CN215028656U - Semiconductor phosphide injection synthesis system - Google Patents
Semiconductor phosphide injection synthesis system Download PDFInfo
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- CN215028656U CN215028656U CN202023142510.2U CN202023142510U CN215028656U CN 215028656 U CN215028656 U CN 215028656U CN 202023142510 U CN202023142510 U CN 202023142510U CN 215028656 U CN215028656 U CN 215028656U
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Abstract
A semiconductor phosphide injection synthesis system belongs to the technical field of preparation of semiconductor phosphide and comprises a furnace body, a shielding bearing box arranged above the furnace body, a phosphorus source carrier arranged in the shielding bearing box, an injection pipe arranged below the phosphorus source carrier and a crucible which is arranged at the bottom in the furnace body in a matching way, wherein the phosphorus source carrier comprises a phosphorus source carrier main body, a phosphorus source carrier upper cover, a heating element base arranged at the bottom in the phosphorus source carrier main body and a heating element arranged on the heating element base; an induction coil is arranged between the heat preservation layer and the inner wall of the shielding bearing box. By improving the structure of the phosphorus source carrier, the heating uniformity of the synthesis system can be improved, the stability is improved, the whole synthesis system can be quantitatively synthesized, and the explosion danger of the phosphorus source carrier is reduced.
Description
Technical Field
The utility model belongs to the technical field of the preparation of semiconductor phosphide, concretely relates to semiconductor phosphide pours into synthesis system into.
Background
The semiconductor phosphide mainly comprises semiconductor materials such as indium phosphide, gallium phosphide and the like. The indium phosphide has the characteristics of high frequency, high speed, radiation resistance and low noise, the working frequency of the indium phosphide reaches 3THz, and when the working frequency of the indium phosphide is more than 100GHz, the indium phosphide has obvious advantages. InP has become a key semiconductor material in ultrahigh frequency, ultra-high speed devices and optoelectronic devices. With the development of terahertz, millimeter wave, optical communication, automatic driving, internet of things and 5G/6G technology in the future, InP plays a greater role and generates greater social benefits. The preparation is extremely difficult because the phosphide has a very high saturated vapor pressure at its melting point.
The phosphide synthesis method mainly comprises horizontal diffusion synthesis and injection synthesis. Generally, the horizontal diffusion synthesis technology is simple, but the synthesis period is long, the material purity is low, and high-quality polycrystalline materials are difficult to obtain. The phosphide injection synthesis technology is an excellent method for preparing polycrystal, has the characteristics of high synthesis rate and high purity of preparation materials, and has the defect that the injection synthesis rate is often required to be low in order to ensure the utilization rate of phosphorus, so that the phenomenon of explosion of a phosphorus source carrier is easy to occur. When the synthesized amount becomes large, the mass of red phosphorus in the phosphorus source carrier increases, uniform heating of red phosphorus is difficult to realize, the thermal response capability of the system is poor, and the temperature control capability of the system is poor, so that the risk of explosion of the phosphorus source carrier is increased. Polycrystalline materials are the basis for preparing single crystal materials, so an injection synthesis device with high synthesis purity, high synthesis efficiency and high phosphorus utilization rate is urgently needed.
Disclosure of Invention
The to-be-solved technical problem of the utility model is to provide a semiconductor phosphide injects synthesis system, through improving phosphorus source carrier structure itself, can improve synthesis system and be heated evenly, the stability of improvement can make whole synthesis system carry out quantitative synthesis, has reduced the danger of phosphorus source carrier explosion.
The utility model adopts the technical proposal that: a semiconductor phosphide injection synthesis system comprises a furnace body, a shielding bearing box arranged above the furnace body, a phosphorus source carrier arranged in the shielding bearing box, an injection pipe arranged below the phosphorus source carrier and a crucible arranged at the bottom in the furnace body in a matching way, wherein the shielding bearing box has vertical displacement freedom degree in the space above the furnace body by virtue of a lifting mechanism, and the phosphorus source carrier comprises a phosphorus source carrier main body, a phosphorus source carrier upper cover, a heating element base arranged at the bottom in the phosphorus source carrier main body and a heating element arranged on the heating element base; the outer wall of the phosphorus source carrier is wrapped with a heat insulation layer, and an induction coil is arranged between the heat insulation layer and the inner wall of the shielding carrying box.
Further, a pressure measuring system is arranged on an upper cover of the phosphorus source carrier, and the pressure measuring system comprises a pressure balance pipe welded with the upper cover of the phosphorus source carrier, a solid boron oxide column arranged in the pressure balance pipe, a pressure measuring sealing cap with a thermocouple a and an auxiliary heater arranged on the outer wall of the pressure balance pipe; the pressure measuring sealing cap is welded with the upper end of the pressure balance pipe, the lower end of the pressure balance pipe is provided with an air inlet communicated with the phosphorus source loader, the pressure balance pipe is provided with an observation graduated scale, and the upper end face of the furnace body is provided with an observation window a.
Further, a thermocouple wire of the thermocouple a is connected with a sensor on the outer side of the furnace body.
Further, the bottom of the phosphorus source carrier main body is provided with an insertion groove for accommodating a thermocouple b; the thermocouple b is in an inverted L shape, the upper end of the thermocouple b penetrates through the bottom of the shielding carrying box and is matched with the insertion groove, and the left side of the thermocouple b penetrates through the furnace wall of the furnace body.
Furthermore, the outer wall of the crucible is provided with a main resistance heater in a surrounding manner, and the middle part of the furnace body is provided with an observation window b matched with the crucible.
Adopt the utility model discloses the beneficial effect who produces: the method comprises the following steps that a plurality of heating bodies in a phosphorus source carrier are heated through induction coils to heat red phosphorus, so that the red phosphorus is heated uniformly and is volatilized and injected into a melt, and meanwhile, a pressure measuring system is arranged on the phosphorus source carrier and is used for measuring the pressure and the temperature in a synthesis system under corrosive atmosphere and an induction magnetic field by combining with the saturated vapor pressure of the phosphorus, so that the whole synthesis system can be monitored and controlled; the device is particularly suitable for large-capacity synthesis, can improve the uniformity of heating of a synthesis system, improves the stability, can ensure that the whole synthesis system carries out quantitative synthesis, and reduces the danger of explosion of a phosphorus source carrier.
Drawings
Fig. 1 is a schematic structural diagram of the present invention;
FIG. 2 is a schematic view of a phosphorus source carrier;
fig. 3 is a schematic structural view of the pressure measuring system.
Detailed Description
Referring to the attached drawings 1-3, a semiconductor phosphide injection synthesis system comprises a furnace body 40, a shielding carrying box 2 arranged above the furnace body, a phosphorus source carrier 11 arranged in the shielding carrying box 2, an injection pipe 6 arranged below the phosphorus source carrier 11 and a crucible 13 which is arranged at the bottom in the furnace body 40 in a matching way, wherein the shielding carrying box 2 has vertical displacement freedom degree in the space above the furnace body 40 by virtue of a lifting mechanism 20, the phosphorus source carrier 11 comprises a phosphorus source carrier main body 11-2, a phosphorus source carrier upper cover 11-1, a heating element base 4 arranged at the bottom in the phosphorus source carrier main body 11-2 and a heating element 12 arranged on the heating element base 4; an insulating layer 7 is wrapped on the outer wall of the phosphorus source carrier 11, and an induction coil 1 is arranged between the insulating layer 7 and the inner wall of the shielding carrying box 2. A pressure gauge 23 is also provided outside the furnace body 40. The induction heating body 12 is used for heating, so that the problem of uneven heating is avoided; the prior art heating is edge sublimation with the edge being especially hot for large synthesis systems, the center of the phosphorus source carrier 11 is also especially cold, and the hot phosphorus gas will desublimate again when encountering the cold zone. May clog the injection tube of the phosphorus source carrier 11, causing the phosphorus source carrier 11 to explode.
A pressure measuring system 10 is arranged on the upper cover 11-1 of the phosphorus source carrier, and comprises a pressure balance tube 10-2 welded with the upper cover 11-1 of the phosphorus source carrier, a solid boron oxide column 17 arranged in the pressure balance tube 10-2, a pressure measuring sealing cap 10-1 with a thermocouple a8 and an auxiliary heater 21 arranged on the outer wall of the pressure balance tube 10-2; the pressure measuring sealing cap 10-1 is welded with the upper end of the pressure balance tube 10-2, the lower end of the pressure balance tube 10-2 is provided with an air inlet hole 10-4 communicated with the phosphorus source carrier 11, the pressure balance tube 10-2 is provided with an observation graduated scale 10-3, and the upper end face of the furnace body 40 is provided with an observation window a 18. The pressure inside the phosphorus source carrier 11 is tested by a pressure measurement system 10. The temperature feedback is insensitive due to the poor thermal conductivity of the liquid boron oxide column 9. The temperature control system cannot feedback control the power of the induction coil 1 by the thermocouple a 8. The power of the induction coil 1 is fed back by the thermocouple b22, and then the temperature in the phosphorus source carrier 11 is adjusted, so that the value of the adjusting pressure P2 is realized, then the required bubbling rate is obtained, and the optimal pressure difference Δ P at the moment is obtained. As the phosphorus element inside the phosphorus source carrier 11 becomes less, the pressure inside the phosphorus source carrier 11 decreases. The power of the induction coil 1 is feedback controlled by a temperature control system, a thermocouple b22, and the pressure P2 in the phosphorus source carrier 11 is kept constant.
The thermocouple wire of the thermocouple a8 is connected with a sensor outside the furnace body 40.
The bottom of the phosphorus source carrier main body 11-2 is provided with an insertion groove 11-3 for accommodating a thermocouple b 22; the thermocouple b22 is in a reverse L shape, the upper end of the thermocouple b22 penetrates through the bottom of the shielding carrying box 2 and is matched with the insertion groove 11-3, and the left side of the thermocouple b22 penetrates through the furnace wall of the furnace body 40.
The outer wall of the crucible 13 is provided with a main resistance heater 15 in a surrounding manner, and the middle part of the furnace body 40 is provided with an observation window b19 matched with the crucible 13.
In specific implementation, thermocouple a8 is fused to pressure sensing sealing cap 10-1, while leaving the two thermocouple wires untouched. The pressure balance tube 10-2 is welded with the upper cover 11-1 of the phosphorus source carrier. The solid boron oxide column 17 is placed in the pressure equalization tube 10-2. The pressure measuring sealing cap 10-1 with the thermocouple a8 is then welded with the pressure equalizing tube 10-2 during the welding process.
Then, the heating element 12 is loaded on the heating element base 4 inside the phosphorus source carrier main body 11-2. Then red phosphorus 3 is loaded into the phosphorus source carrier main body 11-2 according to the required synthesis quality, and the phosphorus source carrier upper cover 11-1 and the phosphorus source carrier main body 11-2 are welded together.
The induction coil 1 is then placed in a shielded carrier box 2. Meanwhile, the outer wall of the phosphorus source carrier 11 is wrapped by the insulating layer 7, and then the phosphorus source carrier 11 wrapped by the insulating layer 7 is placed in the induction coil 1.
The thermocouple wires of the thermocouple a8 were connected to the sensor outside the furnace body 21. The furnace body 21 is provided with an observation window a18 and an observation window b 19.
Putting high-purity indium and boron oxide covering agent 14 into a crucible 13, and vacuumizing the system to 10 DEG-5Pa, filling inert gas. The crucible 13 is heated by the main resistance heater 15 so that the high purity indium and the boron oxide coating agent 14 are melted, and the high purity indium forms a melt 16.
The pressure measuring system was heated by the auxiliary heater 21, and observed through the observation window a18 until the solid boron oxide column 17 was melted, and after the thermocouple a8 was stabilized, the temperature T1 at that time and the scale value L1 on the scale 10-3 were recorded. The volume V1 at this time is calculated from the diameter of the pressure equalizing tube 10-2. At this time, the internal pressure and the external pressure are balanced, and the system pressure is P1.
Then the phosphorus source carrier 11 is descended towards the melt 16 by the lifting mechanism 20, and the thermocouple b23 is inserted into the temperature thermocouple hole 11-3 until the injection pipe 6 is close to the position 3-5mm above the bottom of the crucible.
The induction coil 1 is supplied with an alternating current at a current of n1, and the bubbling of the injection tube 6 is observed through the observation window a 19. While observing the scale value L2 on the scale 10-3, the temperature T2 at that time was recorded, and the volume V2 at that time was obtained. The pressure P2 within the phosphorus source carrier at this point was obtained. The P2 value was obtained according to the klebside equation P1V1/T1= P2V 2/T2. The bubbling rate is regulated by the pressure difference Δ P = P2-P0, P0 being the value of the pressure gauge 23.
The temperature of the phosphorus source carrier 11 is adjusted by the thermocouple b22 to obtain the required bubbling rate and the pressure difference Δ P at the moment.
After the synthesis is completed, the currents of the induction coil 1 and the auxiliary heater 21 are reduced to 0A. The phosphorus source carrier 11 is lifted by the lifting mechanism 20 so that the injection pipe 6 is detached from the boron oxide blanketing agent 14.
After the furnace is removed, the system is deflated to 1 atmosphere, the upper cover 11-1 of the phosphorus source carrier is cut off, and the main body 11-2 of the phosphorus source carrier is cleaned for the next use. At the same time, the manometric sealing cap 10-1 is cut away, leaving thermocouple a8 ready for the next use.
Claims (5)
1. The utility model provides a synthetic system of semiconductor phosphide injection, includes furnace body (40), sets up shielding bearing box (2) in furnace body (40) top, sets up phosphorus source carrier (11) in shielding bearing box (2), sets up injection tube (6) and the configuration setting crucible (13) of bottom in furnace body (40) below phosphorus source carrier (11), its characterized in that: the shielding bearing box (2) has vertical displacement freedom degree in the space above the furnace body (40) by virtue of a lifting mechanism (20), and the phosphorus source carrier (11) comprises a phosphorus source carrier main body (11-2), a phosphorus source carrier upper cover (11-1), a heating element base (4) arranged at the bottom in the phosphorus source carrier main body (11-2) and a heating element (12) arranged on the heating element base (4); an insulating layer (7) is wrapped on the outer wall of the phosphorus source carrier (11), and an induction coil (1) is arranged between the insulating layer (7) and the inner wall of the shielding carrying box (2).
2. The semiconductor phosphide injection synthesis system of claim 1, wherein: a pressure measuring system is arranged on the upper cover (11-1) of the phosphorus source carrier, and comprises a pressure balance tube (10-2) welded with the upper cover (11-1) of the phosphorus source carrier, a solid boron oxide column (17) arranged in the pressure balance tube (10-2), a pressure measuring sealing cap (10-1) with a thermocouple a (8) and an auxiliary heater (21) arranged on the outer wall of the pressure balance tube (10-2); the pressure measuring sealing cap (10-1) is welded with the upper end of the pressure balancing pipe (10-2), the lower end of the pressure balancing pipe (10-2) is provided with an air inlet hole (10-4) communicated with the phosphorus source carrier (11), the pressure balancing pipe (10-2) is provided with an observation graduated scale (10-3), and the upper end face of the furnace body (40) is provided with an observation window a (18).
3. The semiconductor phosphide injection synthesis system of claim 2, wherein: and a thermocouple wire of the thermocouple a (8) is connected with a sensor on the outer side of the furnace body (40).
4. The semiconductor phosphide injection synthesis system of claim 1, wherein: an insertion groove (11-3) for accommodating a thermocouple b (22) is formed in the bottom of the phosphorus source carrier main body (11-2); the thermocouple b (22) is in an inverted L shape, the upper end of the thermocouple b penetrates through the bottom of the shielding carrying box (2) and is matched with the insertion groove (11-3), and the left side of the thermocouple b penetrates through the furnace wall of the furnace body (40).
5. The semiconductor phosphide injection synthesis system of claim 1, wherein: the outer wall of the crucible (13) is provided with a main resistance heater (15) in a surrounding way, and the middle part of the furnace body (40) is provided with an observation window b (19) matched with the crucible (13).
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202023142510.2U CN215028656U (en) | 2020-12-23 | 2020-12-23 | Semiconductor phosphide injection synthesis system |
| PCT/CN2021/104407 WO2022134527A1 (en) | 2020-12-23 | 2021-07-05 | Semiconductor phosphide injection synthesis system and control method thereof |
| JP2022556470A JP2024500256A (en) | 2020-12-23 | 2021-07-05 | Semiconductor phosphide injection synthesis system and control method |
| US17/797,081 US20230049408A1 (en) | 2020-12-23 | 2021-07-05 | Semiconductor Phosphide Injection Synthesis System and Control Method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202023142510.2U CN215028656U (en) | 2020-12-23 | 2020-12-23 | Semiconductor phosphide injection synthesis system |
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| CN215028656U true CN215028656U (en) | 2021-12-07 |
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| CN202023142510.2U Active CN215028656U (en) | 2020-12-23 | 2020-12-23 | Semiconductor phosphide injection synthesis system |
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