CN114808120A - Pressure control device and method for indium phosphide polycrystal production - Google Patents
Pressure control device and method for indium phosphide polycrystal production Download PDFInfo
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- CN114808120A CN114808120A CN202110071219.0A CN202110071219A CN114808120A CN 114808120 A CN114808120 A CN 114808120A CN 202110071219 A CN202110071219 A CN 202110071219A CN 114808120 A CN114808120 A CN 114808120A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D16/00—Control of fluid pressure
- G05D16/20—Control of fluid pressure characterised by the use of electric means
- G05D16/2006—Control of fluid pressure characterised by the use of electric means with direct action of electric energy on controlling means
- G05D16/2013—Control of fluid pressure characterised by the use of electric means with direct action of electric energy on controlling means using throttling means as controlling means
- G05D16/2026—Control of fluid pressure characterised by the use of electric means with direct action of electric energy on controlling means using throttling means as controlling means with a plurality of throttling means
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Abstract
The invention is suitable for the technical field of semiconductor production, and provides a pressure control device for indium phosphide polycrystal production, which comprises: an outer container, a sealed reaction container, a temperature sensor, a pressure sensor and a control unit. Compared with the prior art, the temperature data in the sealed reaction container is acquired through the temperature sensor, the control unit calculates the pressure data in the sealed reaction container according to the temperature data acquired by the temperature sensor and the saturated vapor pressure curve of element phosphorus at different temperatures, and controls the inert gas to be filled into or discharged out of the pressure regulating space according to the difference value between the calculated pressure data and the pressure data of the pressure regulating space, so that the dynamic balance control of the pressure inside and outside the sealed reaction container is realized, the risk of tube explosion of the sealed reaction container caused by sudden temperature rise or fluctuation is avoided, and the stable production of the indium phosphide polycrystal is ensured. The invention also provides a pressure control method for indium phosphide polycrystal production.
Description
Technical Field
The invention belongs to the technical field of semiconductor production, and particularly relates to a pressure control device and method for indium phosphide polycrystal production.
Background
Indium phosphide is one of strategic important semiconductor materials, and has important application in the fields of optical communication, millimeter wave high frequency, low noise, broadband microelectronic integration and the like. Before preparing the indium phosphide single crystal, In and P meeting a certain purity requirement must be synthesized into a compound indium phosphide polycrystal, and then the indium phosphide single crystal can be further prepared on the basis. The rapid and effective synthesis of the indium phosphide polycrystal is an important way for reducing the production cost and improving the production efficiency, and is also a premise for preparing high-quality indium phosphide single crystals. Currently, the commonly used methods for synthesizing indium phosphide polycrystal are horizontal methods, including horizontal bridgeman method (HB) and horizontal temperature gradient freezing method (HGF).
At present, the industrial synthesis of indium phosphide polycrystal mainly adopts phosphorus steam to contact with indium melt, and the indium phosphide polycrystal is synthesized at the temperature higher than the melting point of indium phosphide.
However, the applicant of the present invention has found that in implementing the above technical solution, the current technical solution has at least the following disadvantages:
the melting point of the indium phosphide is 1062 ℃, phosphorus vapor is large at the temperature, the requirements on temperature control and pressure control are very high, and sudden rise or fluctuation of the temperature easily causes untimely pressure balance and has the risk of 'tube explosion' of a sealed reaction tube.
Disclosure of Invention
An object of an embodiment of the present invention is to provide a pressure control apparatus for indium phosphide polycrystal production, which aims to solve the problems mentioned in the background art.
The embodiment of the invention is realized in such a way that the pressure control device and the method for producing the indium phosphide polycrystal comprise the following steps:
an outer container; a sealed reaction vessel used for reacting element phosphorus with element indium to generate indium phosphide is arranged in the external vessel, and a pressure regulating space is formed between the sealed reaction vessel and the element phosphorus;
the temperature sensor is used for acquiring temperature data in the sealed reaction container;
the pressure sensor is used for acquiring pressure data of the pressure regulating space;
a control unit; the control unit generates pressure data in the sealed reaction container according to temperature data acquired by the temperature sensor and saturated vapor pressure curves of element phosphorus at different temperatures, and controls inert gas to be charged into or discharged from the pressure regulating space according to the difference between the generated pressure data and the pressure data of the pressure regulating space.
Preferably, the external container is communicated with an inert gas charging pipeline and an inert gas discharging pipeline, and the control unit controls the inert gas to be charged into the pressure regulating space from the inert gas charging pipeline or discharged out of the pressure regulating space from the inert gas discharging pipeline.
Preferably, the inert gas charging pipeline is provided with a first switch valve and a first flow regulating valve for regulating the charging flow of the inert gas; the inert gas discharge pipeline is provided with a second flow regulating valve for regulating the discharge flow of the inert gas; the opening and closing and the opening degree of the first flow regulating valve and the second flow regulating valve are controlled by the control unit.
Preferably, an inert gas charging pipeline branch communicated with the inert gas charging pipeline is arranged at two ends of the first switch valve and the first flow regulating valve, and a second switch valve is arranged on the inert gas charging pipeline branch.
Preferably, a pressure difference threshold range is preset in the control unit, and when the difference value between the generated pressure data and the pressure data of the pressure regulating space is not within the pressure difference threshold range, the control unit controls the inert gas to be charged into or discharged from the pressure regulating space, otherwise, the inert gas is neither charged into nor discharged from the pressure regulating space.
Preferably, the control unit controls the inert gas to be charged into the pressure-adjusting space when a difference between the generated pressure data and the pressure data of the pressure-adjusting space is not within a pressure difference threshold range and the generated pressure data is higher than the pressure data of the pressure-adjusting space.
Preferably, the control unit controls the inert gas to be discharged from the pressure-adjusting space when a difference between the generated pressure data and the pressure data of the pressure-adjusting space is not within a differential pressure threshold range and the generated pressure data is lower than the pressure data of the pressure-adjusting space.
Preferably, the differential pressure threshold range is-0.08 MPa.
Preferably, the control unit reads temperature data acquired by the temperature sensor at a preset frequency.
Preferably, the frequency of the temperature data acquired by the temperature sensor read by the control unit is 10-30 times/min.
Another object of an embodiment of the present invention is to provide a pressure control method for indium phosphide polycrystal production, comprising the steps of:
acquiring temperature data and pressure data of a pressure regulating space in a sealed reaction container;
generating pressure data in the sealed reaction container according to the acquired temperature data and the saturated vapor pressure curve of the element phosphorus at different temperatures;
and controlling inert gas to be filled into or discharged from the pressure regulating space according to the difference value between the generated pressure data and the pressure data of the pressure regulating space.
Preferably, when the difference between the generated pressure data and the pressure data of the pressure regulating space is not within a preset pressure difference threshold range, the inert gas is controlled to be charged into or discharged from the pressure regulating space, otherwise, the inert gas is neither charged into nor discharged from the pressure regulating space.
Preferably, when the difference value between the generated pressure data and the pressure data of the pressure regulating space is not within the preset pressure difference threshold range and the generated pressure data is higher than the pressure data of the pressure regulating space, the inert gas is controlled to be filled into the pressure regulating space.
Preferably, when the difference between the generated pressure data and the pressure data of the pressure regulating space is not within the preset pressure difference threshold range and the generated pressure data is lower than the pressure data of the pressure regulating space, the inert gas is controlled to be discharged from the pressure regulating space.
Preferably, the differential pressure threshold range is-0.08 MPa.
Preferably, the pressure data within the sealed reaction vessel is generated at a predetermined frequency based on the acquired temperature data and the saturated vapor pressure curve of elemental phosphorus at different temperatures.
Preferably, the frequency is 10 to 30 times/min.
The embodiment of the invention provides a pressure control device for indium phosphide polycrystal production, which comprises: an outer container; a sealed reaction vessel for reacting elemental phosphorus with elemental indium to produce indium phosphide; the sealed reaction container is arranged in the outer container, and a pressure regulating space is formed between the sealed reaction container and the outer container; the temperature sensor is used for acquiring temperature data in the sealed reaction container; the pressure sensor is used for acquiring pressure data of the pressure regulating space; a control unit; the control unit generates pressure data in the sealed reaction container according to temperature data acquired by the temperature sensor and saturated vapor pressure curves of element phosphorus at different temperatures, and controls inert gas to be charged into or discharged from the pressure regulating space according to the difference between the generated pressure data and the pressure data of the pressure regulating space.
Compared with the prior art, the temperature data in the sealed reaction container is acquired through the temperature sensor, the control unit calculates the pressure data in the sealed reaction container according to the temperature data acquired by the temperature sensor and the saturated vapor pressure curve of element phosphorus at different temperatures, and controls the inert gas to be filled into or discharged out of the pressure regulating space according to the difference value between the calculated pressure data and the pressure data of the pressure regulating space, so that the dynamic balance control of the pressure inside and outside the sealed reaction container is realized, the risk of tube explosion of the sealed reaction container caused by sudden temperature rise or fluctuation is avoided, and the stable production of the indium phosphide polycrystal is ensured.
Drawings
FIG. 1 is a schematic structural diagram of a pressure control apparatus for indium phosphide polycrystal production according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a pressure control device with a flow regulating valve according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a pressure control device with an inert gas charging pipe branch according to an embodiment of the present invention;
FIG. 4 is a schematic flow chart illustrating the operation of a pressure control device according to an embodiment of the present invention;
FIG. 5 is a schematic flow chart of a pressure control method for indium phosphide polycrystal production according to an embodiment of the present invention.
In the drawings: 1. an outer container; 2. sealing the reaction vessel; 3. a temperature sensor; 4. a pressure sensor; 5. a control unit; 6. an inert gas discharge line; 7. filling inert gas into the pipeline; 8. a second flow regulating valve; 9. a first on-off valve; 10. a first flow regulating valve; 11. filling inert gas into the pipeline branch; 12. and a second on-off valve.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Specific implementations of the present invention are described in detail below with reference to specific embodiments.
Example 1
As shown in fig. 1, a pressure control device for indium phosphide polycrystal production provided for one embodiment of the present invention comprises:
an outer container 1; a sealed reaction vessel 2 for reacting elemental phosphorus with elemental indium to generate indium phosphide is arranged in the outer vessel 1, and a pressure regulating space is formed between the sealed reaction vessel 2 and the elemental indium phosphide;
the temperature sensor 3 is used for acquiring temperature data in the sealed reaction container 2;
the pressure sensor 4 is used for acquiring pressure data of the pressure regulating space;
a control unit 5; the control unit 5 generates pressure data in the sealed reaction container 2 according to the temperature data acquired by the temperature sensor 3 and the saturated vapor pressure curve of the element phosphorus at different temperatures, and controls the inert gas to be charged into or discharged from the pressure regulating space according to the difference between the generated pressure data and the pressure data of the pressure regulating space.
As shown in fig. 4, the working principle of the embodiment of the present invention is as follows:
when the indium phosphide polycrystal is produced, phosphorus and indium meeting certain purity requirements are placed in the sealed reaction container 2. The phosphorus is heated to sublimate, and the pressure in the sealed reaction container 2 is increased. Temperature data in the sealed reaction vessel 2 can be acquired by the temperature sensor 3, and pressure data in the pressure-regulating space can be acquired by the pressure sensor 4. The acquired temperature data is transmitted to the control unit 5, and the control unit 5 calculates pressure data in the sealed reaction vessel 2 according to the temperature data acquired by the temperature sensor 3 and the saturated vapor pressure curve of the element phosphorus at different temperatures. And then the control unit 5 compares the calculated pressure data with the pressure data of the pressure regulating space, and controls the inert gas to be filled into or discharged from the pressure regulating space according to the difference value of the calculated pressure data and the pressure data of the pressure regulating space, so that the pressure data of the pressure regulating space is equivalent to the pressure data in the sealed reaction vessel 2, the dynamic balance control of the internal and external pressures of the sealed reaction vessel 2 is realized, and the stable production of the indium phosphide polycrystal is ensured.
In this embodiment, the control unit 5 may be selected from a PLC control unit 5, a single chip, or an ARM chip.
Compared with the prior art, the temperature data in the sealed reaction vessel 2 is acquired by the temperature sensor 3, the control unit 5 calculates the pressure data in the sealed reaction vessel 2 according to the temperature data acquired by the temperature sensor 3 and the saturated vapor pressure curve of element phosphorus at different temperatures, and controls the inert gas to be filled into or discharged from the pressure regulating space according to the difference value of the calculated pressure data and the pressure data of the pressure regulating space, so that the dynamic balance control of the pressure inside and outside the sealed reaction vessel 2 is realized, the risk of tube explosion of the sealed reaction vessel 2 caused by sudden temperature rise or fluctuation is avoided, and the stable production of indium phosphide polycrystal is ensured.
As shown in fig. 1, as a preferred embodiment of the present invention, the external container 1 is communicated with an inert gas charging pipe 7 and an inert gas discharging pipe 6, and the control unit 5 controls the inert gas to be charged into the pressure adjusting space from the inert gas charging pipe 7 or to be discharged from the inert gas discharging pipe 6.
Specifically, when the pressure in the pressure regulating space is too low, the control unit 5 controls the inert gas to be filled into the pressure regulating space from the inert gas filling pipeline 7, so that the pressure in the pressure regulating space is equivalent to the pressure in the sealed reaction container 2; when the pressure in the pressure-regulating space is too high, the control unit 5 controls the inert gas to be discharged from the inert gas discharge pipeline 6 to the pressure-regulating space, so that the pressure in the pressure-regulating space is equivalent to the pressure in the sealed reaction vessel 2. By the above control action, the dynamic balance control of the pressures inside and outside the sealed reaction vessel 2 is realized.
As shown in fig. 2, as a preferred embodiment of the present invention, a first switching valve 9 and a first flow rate adjusting valve 10 for adjusting the inert gas charging flow rate are provided on the inert gas charging pipe 7; the inert gas discharge pipeline 6 is provided with a second flow regulating valve 8 for regulating the discharge flow of the inert gas; the opening and closing and the opening degree of the first flow rate adjustment valve 10 and the second flow rate adjustment valve 8 are controlled by the control unit 5.
Specifically, the first flow rate adjustment valve 10 and the second flow rate adjustment valve 8 are electrically connected to the control unit 5. When the pressure in the pressure regulating space is too low, the first switch valve 9 is opened (at the moment, the second flow regulating valve 8 is closed), then an opening instruction is sent to the first flow regulating valve 10 through the control unit 5, the first flow regulating valve 10 is opened after receiving the opening instruction, the inert gas enters the pressure regulating space through the inert gas charging pipeline 7, and the pressure in the pressure regulating space is equivalent to the pressure in the sealed reaction container 2; when the pressure in the pressure regulating space is too high, an opening instruction is sent to the second flow regulating valve 8 through the control unit 5, the second flow regulating valve 8 is opened after receiving the opening instruction (at the moment, the first switch valve 9 is closed), and the inert gas is discharged from the pressure regulating space through the inert gas discharge pipeline 6, so that the pressure in the pressure regulating space is equivalent to the pressure in the sealed reaction container 2. By the above control action, the dynamic balance control of the pressures inside and outside the sealed reaction vessel 2 is realized.
In the process of filling and discharging the inert gas, the opening degrees of the first flow regulating valve 10 and the second flow regulating valve 8 can be controlled through the control unit 5, so that the speed of filling and discharging the inert gas into and out of the pressure regulating space is controlled, and accurate flow control in the process of filling and discharging the inert gas is realized.
As shown in fig. 3, as a preferred embodiment of the present invention, an inert gas charging pipe branch 11 communicating with the inert gas charging pipe 7 is provided at both ends of the first on-off valve 9 and the first flow rate adjusting valve 10, and a second on-off valve 12 is provided on the inert gas charging pipe branch 11.
Specifically, in the preparation stage of indium phosphide polycrystal production, the charging and discharging of the inert gas need not be precisely controlled, and therefore, the use of a flow rate regulating valve is also unnecessary. In view of this, the present embodiment is additionally provided with an inert gas charging pipe branch 11, and a second on-off valve 12 is disposed on the inert gas charging pipe branch 11. In the preparation stage, the second switch valve 12 is opened to fill the inert gas into the pressure regulating space.
As a preferred embodiment of the present invention, a differential pressure threshold range is preset in the control unit 5, and when the difference between the generated pressure data and the pressure data of the pressure regulating space is not within the differential pressure threshold range, the control unit 5 controls the inert gas to be charged into or discharged from the pressure regulating space, otherwise, the inert gas is neither charged into nor discharged from the pressure regulating space.
Specifically, the pressure balance can be achieved by the difference between the internal and external pressures of the sealed reaction vessel 2 within a certain range, which is reflected in the preset pressure difference threshold range in the control unit 5 in this embodiment. Different pressure difference threshold value ranges can be set according to different reaction vessels, reaction conditions and the like.
As a preferred embodiment of the present invention, when the difference between the generated pressure data and the pressure data of the pressure adjusting space is not within the differential pressure threshold range and the generated pressure data is higher than the pressure data of the pressure adjusting space, the control unit 5 controls the inert gas to be charged into the pressure adjusting space.
Specifically, when the pressure data calculated by the control unit 5 is higher than the pressure data of the pressure regulating space, it indicates that the pressure in the sealed reaction vessel 2 is higher than the pressure of the pressure regulating space, and at this time, if the difference between the two pressures is no longer within the range of the pressure difference threshold, it indicates that the pressures inside and outside the sealed reaction vessel 2 are in an unbalanced state, the inert gas needs to be controlled to be filled into the pressure regulating space, and the pressure of the pressure regulating space is increased until the pressure data calculated by the control unit 5 and the pressure data of the pressure regulating space are within the range of the pressure difference threshold.
Through this embodiment, can make the difference of the inside and outside pressure of sealed reaction vessel 2 be in pressure differential threshold value scope all the time, guarantee the steady production of indium phosphide polycrystal.
As a preferred embodiment of the present invention, when the difference between the generated pressure data and the pressure data of the pressure-regulated space is not within the differential pressure threshold range and the generated pressure data is lower than the pressure data of the pressure-regulated space, the control unit 5 controls the inert gas to be discharged from the pressure-regulated space.
Specifically, when the pressure data calculated by the control unit 5 is lower than the pressure data of the pressure regulating space, it indicates that the pressure in the sealed reaction vessel 2 is lower than the pressure of the pressure regulating space, and at this time, if the difference between the two pressures is no longer within the range of the pressure difference threshold, it indicates that the pressures inside and outside the sealed reaction vessel 2 are in an unbalanced state, and it is necessary to control the inert gas to be discharged from the pressure regulating space, so as to reduce the pressure of the pressure regulating space until the pressure data calculated by the control unit 5 and the pressure data of the pressure regulating space are within the range of the pressure difference threshold.
As a preferred embodiment of the invention, the differential pressure threshold range is-0.08 MPa.
Specifically, the applicant of the present invention summarizes the actual production process, and usually, the pressure difference threshold range is-0.08 to 0.08MPa, so that the pressure balance between the inside and the outside of the sealed reaction vessel 2 can be realized.
As a preferred embodiment of the present invention, the control unit 5 reads the temperature data acquired by the temperature sensor 3 at a preset frequency.
Specifically, in order to realize the dynamic balance control of the pressures inside and outside the sealed reaction vessel 2, the control unit 5 needs to read the temperature data acquired by the temperature sensor 3 at a certain frequency, and then control the inert gas to be charged into or discharged from the pressure regulating space at the frequency. If the frequency read by the control unit 5 is not satisfactory, the following problems may occur:
at a certain node of the reaction, the pressure inside and outside the sealed reaction vessel 2 is unbalanced, and the control unit 5 does not read the temperature data acquired by the temperature sensor 3 at the moment, so that the problem is not found, and the sealed reaction vessel 2 is subjected to a 'tube explosion' accident in serious cases.
In a preferred embodiment of the present invention, the frequency of reading the temperature data acquired by the temperature sensor 3 by the control unit 5 is 10 to 30 times/min.
Specifically, the applicant of the present invention summarizes the actual production process, and usually, the frequency of reading the temperature data acquired by the temperature sensor 3 by the control unit 5 should be 10 to 30 times/min.
Example 2
As shown in FIG. 5, an embodiment of the present invention also provides a pressure control method for indium phosphide polycrystal production, comprising the steps of:
acquiring temperature data and pressure data of a pressure regulating space in a sealed reaction container;
generating pressure data in the sealed reaction container according to the acquired temperature data and the saturated vapor pressure curve of the element phosphorus at different temperatures;
and controlling inert gas to be filled into or discharged from the pressure regulating space according to the difference value between the generated pressure data and the pressure data of the pressure regulating space.
As a preferred embodiment of the present invention, when the difference between the generated pressure data and the pressure data of the pressure-regulating space is not within the preset pressure difference threshold range, the inert gas is controlled to be charged into or discharged from the pressure-regulating space, whereas the inert gas is neither charged into nor discharged from the pressure-regulating space.
As a preferred embodiment of the present invention, when a difference value between the generated pressure data and the pressure data of the pressure-regulating space is not within a preset pressure difference threshold range, and the generated pressure data is higher than the pressure data of the pressure-regulating space, the inert gas is controlled to be filled into the pressure-regulating space.
As a preferred embodiment of the present invention, when the difference between the generated pressure data and the pressure data of the pressure adjusting space is not within the preset pressure difference threshold range and the generated pressure data is lower than the pressure data of the pressure adjusting space, the inert gas is controlled to be discharged from the pressure adjusting space.
As a preferred embodiment of the invention, the differential pressure threshold range is-0.08 MPa.
As a preferred embodiment of the present invention, the pressure data in the sealed reaction vessel is generated at a predetermined frequency based on the acquired temperature data and the saturated vapor pressure curve of elemental phosphorus at different temperatures.
As a preferred embodiment of the invention, the frequency is 10 to 30 times/min.
Specifically, the method of example 2 can be carried out by using a pressure control apparatus based on example 1, or by using a related apparatus slightly different from that of example 1. Compared with the prior art, the control method disclosed by the invention has the advantages that the temperature data in the sealed reaction container 2 is obtained, the pressure data in the sealed reaction container 2 is calculated according to the obtained temperature data and the saturated vapor pressure curve of the element phosphorus at different temperatures, and the inert gas is controlled to be filled into or discharged from the pressure regulating space according to the difference value between the calculated pressure data and the pressure data of the pressure regulating space, so that the dynamic balance control of the internal and external pressures of the sealed reaction container 2 is realized, the risk of tube explosion of the sealed reaction container 2 caused by sudden temperature rise or fluctuation is avoided, and the stable production of the indium phosphide polycrystal is ensured.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A pressure control device for indium phosphide polycrystal production, comprising:
an outer container; a sealed reaction vessel used for reacting element phosphorus with element indium to generate indium phosphide is arranged in the external vessel, and a pressure regulating space is formed between the sealed reaction vessel and the element phosphorus;
the temperature sensor is used for acquiring temperature data in the sealed reaction container;
the pressure sensor is used for acquiring pressure data of the pressure regulating space;
a control unit; the control unit generates pressure data in the sealed reaction container according to temperature data acquired by the temperature sensor and saturated vapor pressure curves of element phosphorus at different temperatures, and controls inert gas to be charged into or discharged from the pressure regulating space according to the difference between the generated pressure data and the pressure data of the pressure regulating space.
2. The pressure control device for indium phosphide polycrystal production according to claim 1, wherein the external container is communicated with an inert gas charging pipe and an inert gas discharging pipe, and the control unit controls the inert gas to be charged into the pressure-regulating space from the inert gas charging pipe or to be discharged from the pressure-regulating space from the inert gas discharging pipe.
3. The pressure control device for indium phosphide polycrystal production according to claim 2, wherein the inert gas charging line is provided with a first switching valve and a first flow rate regulating valve for regulating the charging flow rate of the inert gas; the inert gas discharge pipeline is provided with a second flow regulating valve for regulating the discharge flow of the inert gas; the opening and closing and the opening degree of the first flow regulating valve and the second flow regulating valve are controlled by the control unit.
4. The pressure control device for indium phosphide polycrystal production according to claim 3, wherein an inert gas charging pipe branch communicating with an inert gas charging pipe is provided at both ends of the first switching valve and the first flow rate adjusting valve, and a second switching valve is provided on the inert gas charging pipe branch.
5. The pressure control device for indium phosphide polycrystal production according to claim 1, wherein a differential pressure threshold range is preset in the control unit, and when the difference between the generated pressure data and the pressure data of the pressure regulating space is not within the differential pressure threshold range, the control unit controls the inert gas to be charged into or discharged from the pressure regulating space, whereas the inert gas is neither charged into nor discharged from the pressure regulating space.
6. The pressure control device for indium phosphide polycrystal production according to claim 5, wherein the control unit controls the inert gas to be filled in the pressure-regulating space when the difference between the generated pressure data and the pressure data of the pressure-regulating space is not within the pressure difference threshold range and the generated pressure data is higher than the pressure data of the pressure-regulating space.
7. The pressure control device for indium phosphide polycrystal production according to claim 5, wherein the control unit controls the discharge of the inert gas from the pressure-regulating space when the difference between the generated pressure data and the pressure data of the pressure-regulating space is not within the threshold range of the pressure difference and the generated pressure data is lower than the pressure data of the pressure-regulating space.
8. The pressure control device for indium phosphide polycrystal production according to any one of claims 5 to 7, wherein the differential pressure threshold value is in the range of-0.08 to 0.08 MPa.
9. The pressure control device for indium phosphide polycrystal production according to claim 1, wherein the control unit reads temperature data obtained by the temperature sensor at a preset frequency.
10. A pressure control method for indium phosphide polycrystal production is characterized by comprising the following steps:
acquiring temperature data and pressure data of a pressure regulating space in a sealed reaction container;
generating pressure data in the sealed reaction container according to the acquired temperature data and the saturated vapor pressure curve of the element phosphorus at different temperatures;
and controlling inert gas to be filled into or discharged from the pressure regulating space according to the difference value between the generated pressure data and the pressure data of the pressure regulating space.
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| CN111893554A (en) * | 2020-07-22 | 2020-11-06 | 威科赛乐微电子股份有限公司 | Pressure control system and process for indium phosphide single crystal VGF (vacuum vapor deposition) process |
| CN212223145U (en) * | 2020-07-22 | 2020-12-25 | 威科赛乐微电子股份有限公司 | Pressure control system for VGF (vacuum vapor deposition) process of indium phosphide single crystal |
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2021
- 2021-01-19 CN CN202110071219.0A patent/CN114808120A/en active Pending
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| US20040173140A1 (en) * | 2003-03-05 | 2004-09-09 | Liu Xiao Gordon | Apparatus and method for balanced pressure growth of Group III-V monocrystalline semiconductor compounds |
| CN106757360A (en) * | 2016-12-27 | 2017-05-31 | 珠海鼎泰芯源晶体有限公司 | The horizontal synthesizer of indium phosphide polycrystal and control method for pressure balance |
| CN107619027A (en) * | 2017-09-13 | 2018-01-23 | 南京金美镓业有限公司 | A kind of pressure furnace compress control method for producing indium phosphide |
| CN111893554A (en) * | 2020-07-22 | 2020-11-06 | 威科赛乐微电子股份有限公司 | Pressure control system and process for indium phosphide single crystal VGF (vacuum vapor deposition) process |
| CN212223145U (en) * | 2020-07-22 | 2020-12-25 | 威科赛乐微电子股份有限公司 | Pressure control system for VGF (vacuum vapor deposition) process of indium phosphide single crystal |
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