessel is consumed by the reaction with the nitrogen gas, and when the liquid Ga in the reaction vessel is depleted, the gallium nitride crystal grows. Will stop.

  In order to obtain a large gallium nitride crystal, the crystal growth of gallium nitride needs to be performed for a long time, and the required amount of liquid Ga for that purpose increases. In this case, if a large amount of liquid Ga is stored in the reaction vessel from the beginning, the size of the reaction vessel increases, so that the apparatus configuration is increased and a large amount of energy is required for heating the reaction vessel. .

  Therefore, it is proposed that the gallium nitride crystal manufacturing apparatus is provided with a gallium supply pipe for supplying liquid Ga into the reaction vessel disposed inside the pressure vessel from the outside of the pressure vessel. Has been.

  According to the gallium nitride crystal manufacturing apparatus having such a configuration, liquid Ga is supplied from the gallium supply pipe into the reaction vessel, and the amount corresponding to the consumption rate of liquid Ga accompanying the growth of the gallium nitride crystal in the reaction vessel; Thus, the gallium nitride crystal growth can be continued for a long time, for example, several hundred hours, even in a reaction vessel with a reduced capacity. Thus, a large gallium nitride crystal can be obtained.

  By the way, the production reaction of gallium nitride proceeds by contact of gallium and nitrogen in the presence of sodium. Therefore, in the gallium nitride crystal manufacturing apparatus of the type having the gallium supply pipe as described above, sodium vapor generated from the liquid Na contained in the reaction vessel and present in the pressure vessel, and the above Nitrogen gas supplied into the pressure vessel flows into the upstream side from the opening of the tip of the gallium supply pipe, and gallium nitride crystals are produced by contact of gallium and nitrogen in the presence of sodium at the inflow location. The reaction proceeds, and the gallium supply pipe may be blocked by the gallium nitride crystal generated by this reaction.

  Therefore, conventionally, except when the liquid Ga is dropped from the gallium supply pipe to the reaction vessel, the tip of the gallium supply pipe is covered, or the gallium supply pipe itself is positioned at the tip. Measures are taken to move to a region below the growth temperature of the gallium nitride crystal, or to move (increase) the interface of liquid Ga in the gallium supply pipe to a region below the growth temperature of the gallium nitride crystal. It is considered (for example, refer to Patent Document 1).

JP 2006-62947 A

  However, in the case shown in Patent Document 1, when adopting a method of covering the tip of the gallium supply pipe or a method of moving the gallium supply pipe itself, a movable part for carrying out each method is provided. There is a problem that the structure of the pressure vessel is complicated because the pressure vessel must be equipped with the equipped device.

  Further, when the supply of gallium is stopped, the method of moving the interface of liquid Ga in the gallium supply pipe to a region below the growth temperature of the gallium nitride crystal is in the space on the tip side of the interface of liquid Ga in the gallium supply pipe. Since sodium vapor and nitrogen gas enter from the opening of the tip, when the supply of liquid Ga through the gallium supply pipe is resumed, gallium nitride crystals are generated in the gallium supply pipe as described above. We cannot prevent fear.

  Therefore, the present invention can prevent the formation of gallium nitride crystals in the gallium supply tube without complicating the structure of the pressure vessel in the gallium nitride crystal manufacturing apparatus, and can block the gallium supply tube. It is an object of the present invention to provide a gallium supply method and apparatus for a gallium nitride crystal manufacturing apparatus capable of preventing the above.

In order to solve the above-mentioned problems, the present invention, corresponding to claim 1, contains sodium flux and gallium melt in a reaction vessel provided in the pressure vessel, and nitrogen gas is present in the pressure vessel. In such a pressure vessel, the pressure vessel in the gallium nitride crystal production apparatus is configured to produce gallium nitride crystals by pressurizing and heating sodium flux and gallium in the reaction vessel in the pressure vessel. A supply pipe is passed through the pressure vessel wall, the tip opening inserted inside the pressure vessel is arranged toward the inside of the reaction vessel, and a carrier gas is always circulated through the supply tube from the outside of the pressure vessel. is, the flow rate of the carrier gas to be circulated to the supply pipe, the flow rate of the carrier gas in the distal end opening portion of at least the feed pipe than the diffusion rate of the sodium vapor in the carrier gas Set to be faster, by conveying the molten gallium by the flow of the carrier gas flowing through the said feed pipe, and gallium supply method of the gallium nitride crystal manufacturing apparatus so as to supply to the reaction vessel.

  Further, in each of the above-described structures, nitrogen gas is used as the carrier gas to be present in the pressure-resistant container when the gallium nitride crystal is manufactured.

In each of the above configurations,
In the horizontal pipe provided on the upstream side of the supply pipe, a gallium melt is supplied so as to overflow from the gallium supply line connected to the lower end side position of the peripheral wall of the horizontal pipe from below, and the gallium melt is The carrier gas is blown away by the flow of the carrier gas flowing through the horizontal pipe.

  Similarly, in each of the above-described configurations, the gallium melt flowing down along the inner wall of the supply pipe is blown away by the flow of the carrier gas accelerated by the throttle portion that restricts the flow path area provided in the middle of the supply pipe. To be transported.

Corresponding to claim 5 , sodium flux and gallium melt are accommodated in a reaction vessel provided in the pressure vessel, and in the pressure vessel, nitrogen gas is present in the pressure vessel. The pressure vessel in the gallium nitride crystal manufacturing apparatus is configured to pressurize and heat the sodium flux and the gallium melt in the reaction vessel to produce a gallium nitride crystal, and the tip opening is the reaction vessel. A carrier pipe arranged so as to penetrate the inside of the pressure vessel wall through the pressure vessel wall so that the carrier gas can be constantly supplied to the base end side of the supply tube outside the pressure vessel connect the supply means, further, in the middle position of the flow path of the carrier gas, and connect the gallium supply line for supplying a melt of gallium, the carrier gas to flow through the feed pipe Fast and set as the flow rate of the carrier gas in the tip opening of at least the supply pipe is faster than the diffusion rate of the sodium vapor in the carrier gas, a gallium supplied to the supply pipe from the gallium supply line the melt, the gallium supply device of the gallium nitride crystal production apparatus having the configuration can be supplied onto the Symbol reaction vessel is transported by the flow of the carrier gas.

  Further, in the above configuration, the carrier gas supplied from the carrier gas supply means is configured to be nitrogen gas.

  Furthermore, in each of the above configurations, a horizontal pipe is provided on the upstream side of the supply pipe outside the pressure vessel, and a gallium supply line is connected to the lower end side position of the middle portion of the horizontal pipe from below, from the gallium supply line. The gallium melt supplied by overflowing into the horizontal pipe is blown off by the carrier gas flowing through the horizontal pipe and can be transported.

  Similarly, in each of the above-described configurations, a throttle portion that restricts the flow path area is provided in the middle of the pressure vessel of the supply pipe, and the gallium melt flowing down along the inner wall of the supply pipe is increased by the throttle portion. The carrier gas is blown away by the flow of the carrier gas to be transported.

According to the present invention, the following excellent effects are exhibited.
(1) Sodium flux and gallium melt are contained in a reaction vessel provided in the pressure vessel, and in the pressure vessel, nitrogen in the reaction vessel is contained in the pressure vessel. Pressurize and heat gallium flux and gallium nitride to produce gallium nitride crystals, and insert the supply pipe through the pressure vessel wall into the pressure vessel in the gallium nitride crystal manufacturing apparatus. The tip opening portion is disposed toward the inside of the reaction vessel, and the carrier gas is constantly circulated from the outside of the pressure vessel to the supply pipe , and the flow rate of the carrier gas to be circulated through the supply pipe is at least the supply carry the flow rate of the carrier gas in the distal end opening portion of the tube is set to be faster than the diffusion rate of the sodium vapor in the carrier gas, it flows through the supply tube A gallium supply method of a gallium nitride crystal manufacturing apparatus that transports a gallium melt by a gas flow and supplies the gallium melt to the reaction vessel, and a tip opening portion in the pressure vessel of the gallium nitride crystal manufacturing apparatus. A supply pipe arranged to face the inside of the reaction vessel is provided through the pressure vessel wall so that the carrier gas can be constantly supplied to the base end side of the supply tube outside the pressure vessel. A carrier gas supply means is connected, and further, a gallium supply line for supplying a gallium melt is connected to an intermediate position of the carrier gas distribution path, and the flow rate of the carrier gas to be circulated through the supply pipe is At least, the flow rate of the carrier gas at the tip opening of the supply pipe is set to be faster than the diffusion rate of sodium vapor in the carrier gas. The melt gallium supplied to the supply pipe from the gallium supply line, gallium supply of the gallium nitride crystal production apparatus having the configuration can be supplied onto the Symbol reaction vessel is transported by the flow of the carrier gas Since it is an apparatus, it is possible to prevent the sodium vapor existing in the pressure vessel from entering from the front end opening of the supply pipe, which is a path for supplying the melt of gallium to the reaction vessel. Since it is possible to prevent a reaction in which the gallium nitride crystal is generated in the supply pipe from proceeding, the possibility that the supply pipe is blocked by the gallium nitride crystal can be eliminated.
(2) Moreover, since it is not necessary to add a movable device configuration to the pressure vessel, it is possible to prevent the pressure vessel from being complicated.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows an embodiment of a gallium supply method and apparatus for a gallium nitride crystal manufacturing apparatus according to the present invention. FIG. It is a schematic diagram which shows the other form of implementation of this invention. FIG. 7 shows still another embodiment of the present invention, in which (A) is a schematic diagram showing the overall configuration, and (B) is a cut-away side view showing an enlarged portion B of (A).

  Hereinafter, embodiments for carrying out the present invention will be described with reference to the drawings.

  FIGS. 1A and 1B show an embodiment of the gallium supply method and apparatus of the gallium nitride crystal manufacturing apparatus according to the present invention.

  Here, the gallium nitride crystal manufacturing apparatus 1 to which the present invention is applied will be briefly described. The gallium nitride crystal manufacturing apparatus 1 is provided in the pressure vessel 2 and contains the liquid Na4 and liquid Ga5 (storage). And a heating means (not shown) such as a heater for heating the reaction vessel 3 in the pressure vessel 2.

  The gallium supply apparatus of the gallium nitride crystal production apparatus of the present invention applied to the gallium nitride crystal production apparatus 1 (hereinafter simply referred to as the gallium supply apparatus of the present invention) is connected to the pressure vessel 2 and the vessel wall of the pressure vessel 2. , For example, a supply pipe 6 that penetrates the upper part of the container wall in the inner and outer directions, and a tip opening serving as an inner end of the pressure-resistant container 2 in the supply pipe 6 is provided inside the reaction container 3. Place it toward the.

  One end of a horizontal pipe 7 that extends in the horizontal direction is connected to the base end side, which is the outer end of the pressure vessel 2 in the supply pipe 6, and the other end of the horizontal pipe 7 is used as a carrier gas. A carrier gas supply means 9 for supplying the nitrogen gas 8 is connected via a carrier gas line 10. As a result, the nitrogen gas 8 supplied from the carrier gas supply means 9 through the carrier gas line 10 can be always circulated through the horizontal pipe 7 and the supply pipe 6 and also passes through the supply pipe 6. The nitrogen gas 8 thus supplied can be supplied as a nitrogen source for producing a gallium nitride (GaN) crystal to the inside of the pressure vessel 2 from the opening at the tip of the supply pipe 6.

  Furthermore, the upstream side of the gallium supply line 12 with the supply pump 13 is placed in the gallium storage tank 11 in which the liquid Ga5 is stored as a thermostatic tank that can be maintained at a temperature higher than about 30 ° C., which is the melting point of gallium (Ga). Connect one end to be the end.

  A rising pipe 12a extending upward in the required dimension toward the downstream side is provided near the other end, which is closer to the downstream end of the gallium supply line 12, and the upper end of the rising pipe 12a is connected to the horizontal pipe 7. It is set as the structure connected to the lower end side position of the surrounding wall in the middle place. Thereby, the liquid Ga5 guided from the gallium reservoir 11 through the gallium supply line 12 by the operation of the supply pump 13 is caused to overflow from the upper end of the rising pipe 12a of the gallium supply line 12, so that the horizontal pipe 7 can be supplied to the inside.

  The flow rate of the nitrogen gas 8 supplied from the carrier gas supply means 9 and constantly flowing through the horizontal pipe 7 and the supply pipe 6 is such that the flow rate at the tip opening of the supply pipe 6 is at least sodium vapor. The liquid Ga5 is supplied to the horizontal pipe 7 from the upper end of the rising pipe 12a of the gallium supply line 12 so as to be faster than the diffusion speed in the nitrogen gas 8 which is a gas. It is assumed that the speed is set so that it can be blown off and made into a mist (droplet) and air-flow conveyed by the flow of nitrogen gas 8 as a carrier gas that circulates in the air.

  As a result, the liquid Ga5 introduced from the gallium reservoir 11 through the gallium supply line 12 and its riser pipe 12a by the operation of the supply pump 13 overflows from the upper end of the riser pipe 12a. When supplied to the inside, the liquid Ga5 is blown off by the nitrogen gas 8 flowing through the horizontal pipe 7 to be misted, and the mist of the liquid Ga5 is nitrogen gas flowing through the horizontal pipe 7 and the supply pipe 6 8, the liquid Ga5 mist discharged from the front end opening of the supply pipe 6 is transported to the front end opening of the supply pipe 6, and the liquid Na 4 stored in the reaction vessel 3. And liquid Ga5 can be supplied to the mixed liquid.

  14 is a gas replacement line for supplying nitrogen gas 8 from the carrier gas supply means 9 to the gallium storage tank 11 to replace the internal space of the gallium storage tank 11 with nitrogen gas, and 15 is the gallium storage tank 11 and gallium. A valve for cutting off the connection with the supply line 12, 16 is a valve for cutting off the communication between the rising pipe 12a of the gallium supply line 12 and the horizontal pipe 7, and 17 is the gallium supply line 12 during maintenance. This is a liquid gallium discharge line with an on-off valve 18 so that the liquid Ga5 in the inside can be extracted.

  Although not shown, the path through which the liquid Ga5 supplied from the gallium reservoir 11 reaches the reaction vessel 3 is all provided with a heating means, a heat retaining means, etc. It is assumed that a temperature higher than the melting point of melting gallium can be maintained.

  When the gallium nitride crystal manufacturing apparatus 1 equipped with the gallium supply apparatus of the present invention having the above-described configuration is used, nitrogen gas introduced from the carrier gas supply means 9 through the carrier gas line 10, the horizontal pipe 7 and the supply pipe 6. 8 is supplied into the pressure vessel 2, the pressure vessel 2 is set to 5-10 MPa, and the liquid Na 4 and the liquid Ga 5 serving as flux contained in the reaction vessel 3 provided in the pressure vessel 2 are added. The mixture is heated by a heating means such as a heater and maintained at a reaction condition of 600 to 1000 ° C. As a result, the gallium and nitrogen gas are reacted to grow a gallium nitride crystal (not shown) using a seed crystal (not shown) provided in advance in the inner bottom of the reaction vessel 3 as a nucleus.

  When the crystal of gallium nitride is grown as described above, the liquid Ga5 in the reaction vessel 3 is consumed. Therefore, the gallium nitride is adjusted so that the supply rate according to the consumption rate of the liquid Ga5 in the reaction vessel 3 is obtained. The supply pump 13 on the supply line 12 is operated continuously or intermittently. Thereby, the liquid Ga5 in the gallium reservoir 11 is supplied into the horizontal pipe 7 through the gallium supply line 12 and the rising pipe 12, and the liquid Ga5 supplied into the horizontal pipe 7 is supplied with the carrier gas. The supply means 9 leads to the horizontal pipe 7 through the carrier gas line 10 and is blown off by the flow of the nitrogen gas 8 flowing through the horizontal pipe 7 to be misted. Is supplied to the reaction vessel 3 in the pressure vessel 2 through the horizontal pipe 7 and the supply pipe 6.

  Therefore, in the reaction vessel 3, the liquid Ga5 is sequentially supplied in an amount corresponding to the consumption rate of the liquid Ga5 accompanying the growth of the gallium nitride crystal in the reaction vessel 3. By continuously performing for a long time, for example, several hundred hours, a large gallium nitride crystal can be obtained.

  At this time, the supply of the liquid Ga5 to the reaction vessel 3 is carried out by air current conveyance using the flow of the nitrogen gas 8 which is always circulated through the supply pipe 6, and the flow rate of the nitrogen gas 8 is increased. However, the sodium vapor existing in the pressure-resistant vessel 2 is supplied to the supply pipe 6 at a tip opening of the supply pipe 6 so as to be faster than the speed at which the sodium vapor diffuses in the nitrogen gas 8. The possibility of entering the inside of the pipe 6 and the horizontal pipe 7 on the upstream side thereof can be prevented. For this reason, since there is no sodium in the supply pipe 6 and the horizontal pipe 7, the progress of the reaction of generating a gallium nitride crystal with gallium and nitrogen is avoided.

  Thus, according to the gallium supply method and apparatus of the gallium nitride crystal manufacturing apparatus of the present invention, the supply pipe 6 and the horizontal pipe 7 which are pipes for supplying the liquid Ga5 to the reaction vessel 3 are connected to the inside of the pressure vessel 2. In this case, it is possible to prevent the sodium vapor generated from the liquid Na4 from entering, and to prevent the generation of gallium nitride crystals in the supply pipe 6 and the horizontal pipe 7. It is possible to eliminate the possibility that the horizontal tube 7 is blocked by the gallium nitride crystal.

  When the operation of the supply pump 13 on the gallium supply line 12 is stopped when the liquid Ga5 is not supplied to the reaction vessel 3, the gallium supply line is operated by the operation of the supply pump 13 up to that time. The liquid Ga5 that has already been supplied into the horizontal pipe 7 from the upper end of the 12 riser pipes 12a is all supplied to the reaction vessel 3 through the horizontal pipe 7 and the supply pipe 6 by airflow conveyance with nitrogen gas 8. Therefore, it is possible to prevent the liquid Ga5 from remaining inside the horizontal pipe 7 and the supply pipe 6. Therefore, the supply pipe 6 and the horizontal pipe 7 which are pipes for supplying the liquid Ga5 are made of gallium nitride. The possibility of being clogged by the crystals can be more reliably prevented.

  Moreover, since there is no need to add a movable device configuration as shown in Patent Document 1 to the pressure vessel 2, it is possible to prevent the pressure vessel 2 from being complicated.

  Further, since the nitrogen gas 8 is used as a carrier gas for carrying the mist of the liquid Ga5 by airflow, it is present in the pressure resistant vessel 2 when the gallium nitride crystal production reaction in the reaction vessel 3 proceeds. This eliminates the need to separately provide a supply pipe for supplying the necessary nitrogen gas 8 into the pressure vessel 2, so that the pressure vessel 2 can have a simpler configuration.

  In the above embodiment, a horizontal pipe 7 is provided on the upstream side of the supply pipe 6 attached to the pressure vessel 2 in order to carry the liquid Ga5 in an air flow, and the liquid is supplied from the gallium storage tank 11 in the middle of the horizontal pipe 7. The structure formed by connecting the upper end of the rising pipe 12a provided in the gallium supply line 12 that guides Ga5 is that the liquid Ga5 supplied to the horizontal pipe 7 is satisfactorily cut when the supply of the liquid Ga5 is stopped. Considering from the viewpoint, it is preferable to adopt this configuration. However, when the supply of liquid Ga5 is stopped as described above, when the liquid drainage performance is not so high, as shown in FIG. The downstream end of the rising pipe 12a is omitted, and the downstream end of the gallium supply line 12 is connected to the horizontal pipe 7 from above. Unishi may be.

  Other configurations in FIG. 2 are the same as those shown in FIG. 1A, and the same components are denoted by the same reference numerals.

  Even in such a configuration, as in the embodiment shown in FIGS. 1 (a) and 1 (b), the supply pipe 6 and the horizontal pipe 7 which are pipes for supplying the liquid Ga5 to the reaction vessel 3 are connected to the pressure vessel. 2 can prevent the sodium vapor existing in 2 from entering, so that the possibility that the supply pipe 6 and the horizontal pipe 7 may be blocked by crystals of gallium nitride can be eliminated, and the structure of the pressure vessel 2 can be reduced. The effect that it does not become complicated can be acquired.

  Further, in the embodiment shown in FIGS. 1A and 1B, when the liquid Ga5 guided through the gallium supply line 12 and its rising pipe 12a is supplied into the horizontal pipe 7, the liquid Ga5 is supplied to the horizontal pipe. 7 shows a configuration in which the gas is blown off by the nitrogen gas 8 serving as a carrier gas flowing through the inside of the gas generator 7 to be misted. However, if the liquid Ga5 can be blown off to be misted, FIG. 1 (A) (B) In place of the configuration in which the upper end of the rising pipe 12a, which is the downstream end of the gallium supply line 12, is connected to the horizontal pipe 7 provided on the upstream side of the supply pipe 6 as shown in FIG. (B) As shown in (b), a liquid Ga5 supplied from the gallium supply line 12 by connecting the downstream end of the gallium supply line 12 to an inclined tube 19 provided on the upstream side of the supply pipe 6. But While flowing down (along) along the inner surfaces of the oblique pipe 19 and the supply pipe 6, the supply pipe 6 is circulated by narrowing the flow path area at a position near the lower end of the supply pipe 6. A throttle portion 20 that can accelerate the flow velocity of the nitrogen gas 8 is provided, and the inner surface of the inclined tube 19 and the supply pipe 6 is made to flow as described above by the flow of the nitrogen gas 8 accelerated by the throttle portion 20. A configuration may also be adopted in which the liquid Ga5 that has flowed down to the throttle unit 20 is blown off to be misted.

  3A and 3B, the sodium vapor existing in the pressure-resistant vessel 2 is supplied to the supply pipe 6 in the same manner as the embodiment shown in FIGS. The possibility that the supply pipe 6 for supplying the liquid Ga5 to the reaction vessel 3 may be blocked by the crystal of gallium nitride can be eliminated, and the pressure vessel 2 can be prevented. It is possible to obtain an effect that the configuration of the system is not complicated.

  Furthermore, the present invention is not limited only to the above embodiment, and the case where nitrogen gas 8 is used as a carrier gas for air-transporting liquid Ga5 has been described. The gas Ga 5, the liquid Na 4 used as a flux, the reactivity with the nitrogen gas 8, and the gas not reactive with gallium nitride, such as hydrogen or a Group 18 element (inert gas), nitrogen gas 8 Other carrier gases may be used. As described above, when a gas other than the nitrogen gas 8 is used as the carrier gas, a nitrogen gas supply line for supplying the nitrogen gas used as a nitrogen source when the gallium nitride generation reaction proceeds to the pressure resistant vessel 2; A separately connected configuration may be used.

  The ratios and shapes of the components of the pressure vessel 2 and the reaction vessel 3 of the gallium nitride crystal manufacturing apparatus shown in FIGS. 1 (a), (b), 2 and 3 (a) and (b) are as follows. This is for the convenience of illustration, and does not limit the size or shape of each component device in an actual apparatus.

  Of course, various modifications can be made without departing from the scope of the present invention.

DESCRIPTION OF SYMBOLS 1 Gallium nitride crystal manufacturing apparatus 2 Pressure-resistant container 3 Reaction container 4 Liquid Na (sodium flux)
5 Liquid Ga (Gallium melt)
6 Supply pipe 7 Horizontal pipe 8 Nitrogen gas (carrier gas)
9 Carrier gas supply means 12 Gallium supply line 20 Restriction section

Claims (8)

Sodium flux and gallium melt are contained in a reaction vessel provided in the pressure vessel, and in the state where nitrogen gas is present in the pressure vessel, the sodium flux in the reaction vessel is contained in the pressure vessel. In the gallium nitride crystal manufacturing apparatus in which gallium nitride is manufactured by pressurizing and heating gallium, the tip opening is inserted through the pressure vessel wall and inserted into the pressure vessel. The carrier gas is continuously circulated from the outside of the pressure vessel to the supply pipe , and the flow rate of the carrier gas to be circulated through the supply pipe is set at least at the tip of the supply pipe. carrier gas flow rate of the carrier gas at the opening is set to be faster than the diffusion rate of the sodium vapor in the carrier gas, it flows through the supply tube By conveying the molten gallium by the flow, gallium supply method of the gallium nitride crystal manufacturing apparatus which is characterized in that to supply to the reaction vessel. As the carrier gas, a gallium supply method according to claim 1 gallium nitride crystal manufacturing apparatus according to to use a nitrogen gas for existing in the pressure vessel during the production of crystals of gallium nitride. In the horizontal pipe provided on the upstream side of the supply pipe, a gallium melt is supplied so as to overflow from the gallium supply line connected to the lower end side position of the peripheral wall of the horizontal pipe from below, and the gallium melt is The gallium supply method of a gallium nitride crystal manufacturing apparatus according to claim 1 or 2 , wherein the gallium nitride crystal manufacturing apparatus is carried by being blown away by a flow of a carrier gas flowing through the horizontal pipe. The melt gallium flowing down along the inner wall of the supply pipe, so as to convey blowing by the flow of carrier gas is accelerated by the throttle portion throttling the flow area provided in the middle position of the supply pipe according to claim 1 Or the gallium supply method of the gallium nitride crystal manufacturing apparatus of 2 or 2 . Sodium flux and gallium melt are contained in a reaction vessel provided in the pressure vessel, and in the state where nitrogen gas is present in the pressure vessel, the sodium flux in the reaction vessel is contained in the pressure vessel. Pressurized and heated gallium melt to produce a gallium nitride crystal so that a tip opening is disposed in the pressure vessel in the gallium nitride crystal production apparatus facing the inside of the reaction vessel. A carrier gas supply means provided so that a carrier gas can be constantly supplied to the base end side of the supply pipe outside the pressure vessel, and the carrier pipe is further provided. in the middle position of the flow path of the gas, connecting the gallium supply line for supplying a melt of gallium, the flow rate of the carrier gas to flow through the feed tube, at least the test And flow rate of the carrier gas in the distal end opening portion of the tube is set to be faster than the diffusion rate of the sodium vapor in the carrier gas, a melt of gallium supplied to the supply pipe from the gallium supply line, the gallium feeder of the gallium nitride crystal manufacturing apparatus characterized by having the structure can be supplied onto the Symbol reaction vessel is transported by the flow of carrier gas. The gallium supply apparatus for a gallium nitride crystal manufacturing apparatus according to claim 5 , wherein the carrier gas supplied from the carrier gas supply means is nitrogen gas. A horizontal pipe is provided on the upstream side of the supply pipe outside the pressure vessel, and a gallium supply line is connected to the lower end side position of the horizontal pipe from below, and is supplied by overflowing from the gallium supply line into the horizontal pipe. The gallium supply apparatus of a gallium nitride crystal manufacturing apparatus according to claim 5 or 6 , wherein the gallium melt to be blown off can be transported by a carrier gas flowing in the horizontal pipe. A throttle part that restricts the flow path area is provided at an intermediate position inside the pressure vessel of the supply pipe, and the gallium melt flowing down along the inner wall of the supply pipe is caused by the flow of the carrier gas accelerated by the throttle part. The gallium supply apparatus for a gallium nitride crystal manufacturing apparatus according to claim 5 or 6 , wherein the gallium nitride crystal manufacturing apparatus can be blown away and conveyed.

Images