CN117867636A - Gallium oxide crystal manufacturing device and manufacturing method based on heat exchange method - Google Patents

Abstract

The invention discloses a gallium oxide crystal manufacturing device and a gallium oxide crystal manufacturing method based on a heat exchange method, wherein the gallium oxide crystal manufacturing device comprises a box body, a crucible frame, a heating component and a sealing cover, a crystal taking door is arranged on the box body, a crucible is arranged in the crucible frame, and a first heat dissipation channel is arranged at the bottoms of the crucible and the crucible frame; the heating component is arranged in the box body and surrounds the crucible frame; the sealing cover is arranged in the box body and can move up and down in the box body towards the crucible frame, a fixing component for fixing seed crystals is arranged in the sealing cover, and a second heat dissipation channel is arranged in the sealing cover; the first heat dissipation channel is internally provided with a first heat dissipation component, and the second heat dissipation channel is internally provided with a second heat dissipation component. According to the invention, the heat of the upper layer and the lower layer of the gallium oxide crystal is reduced through the first heat dissipation component and the second heat dissipation component, the growth stability of the gallium oxide crystal is improved, and the gallium oxide crystal similar to the crucible in shape can be better grown.

Description

Gallium oxide crystal manufacturing device and manufacturing method based on heat exchange method

Technical Field

The invention relates to the technical field of crystal manufacturing, in particular to a gallium oxide crystal manufacturing device based on a heat exchange method and a manufacturing method thereof.

Background

Gallium oxide has received continuous attention as an "ultra wide band gap semiconductor" material. The ultra-wide band gap semiconductor also belongs to a fourth-generation semiconductor, and compared with the third-generation semiconductor silicon carbide and gallium nitride, the band gap of gallium oxide reaches 4.9eV, and the wider band gap means that electrons need more energy to transition from valence band to conduction band, so that the gallium oxide has the characteristics of high voltage resistance, high temperature resistance, high power, radiation resistance and the like. And under the same specification, the wide forbidden band material can manufacture devices with smaller die size and higher power density, saves matched heat dissipation and wafer area, and further reduces the cost.

At present, the existing gallium oxide crystal growth modes are various, and the heat exchange method has the advantages that the interface is stable, no mechanical disturbance exists during the growth of the gallium oxide crystal, the buoyancy convection is small, so that the defects generated by the crystal growth can be reduced, the thermal stress of the crystal can be well reduced, however, the existing heat exchange technology mainly grows from bottom to top, the crystal size is small, the crystal is thicker, the cutting is difficult, and the damage is very easy to occur, so that a device for solving the problems is needed.

Accordingly, the prior art is still in need of improvement and development.

Disclosure of Invention

The invention aims to solve the technical problems that the gallium oxide crystal manufacturing device and the gallium oxide crystal manufacturing method based on a heat exchange method are provided for overcoming the defects of the prior art, and aims to solve the problems that the gallium oxide crystal manufactured in the prior art is smaller in size, thicker in crystal and difficult to cut.

The technical scheme adopted for solving the technical problems is as follows:

a gallium oxide crystal production apparatus based on a heat exchange method, comprising:

the box body is provided with a crystal taking door;

the crucible rack is arranged in the box body, a crucible for placing gallium oxide solids is arranged in the crucible rack, and a first heat dissipation channel is arranged at the bottoms of the crucible and the crucible rack;

the heating assembly is arranged in the box body and surrounds the crucible frame;

the sealing cover is arranged in the box body and can move up and down in the box body towards the crucible frame, a fixing component for fixing seed crystals is arranged in the sealing cover, and a second heat dissipation channel is arranged in the sealing cover;

the first heat dissipation channel is internally provided with a first heat dissipation component for taking away the growth heat of the gallium oxide crystals, and the second heat dissipation channel is internally provided with a second heat dissipation component for taking away the growth heat of the gallium oxide crystals.

In an improvement of a gallium oxide crystal manufacturing apparatus based on a heat exchange method, the first heat dissipation assembly includes:

one end of the first air inlet pipe is connected with the first heat dissipation channel, the other end of the first air inlet pipe extends out of the box body and is connected with an external cold source, and the first air inlet pipe is used for inputting cold air;

the first air outlet holes are formed in the peripheral wall of the crucible frame where the first heat dissipation channel is located.

In an improvement of the gallium oxide crystal manufacturing apparatus based on the heat exchange method, the second heat dissipation assembly includes:

one end of the second air inlet pipe is connected with the second heat dissipation channel, the other end of the second air inlet pipe extends out of the box body and is connected with an external cold source, and the second air inlet pipe is used for inputting cold air;

the second air outlet holes are formed in the peripheral wall of the sealing cover where the second heat dissipation channel is located;

wherein the second air inlet pipe is a deformation telescopic pipe.

In an improvement mode of the gallium oxide crystal manufacturing device based on the heat exchange method, the manufacturing device further comprises a telescopic assembly, the telescopic assembly is arranged on the box body, and the telescopic assembly is connected with the sealing cover and can enable the sealing cover to move in a telescopic manner towards the crucible frame.

In an improvement of a gallium oxide crystal manufacturing apparatus based on a heat exchange method, the expansion assembly includes:

the hydraulic shell is fixed on the box body;

the hydraulic cylinder is fixed in the hydraulic shell;

one end of the hydraulic rod is in driving connection with the hydraulic cylinder, and the other end of the hydraulic rod penetrates through the box body, extends into the box body and is connected with the sealing cover.

In an improved mode of a gallium oxide crystal manufacturing device based on a heat exchange method, a plurality of shock absorption columns are arranged in a box body, and a plurality of crucible frames are arranged on the shock absorption columns.

In an improvement of a gallium oxide crystal manufacturing apparatus based on a heat exchange method, the fixing member includes:

the telescopic members are circumferentially arranged along the inner wall of the sealing cover and surround to form a clamping channel;

the fixed station, detachable set up in the centre gripping passageway, the fixed station is provided with detachable seed crystal.

In an improvement of a gallium oxide crystal manufacturing apparatus based on a heat exchange method, the heating assembly includes:

and the heating pipes are arranged in the box body and are circumferentially arranged along the circumferential path of the crucible frame.

In an improved mode of a gallium oxide crystal manufacturing device based on a heat exchange method, a plurality of clamping blocks are arranged in a sealing cover, a plurality of clamping grooves are formed in a crucible, the clamping blocks are clamped with the clamping grooves, and the sealing cover is fixedly connected with a crucible frame.

A method for manufacturing a gallium oxide crystal manufacturing apparatus according to any one of the above embodiments, comprising:

fixing seed crystals on the fixing component, and putting preset gallium oxide solids into a crucible;

controlling a heating component to heat the preset gallium oxide solid, wherein the preset gallium oxide solid is melted into a gallium oxide melt;

the telescopic component is controlled to push the sealing cover to be fixedly butted with the crucible frame, and the seed crystal and the gallium oxide melt are contacted and reacted to form gallium oxide crystals; simultaneously, the first heat dissipation component is controlled to cool the sealing cover, and the second heat dissipation component is controlled to cool the crucible frame;

after the growth time is reached, the first heat dissipation assembly and the second heat dissipation assembly are controlled to be closed; the growth time is determined according to the air inlet flow of the first heat dissipation assembly and the second heat dissipation assembly, and the air inlet flow is determined according to the heat emitted by the gallium oxide crystal;

and (3) moving up the sealing cover, and taking out the gallium oxide crystal on the crucible.

The beneficial effects are that:

the crystal growth direction of the invention is different from the traditional heat exchange method, crystal growth is carried out by diffusing from the center to the periphery, and cold air is simultaneously input into the first heat dissipation channel and the second heat dissipation channel, and as gallium oxide solid and seed crystal reaction positions are positioned between the first heat dissipation channel and the second heat dissipation channel, the heat quantity of growth of the upper surface and the lower surface of gallium oxide crystal can be reduced, the instability of growth of gallium oxide crystal is reduced, the sealing cover is accurately abutted with the crucible frame, the probability of defect occurrence of gallium oxide crystal caused by mechanical displacement of the device can be reduced, and gallium oxide crystal similar to the crucible in shape can be better grown.

Drawings

Fig. 1 is a schematic perspective view of a gallium oxide crystal manufacturing apparatus according to the heat exchange method;

FIG. 2 is a schematic view of the external structure of the sealing cover and the crucible frame provided by the invention;

FIG. 3 is a schematic view of the internal structure of the seal cap and crucible frame provided by the invention;

FIG. 4 is a cross-sectional view at A of FIG. 2;

FIG. 5 is a cross-sectional view at B of FIG. 2;

FIG. 6 is a graph of gas flow versus time in the present invention.

Reference numerals illustrate:

1. a case; 2. taking a crystal gate; 3. a telescoping assembly; 310. a hydraulic cylinder; 320. a hydraulic rod; 330. a hydraulic housing; 4. a second heat dissipation assembly; 410. a second air inlet pipe; 420. a second air outlet hole; 5. a first heat dissipation assembly; 510. a first air inlet pipe; 520. a first air outlet hole; 6. sealing cover; 7. a fixing assembly; 710. a chuck; 720. a telescopic column; 730. a spring; 740. a fixed table; 8. seed crystal; 9. a crucible; 10. a crucible holder; 11. a heating assembly; 12. a second heat dissipation channel; 13. gallium oxide solids; 14. a clamping block; 15. a clamping groove.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more clear and clear, the present invention will be further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.

Referring to fig. 1-5, the present invention provides a gallium oxide crystal manufacturing apparatus based on a heat exchange method.

As shown in fig. 1 to 2, the gallium oxide crystal manufacturing device comprises a box body 1, a crucible frame 10, a heating component 11 and a sealing cover 6, wherein a crystal taking door 2 is arranged on the box body 1, and the crystal taking door 2 is used for opening or closing the box body 1 so as to be convenient for taking formed gallium oxide crystals; the box body 1 is in a cylindrical shape, and is internally provided with a cavity, and is made of heat-resistant materials, such as stainless steel or heat-resistant plastics, so that the influence of the heating component 11 on the crucible frame 10 is reduced, and the crucible frame 10 is prevented from being deformed by heat. The crucible frame 10 is arranged at the bottom in the box body 1, a crucible 9 for placing gallium oxide solids 13 is arranged in the crucible frame 10, and the crucible 9 is detachably connected with the crucible frame 10, so that gallium oxide crystals in the crucible 9 after growth can be conveniently taken out; the bottom of the crucible frame 10 and the bottom of the crucible 9 are provided with a first heat dissipation channel, and it can be understood that the first heat dissipation channel refers to a distance between the inner wall of the bottom of the crucible frame 10 and the bottom of the crucible 9, and the distance can be selected and set according to actual requirements, for example, 5cm, 4cm, and 3cm are different. The heating component 11 is arranged in the box body 1 and is circumferentially arranged around the crucible frame 10, so that gallium oxide solids 13 in the crucible 9 of the crucible frame 10 can be heated, the heating effect is better, and the heating is uniform. The sealing cover 6 is arranged in the middle of the box body 1 and can move up and down in the box body 1 towards the crucible frame 10, so that the sealing cover 6 can seal the crucible 9 on the crucible frame 10. A fixing component 7 for fixing seed crystals 8 is arranged in the sealing cover 6, the sealing cover 6 is composed of a first round table and a second round table, the first round table is arranged above the second round table, the first round table and the second round table are both provided with cavities, the diameter of the first round table is smaller than that of the second round table, and the fixing component 7 is arranged on the second round table; a second heat dissipation channel 12 is arranged in the sealing cover 6, and the second heat dissipation channel 12 refers to all cavities of the first round table and the second round table except the fixing component 7; the first heat dissipation channel is internally provided with a first heat dissipation component 5 for taking away the growth heat of the gallium oxide crystal, the heat of the upper layer of the gallium oxide crystal is reduced through the first heat dissipation component 5, the second heat dissipation channel 12 is internally provided with a second heat dissipation component 4 for taking away the growth heat of the gallium oxide crystal, and the heat of the lower layer of the gallium oxide crystal is reduced through the second heat dissipation component 4.

In this embodiment, a suitable seed crystal 8 and a gallium oxide solid 13 are selected, the seed crystal 8 is fixed on the fixing component 7 in the sealing cover 6, the gallium oxide solid 13 is installed in the crucible 9 on the crucible frame 10, and the gallium oxide solid 13 refers to gallium oxide powder solid. Firstly, the heating component 11 heats gallium oxide solid 13 in the crucible 9 to enable gallium oxide to be fixedly melted into gallium oxide melt, then the sealing cover 6 is pushed to be in butt joint with the crucible frame 10 to be closed, the seed crystal 8 and the gallium oxide melt are contacted and reacted to form gallium oxide crystals, meanwhile, the first heat dissipation component 5 and the second heat dissipation component 4 are controlled to be opened, the first heat dissipation component 5 cools down the first heat dissipation channel, the second heat dissipation component 4 cools down the second heat dissipation channel 12, heat of an upper layer and a lower layer in the gallium oxide crystal growth process is reduced, thermal stress in the gallium oxide crystal growth process is reduced, and therefore stability of gallium oxide crystal growth is improved.

As shown in fig. 2 and 3, in a preferred embodiment of the present invention, the first heat dissipating module 5 includes a first air inlet pipe 510 and a first air outlet 520, one end of the first air inlet pipe 510 is connected to the center of the first heat dissipating channel, and the other end extends to the outside of the case 1 and is connected to an external cold source, wherein the first air inlet pipe 510 is used for inputting cold air, and the external cold source is a device for delivering cold air, such as a refrigerator; it is noted that the air inlet of the first air inlet pipe 510 is located at the middle of the crucible frame 10 so that cool air enters the first heat dissipation passage in the crucible frame 10 from the middle. The plurality of first air outlet holes 520 are all arranged on the peripheral wall of the crucible frame 10 where the first heat dissipation channel is located, and are uniformly distributed, so that the input cool air dissipates heat from the peripheral wall of the crucible frame 10, and the effect that the cool air enters from the first air inlet pipe 510 in the middle and flows out of the first air outlet holes 520 on the peripheral wall of the crucible frame 10 is formed, thereby being beneficial to the production and the manufacture of gallium oxide crystals. In addition, a first valve is provided on the first intake pipe 510 for controlling intake of the first intake pipe 510.

As shown in fig. 1 to 3, in a preferred embodiment of the present invention, the second heat dissipating assembly 4 includes a second air inlet pipe 410 and a second air outlet 420, the air inlet of the second air inlet pipe 410 is located in the middle of the sealing cover 6, preferably, two second air inlet pipes 410 are provided, the two second air inlet pipes 410 are respectively installed at the left side and the right side of the case 1, the air inlets of the two second air inlet pipes 410 are connected to each other and form an air inlet located in the middle of the sealing cover 6, the two second air inlet pipes 410 are connected to an external cold source, and by providing two second air inlet pipes 410 to make the air intake amount more, the second air inlet pipes 410 are used for inputting cold air, and cold air inlets are formed on the peripheral wall of the sealing cover 6 of the seed crystal 8, i.e., the air inlets of the second air inlet pipes 410 and the seed crystal 8 are arranged in concentric circles. The second air outlet holes 420 are all arranged on the peripheral wall of the sealing cover 6 where the second heat dissipation channel 12 is located, and the intervals between the adjacent second air outlet holes 420 are the same, so that the heat of the gallium oxide crystal can be dissipated from the peripheral wall of the sealing cover 6, and the upper surface of the gallium oxide crystal is cooled conveniently. The second air inlet pipe 410 is a deformed telescopic pipe, that is, the second air inlet pipe 410 is equivalent to a hose, and has better elasticity, so that the sealing cover 6 does not affect the connection stability of the second air inlet pipe 410 when moving, and it can be understood that the second air inlet pipe 410 may also be a bent corrugated pipe. In addition, due to the arrangement of the heat dissipation of the peripheral wall by adopting the cold air which is introduced in the middle, the growth stability of the upper surface of the gallium oxide crystal during growth can be effectively improved. It should be noted that, each second air inlet pipe 410 is provided with a second valve, and the second valve is used for controlling the opening and closing of the second air inlet pipe 410, so as to control the input cold air.

In the above two embodiments, the external cold sources of the first air inlet pipe 510 and the second air inlet pipe 410 are the same, that is, the first air inlet pipe 510 and the second air inlet pipe 410 are connected to the same refrigeration device, the refrigeration device is a refrigerator, the cool air of the refrigerator adopts helium, and the helium is colorless and odorless, which is easy to manufacture and has low cost. In this application, through the input air of same outside cold source, reduce cost, only need several pipelines can be with first intake pipe 510 and second intake pipe 410 connection, simple structure, convenient to use.

As shown in fig. 2 and 3, in a preferred embodiment of the present invention, the manufacturing apparatus further includes a telescopic assembly 3, the telescopic assembly 3 is disposed on the case 1, and the telescopic assembly 3 is connected to the sealing cover 6, so that the sealing cover 6 can move telescopically toward the crucible frame 10. In the present application, the telescopic assembly 3 is used for moving the sealing cover 6, and the telescopic assembly 3 has various types, such as an electric telescopic rod, a hydraulic telescopic rod, etc., and a person skilled in the art can select the setting according to actual requirements.

As shown in fig. 2 and 3, in a preferred embodiment of the present invention, the telescopic assembly 3 further includes a hydraulic housing 330, a hydraulic cylinder 310 and a hydraulic rod 320, wherein the hydraulic housing 330 is fixed on the case 1 and is located at a middle position of the case 1, the hydraulic cylinder 310 is fixed in the hydraulic housing 330, and the hydraulic cylinder 310 is protected from others or foreign objects through the hydraulic housing 330. One end of the hydraulic rod 320 is in driving connection with the hydraulic cylinder 310, the other end of the hydraulic rod 320 penetrates through the box body 1 to extend to the middle in the box body 1 and is fixedly connected with the center of the sealing cover 6, such as welding or bolting, and as the hydraulic rod 320 is connected with the center of the sealing cover 6, the stress at each position of the sealing cover 6 is uniform, the lifting is more stable, and the sealing cover 6 is prevented from shaking.

As shown in fig. 2 and 3, in a preferred embodiment of the present invention, a plurality of shock-absorbing columns are disposed in the case 1, the number of shock-absorbing columns may be selected according to practical requirements, for example, three, four, five, etc., in this application, preferably 2 shock-absorbing columns are disposed on the left side and the right side of the crucible frame 10, and are symmetrical along the center of the case 1, and the two shock-absorbing columns support the crucible frame 10, raise the position of the crucible frame 10 in the case 1, so that the first air inlet pipe 510 may be directly connected to the bottom center position of the crucible frame 10, thereby facilitating the observation of a user, reducing the installation difficulty of the first air inlet pipe 510, and simultaneously, reducing the pressure applied to the first air inlet pipe 510 due to the provision of the shock-absorbing columns, and avoiding the gravity of the crucible frame 10 and the crucible 9 from being applied to the first air inlet pipe 510. More specifically, the shock-absorbing column includes first post, second post and damping spring 730, and the bottom in box 1 is fixed to first post, installs the second post that can follow first post and remove on the first post, and first post and second post are gone up and are overlapped jointly and are equipped with damping spring 730, and damping spring 730 can effectually reduce the vibration influence of crucible frame 10.

As shown in fig. 2 to 4, in a preferred embodiment of the present invention, the fixing assembly 7 includes a plurality of telescopic members and a fixing table 740, the plurality of telescopic members are circumferentially arranged along the inner wall of the sealing cover 6, the distance between each telescopic member is equal, and the plurality of telescopic members surround to form a clamping channel, preferably, in this application, the number of telescopic members is set to 3, so that the clamping of the telescopic members is more stable. The fixed stage 740 is detachably arranged in the clamping channel, and the detachable seed crystal 8 is arranged on the fixed stage 740, so that the seed crystal 8 and the fixed stage 740 can be detached, and a user can conveniently take and put the seed crystal 8. It can be appreciated that, in order to fix the clamping channel and the fixing table 740 more firmly, the end of the telescopic member is provided with a bolt, the fixing table 740 is provided with a slot corresponding to the bolt, and the bolt of the telescopic member is inserted into the slot of the fixing table 740, so that the fixing table 740 is fixed firmly, and the fixing table 740 is ensured not to fall off.

As shown in fig. 2 and 3, in a preferred embodiment of the present invention, the heating assembly 11 includes heating pipes disposed within the case 1 and circumferentially arranged along the circumferential path of the crucible frame 10. Specifically, the heating pipe is current heater strip, and the heating pipe has the three-layer, arranges along the direction of height of box 1, and the heating pipe is in concentric different diameter's circular position with crucible frame 10, ensures that each position is heated evenly around crucible frame 10 for gallium oxide solid 13 in the crucible 9 is heated evenly, and gallium oxide solid 13 melts into gallium oxide fuse-element more easily, accelerates the melting rate of gallium oxide solid 13.

As shown in fig. 4 and 5, in a preferred embodiment of the present invention, a plurality of clamping blocks 14 are disposed in the sealing cover 6, a plurality of clamping grooves 15 are disposed on the crucible 9, and the clamping blocks 14 are clamped with the clamping grooves 15, so as to fixedly connect the sealing cover 6 with the crucible frame 10. In this application, the fixture block 14 of sealed lid 6 is located sealed lid 6 perisporium bottom, evenly is provided with a plurality of, and crucible 9 sets up the draw-in groove 15 with fixture block 14 corresponding quantity for sealed lid 6 and crucible 9's block connection through sealed lid 6 for sealed lid 6 and crucible frame 10 butt joint are accurate.

The device of the invention has the following application principle:

selecting a proper seed crystal 8 to be placed in a fixed table 740, selecting a proper gallium oxide solid 13 to be placed in a crucible 9, firstly controlling a heating component 11 to heat the gallium oxide solid 13, and melting the gallium oxide solid 13 into a gallium oxide melt when the heating temperature is higher than the melting point of the gallium oxide solid 13; then the telescopic component 3 is controlled to push the sealing cover 6 to move towards the crucible frame 10, the first air inlet pipe 510 is driven to deform and stretch, seed crystals 8 on the sealing cover 6 react with gallium oxide melt in the crucible 9 to form gallium oxide crystals, meanwhile, cold air with preset flow is introduced into the first air inlet pipe 510 and the second air inlet pipe 410, the cold air enters from the middle of the upper layer and the lower layer of the gallium oxide crystals, heat in the middle of the upper layer and the lower layer is taken away, and then the cold air is dissipated from the first air outlet holes 520 and the second air outlet holes 420 around the upper layer and the lower layer;

when the preset gallium oxide crystal growth time is reached, the air inlet of the first air inlet pipe 510 and the second air inlet pipe 410 is cut off, the crystal taking door 2 on the box body 1 is opened, the telescopic component 3 is controlled to push the sealing cover 6 to move towards the direction away from the crucible frame 10, the crucible 9 in the crucible frame 10 is taken out, and the grown gallium oxide crystal is taken out from the crucible 9.

The present invention also provides a method for manufacturing a gallium oxide crystal manufacturing apparatus according to any one of the above aspects, comprising:

s100, fixing seed crystals on a fixing assembly, and putting preset gallium oxide solids into a crucible;

s200, controlling a heating component to heat the preset gallium oxide solid, wherein the preset gallium oxide solid is melted into a gallium oxide melt;

s300, controlling the telescopic component to push the sealing cover to be in butt joint with the crucible frame for fixation, and enabling the seed crystal to be in contact reaction with the gallium oxide melt for forming gallium oxide crystals; simultaneously, the first heat dissipation component is controlled to cool the sealing cover, and the second heat dissipation component is controlled to cool the crucible frame;

s400, after the growth time is reached, controlling the first heat dissipation assembly and the second heat dissipation assembly to be closed; the growth time is determined according to the air inlet flow of the first heat dissipation assembly and the second heat dissipation assembly, and the air inlet flow is determined according to the heat emitted by the gallium oxide crystal;

s500, moving up the sealing cover, and taking out the gallium oxide crystal on the crucible.

The invention also provides a manufacturing method of the gallium oxide crystal manufacturing device according to any one of the above technical schemes, and the gallium oxide crystal manufacturing device based on the heat exchange method according to any one of the above technical schemes is provided, so that all the above beneficial effects are provided, and the description is omitted. Further, the gallium oxide melt refers to a molten state generated when gallium oxide powder reaches a melting point.

As can be seen from the above embodiments, the growth time is determined according to the air intake flow rates of the first heat dissipation component and the second heat dissipation component, the air intake flow rate is determined according to the heat released by the preset gallium oxide crystal, and an embodiment will be described in detail below.

Assuming that a gallium oxide single crystal of 4 inches and a thickness of 10mm was grown, the volume of the single crystal was V _Crystal ＝81.03cm ³ Density ρ of gallium oxide _{Gallium oxide} ＝5.9g/cm ³ The mass of the single crystal is m _Crystal =478 g. Specific heat capacity c of gallium oxide _{Ratio of} =5.19J/g, melting point 1740 ℃, assuming initial temperature of gallium oxide is 1800 ℃, the heat evolved when cooling to 1740 ℃ is:

Q _{lowering blood pressure} ＝c _{Ratio of} *m _Crystal (t _{Initially, the method comprises} -t _{Powder (D)} )；

＝5.19J/g×478g×(1800-1740℃)＝148849J≈149KJ；

The crystallization latent heat is the heat released when a unit mass of a substance is converted from a liquid state to a solid state under the condition that the temperature is kept unchanged, and the crystallization latent heat of gallium oxide is as follows:

Q _{diving device} ＝4.6×10 ⁵ J/kg；

Gallium oxide is solid-liquid coexisting phase at 1740 ℃, and the heat released by the crystallization of gallium oxide single crystal is:

Q _{put =} m _Crystal *Q _{Diving device} ＝478g×4.6×10 ⁵ J/Kg＝219880J≈220KJ；

To sum up, gallium oxide crystallization requires heat release Q _{Total (S)} ＝Q _{Fall +} Q _{Put =} 149KJ+220KJ＝369KJ。

Helium is used to remove heat evolved by gallium oxide crystallization, known as gallium oxide having a constant pressure heat capacity c at room temperature of 20 DEG C _{Fixing device} Given an initial inlet temperature of helium of 20 ℃, an outlet temperature of 220 ℃, only 20% of helium is used for gallium oxide crystallization due to losses such as ambient temperature, the heat taken away by the helium gas is required for crystallization of the gallium oxide melt is:

Q _helium ＝0.2c _{Fixing device} m _Crystal (t _{Initially, the method comprises} -t _{Powder (D)} )≈369KJ；

Deriving helium m _Helium = 1776.4g, the helium density is known as ρ _Helium ＝178.6g/m ³ ；

According to V _{Total (S)} ＝m _Helium /ρ _Helium ＝1776.4g/178.6g/m ³ ＝9.95m ³ ＝9950L。

Assume that a single crystal of gallium oxide of 4 inches is grown by radiation from the center at a growth rate of 1.27cm/h (0.0212 cm/min), i.e., 4 hours. Since the gallium oxide single crystal wafer is crystallized from the center of the circle and then slowly crystallized outwards, the larger the quality of the gallium oxide single crystal grown in unit time is along with the crystallization of the gallium oxide from the outer edge.

It can be seen that if the growth rate of 0.0212cm/min is fixed and the heat released during the growth of the gallium oxide single crystal is blown away by helium, a growth radius of r=0.0212 t can be expressed as an increased mass per unit time:

Δm＝π(r+Δr) ² -πr ² ＝[π(0.0212t+Δt) ² -π*0.0212t ² ]ρ _{gallium oxide} ；

The amount of heat required to be taken away per unit time is Δq=Δm/m _Crystal *Q _{Total (S)} The flow rate required per unit time is y=Δm/m _Helium *V _{Total (S)} ；

Thus, the flow y is a function of time t, expressed as:

y＝π[0.0212(t+Δt)] ² -(0.0212t) ² }*1*5.9/478*9950；

＝0.17228[(t+Δt) ² -t ² ]；

＝0.17228(2t+Δt)；

by plotting the function, as shown in fig. 6, the flow y is calculated as a function of time t, and the expression is y= 0.17228 (2t+Δt).

Further, growing gallium oxide single crystals with the thickness of 4 inches and 10mm, wherein when helium gas flow is purged at the speed of y= 0.17228 (2t+Δt), the gallium oxide single crystals uniformly spread from the center to the edge at a uniform growth speed of 1.27cm/h, and after the central part is condensed and crystallized, the peripheral crystals uniformly grow;

still further, when the helium flow is purged at a rate less than y= 0.17228 (2t+Δt), the growth rate is less than 1.27cm/h, the crystal growth becomes slower and slower along with the circumferential change, the central portion is coagulated and crystallized first, and the crystal growth around becomes slower and slower;

further, when the helium flow is purged at a rate greater than y= 0.17228 (2t+Δt), the growth rate is greater than 1.27cm/h, the gallium oxide crystal growth is uniformly accelerated and diffused from the center to the edge, and after the central part is condensed and crystallized, the peripheral crystals are accelerated and grown and crystallized.

Therefore, the growth rate of the gallium oxide crystal is controlled by controlling the flow of the gas, so that the growth quality of the gallium oxide crystal is controlled, and a reference basis and thought are provided for the growth of the gallium oxide crystal.

In summary, the invention provides a gallium oxide crystal manufacturing device and a manufacturing method thereof based on a heat exchange method, wherein gallium oxide solids in a crucible of a crucible frame are heated by a heating component, the gallium oxide solids are changed into gallium oxide melt, then a sealing cover is pushed to move towards the crucible frame, when the crucible frame and the sealing cover are closed, seed crystals in the sealing cover react with the gallium oxide melt to form gallium oxide crystals, meanwhile, a first heat dissipation component is controlled to take away heat of a first heat dissipation channel of the crucible frame, a second heat dissipation component is controlled to take away heat of a second heat dissipation channel of the sealing cover, so that the upper surface and the lower surface of the gallium oxide crystals are cooled, and the growth stability of the gallium oxide crystals is improved.

It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.

Claims (10)

1. A gallium oxide crystal production apparatus by a heat exchange method, comprising:

the box body is provided with a crystal taking door;

the crucible rack is arranged in the box body, a crucible for placing gallium oxide solids is arranged in the crucible rack, and a first heat dissipation channel is arranged at the bottoms of the crucible and the crucible rack;

the heating assembly is arranged in the box body and surrounds the crucible frame;

the sealing cover is arranged in the box body and can move up and down in the box body towards the crucible frame, a fixing component for fixing seed crystals is arranged in the sealing cover, and a second heat dissipation channel is arranged in the sealing cover;

the first heat dissipation channel is internally provided with a first heat dissipation component for taking away the growth heat of the gallium oxide crystals, and the second heat dissipation channel is internally provided with a second heat dissipation component for taking away the growth heat of the gallium oxide crystals.

2. The apparatus for manufacturing gallium oxide crystal according to claim 1, wherein the first heat dissipating member comprises:

one end of the first air inlet pipe is connected with the first heat dissipation channel, the other end of the first air inlet pipe extends out of the box body and is connected with an external cold source, and the first air inlet pipe is used for inputting cold air;

the first air outlet holes are formed in the inner wall of the crucible frame where the first heat dissipation channel is located.

3. The gallium oxide crystal manufacturing apparatus according to claim 1, wherein the second heat dissipating member comprises:

one end of the second air inlet pipe is connected with the second heat dissipation channel, the other end of the second air inlet pipe extends out of the box body and is connected with an external cold source, and the second air inlet pipe is used for inputting cold air;

the second air outlet holes are formed in the inner wall of the sealing cover where the second heat dissipation channel is located;

wherein the second air inlet pipe is a deformation telescopic pipe.

4. The gallium oxide crystal manufacturing apparatus according to claim 1, further comprising a telescopic assembly provided on the case, wherein the telescopic assembly is connected to the sealing cover, and the sealing cover is capable of moving telescopically toward the crucible frame.

5. The apparatus for producing gallium oxide crystals according to claim 4, wherein the expansion and contraction unit comprises:

the hydraulic shell is fixed on the box body;

the hydraulic cylinder is fixed in the hydraulic shell;

one end of the hydraulic rod is in driving connection with the hydraulic cylinder, and the other end of the hydraulic rod penetrates through the box body, extends into the box body and is connected with the sealing cover.

6. The gallium oxide crystal manufacturing apparatus based on the heat exchange method according to claim 1, wherein a plurality of shock-absorbing columns are provided in the case body, and the crucible frame is provided on a plurality of the shock-absorbing columns.

7. The apparatus for manufacturing gallium oxide crystals based on a heat exchange method according to claim 1, wherein the fixing means comprises:

the telescopic members are circumferentially arranged along the inner wall of the sealing cover and surround to form a clamping channel;

the fixed station, detachable set up in the centre gripping passageway, the fixed station is provided with detachable seed crystal.

8. The gallium oxide crystal manufacturing apparatus according to claim 1, wherein the heating unit comprises:

and the heating pipes are arranged in the box body and are circumferentially arranged along the circumferential path of the crucible frame.

9. The gallium oxide crystal manufacturing device based on the heat exchange method according to claim 1, wherein a plurality of clamping blocks are arranged in the sealing cover, a plurality of clamping grooves are arranged on the crucible, the clamping blocks are connected with the clamping grooves in a clamping manner, and the sealing cover is fixedly connected with the crucible frame.

10. A manufacturing method of the gallium oxide crystal manufacturing apparatus based on the heat exchange method according to any one of claims 1 to 9, comprising:

fixing seed crystals on the fixing component, and putting preset gallium oxide solids into a crucible;

controlling a heating component to heat the preset gallium oxide solid, wherein the preset gallium oxide solid is melted into a gallium oxide melt;

the telescopic component is controlled to push the sealing cover to be fixedly butted with the crucible frame, and the seed crystal and the gallium oxide melt are contacted and reacted to form gallium oxide crystals; simultaneously, the first heat dissipation component is controlled to cool the sealing cover, and the second heat dissipation component is controlled to cool the crucible frame;

after the growth time is reached, the first heat dissipation assembly and the second heat dissipation assembly are controlled to be closed; the growth time is determined according to the air inlet flow of the first heat dissipation assembly and the second heat dissipation assembly, and the air inlet flow is determined according to the heat emitted by the gallium oxide crystal;

and (3) moving up the sealing cover, and taking out the gallium oxide crystal in the crucible.