CN113355657A - Source-dividing positioning vacuum tube furnace device - Google Patents
Source-dividing positioning vacuum tube furnace device Download PDFInfo
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- CN113355657A CN113355657A CN202110586714.5A CN202110586714A CN113355657A CN 113355657 A CN113355657 A CN 113355657A CN 202110586714 A CN202110586714 A CN 202110586714A CN 113355657 A CN113355657 A CN 113355657A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45561—Gas plumbing upstream of the reaction chamber
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention belongs to the technical field of chemical vapor deposition vacuum equipment and micro-nano film production, and particularly discloses a source-separating positioning vacuum tube furnace device which comprises a gas flow controller, a source placing component, a first flange plate, a tube furnace quartz tube and a second flange plate, wherein the source placing component comprises a first interface, a source placing tube, an extension tube and a temperature measuring tube; one end face of the first flange plate is provided with a plurality of second interfaces which are correspondingly arranged with the plurality of source placing components one by one, and the first flange plate and the second flange plate are respectively arranged at two ends of the quartz tube of the tube furnace. The device provided by the invention can independently and separately control each molecular source required by chemical vapor deposition growth, independently adjust the temperature, flow rate and position of each molecular source, can accurately meet the growth requirement of a nano film, and is easy to expand and convenient to adjust the flange end vacuum interface.
Description
Technical Field
The invention belongs to the technical field of chemical vapor deposition vacuum equipment and micro-nano film production, and particularly relates to a source-splitting positioning vacuum tube furnace device.
Background
The chemical vapor deposition technology is a material growth preparation technology which uses a high-temperature tube furnace in a vacuum/atmospheric environment, utilizes chemical reaction of an evaporated gaseous molecular source at a certain reaction temperature and deposits a nano-scale thin film on a substrate. The method has the characteristics of easy realization of technical conditions, low cost, high quality of the grown film and the like. The technology is widely used for semiconductor material research, laboratory preparation of high-quality two-dimensional materials such as graphene, transition metal halide and the like.
The tubular furnace of traditional chemical vapor deposition simple structure, the cover gas is direct from inlet end flange input, places reaction source and substrate in the furnace body quartz capsule inside, consequently can't adjust the position of reaction source and substrate during the growth, all directly is carried by the cover gas after every molecule source evaporation moreover, lacks independent adjustment. The growth of high quality two-dimensional materials requires precise control of the molecular source evaporation temperature and ratio, while the relative position of the reactive source and the substrate also significantly affects the deposition quality. Because of lack of accurate control of each growth parameter variable, the repeatability of the growth result is poor, the reliability of the experimental conditions is low, and the cost of the process flow is huge.
The design of the early adjustable relative position of the reactive molecule source and the substrate solves the problem that the growth parameters are difficult to adjust to a certain extent. But its complex mechanical design increases cost, reduces reliability, has poor vacuum expandability, and is overly dependent on the skill level of the operator during growth.
Disclosure of Invention
The invention aims to: the device provided by the invention can independently and separately control each molecular source required by chemical vapor deposition growth, independently adjust the temperature, flow rate and position of each molecular source, can accurately meet the growth requirement of a nano film, and is easy to expand a flange end vacuum interface and convenient to adjust.
In order to achieve the purpose, the invention adopts the following technical scheme: a vacuum tube furnace device with a source separation positioning function comprises a gas flow controller, a source placing component, a first flange plate, a tube furnace quartz tube and a second flange plate, wherein the gas flow controller is used for outputting gas with the volume flow of 5-200 sccm; the source placing component comprises a first interface, a source placing pipe, an extension pipe and a temperature measuring pipe, the source placing pipe and the gas flow controller are mutually communicated through the first interface, the extension pipe is sleeved outside the source placing pipe, and one end of the temperature measuring pipe penetrates through the first interface and is contained in the source placing pipe; a plurality of second interfaces are arranged on one end face of the first flange plate, and the second interfaces are connected with the source placing components in a one-to-one corresponding mode; one end of the quartz tube of the tube furnace is fixedly arranged on the first flange plate; the second flange plate is detachably arranged at the other end of the quartz tube of the tube furnace.
Further, still include step motor and control system, step motor is used for the drive flexible pipe carries out concertina movement, control system with step motor electric connection, control system is used for controlling step motor's step speed and step number.
The temperature measuring device further comprises a temperature measuring line and a temperature measuring meter, wherein one end of the temperature measuring line is inserted into the temperature measuring pipe, and the other end of the temperature measuring line is connected to the temperature measuring meter.
Furthermore, the telescopic pipe is provided with at least two sections, the length of the telescopic pipe is 1000-1200 mm, and the maximum compressible stroke of the telescopic pipe is 800 mm.
Further, the second interface is a CF interface.
Furthermore, four vacuum KF interfaces are radially distributed on the surface of the second flange plate, and the four vacuum KF interfaces are respectively connected with a vacuum gauge, a vacuum valve, a cold trap and a vacuum pump.
Further, the first flange plate and the second flange plate are provided with optical observation windows.
Furthermore, the first flange plate, the tube furnace quartz tube and the second flange plate are fixedly connected through vacuum double-O rubber rings.
Furthermore, one end of the temperature measuring tube is a closed end, and the closed end is accommodated in the source placing tube.
Furthermore, the first interface and the source placing pipe are fixedly connected through a vacuum KF25 quick-release clamp, and at least two KF16 reserved vacuum connecting ports are radially arranged on the first interface.
The invention has the beneficial effects that:
the source-separating positioning vacuum tube furnace device can independently and separately control each molecular source required by chemical vapor deposition growth, independently adjust the temperature, the evaporation flow rate and the position of each molecular source, and immediately control the start and stop of the growth.
And secondly, the design of vacuum interfaces of all elements can meet the requirements of high-vacuum growth environment and high temperature resistance.
And thirdly, the part has good vacuum expansibility, and standard KF interfaces are reserved for the first interface and the second flange plate and are used for installing pressure, temperature, airflow and other parameter detection and control equipment.
Drawings
FIG. 1 is a schematic structural diagram of a source-split positioning vacuum tube furnace apparatus according to an embodiment of the present invention;
FIG. 2 is a second schematic structural view of a source-positioned vacuum tube furnace apparatus according to an embodiment of the present invention;
FIG. 3 is a third schematic structural view of a vacuum tube furnace apparatus with a source-separated positioning according to an embodiment of the present invention;
FIG. 4 is a schematic structural view of a telescopic tube according to an embodiment of the present invention;
FIG. 5 is a schematic view of a first flange according to an embodiment of the present invention;
fig. 6 is a schematic structural diagram of a second flange according to an embodiment of the present invention.
Wherein: 1-a gas flow controller; 2-placing a source component; 21-a first interface; 22-source placing tube; 23-a telescopic tube; 24-a temperature measuring tube; 3-a first flange plate; 31-a second interface; 4-tube furnace quartz tube; 5-a second flange plate; 6-a step motor; 7-a control system; 8-temperature measuring line; 9-a temperature detector; 10-vacuum pump.
Detailed Description
In the description of the present application, unless explicitly stated or limited otherwise, the terms "first", "second", "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; the term "plurality" means two or more; the terms "connected," "secured," and the like are to be construed broadly and unless otherwise stated or indicated, and for example, "connected" may be a fixed connection, a removable connection, an integral connection, or an electrical connection; "connected" may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In the description of the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to make the technical solutions and advantages of the present invention clearer, the present invention and its advantages will be described in further detail below with reference to the following detailed description and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
As shown in fig. 1 to 6, the source-splitting positioning vacuum tube furnace device provided in this embodiment includes a gas flow controller 1, a source placing component 2, a first flange 3, a tube furnace quartz tube 4, a second flange 5, a stepping motor 6, a control system 7, a temperature measuring line 8 and a temperature measuring meter 9, wherein the gas flow controller 1 is configured to output a gas with a volume flow of 5 to 200 sccm; the source placing component 2 comprises a first interface 21, a source placing pipe 22, an extension pipe 23 and a temperature measuring pipe 24, the source placing pipe 22 and the gas flow controller 1 are communicated with each other through the first interface 21, the extension pipe 23 is sleeved outside the source placing pipe 22, and one end of the temperature measuring pipe 24 penetrates through the first interface 21 and is contained in the source placing pipe 22; one end face of the first flange plate 3 is provided with a plurality of second interfaces 31, and the plurality of second interfaces 31 are connected with the plurality of source placing components 2 in a one-to-one correspondence manner; one end of a quartz tube 4 of the tube furnace is fixedly arranged on the first flange plate 3; the second flange plate 5 is detachably mounted at the other end of the quartz tube 4 of the tube furnace, the stepping motor 6 is used for driving the extension tube 23 to perform telescopic motion, the control system 7 is electrically connected with the stepping motor 6, the control system 7 is used for controlling the stepping rotating speed and the step number of the stepping motor 6, one end of the temperature measuring line 8 is inserted into the temperature measuring tube 24, the other end of the temperature measuring line 8 is connected onto the temperature measuring meter 9, the first flange plate 3 is fixedly connected with the quartz tube 4 of the tube furnace and the second flange plate 5 through vacuum double-O rubber rings, one end of the temperature measuring tube 24 is a closed end, the closed end is accommodated in the source placing tube 22, the first interface 21 is fixedly connected with the source placing tube 22 through a vacuum KF25 quick-release clamp, and the first interface 21 is provided with at least two KF16 reserved vacuum connecting ports along the radial direction.
Specifically, the first interface 21 is a four-way air inlet interface, the source placing pipe 22 is a source placing quartz pipe, the extension pipe 23 is a vacuum corrugated pipe, the temperature measuring pipe 24 is a thermocouple temperature measuring quartz pipe, the temperature measuring line 8 is a K-type thermocouple temperature measuring line 8, the first flange 3 is an air inlet interface flange, the second flange 5 is an air outlet interface flange, and the stepping motor 6 is controlled in stepping speed and stepping number by the upper computer stepping motor control software (i.e., the control system 7).
Preferably, the vacuum bellows used in this embodiment is divided into five sections, the total length is 1200mm, the maximum compressible stroke is 800mm, the stepping motor 6 is connected to the vacuum bellows in sections through a screw mechanism, so that each section of the vacuum bellows can be driven to perform telescopic motion, and the compression stroke of the vacuum bellows can be accurately controlled, wherein the vacuum bellows can also be divided into a plurality of sections, such as 2 sections, 3 sections or 4 sections, and the compressible stroke is proportional to the total length of the vacuum bellows.
In the embodiment, the first flange 3 is a vacuum quartz tube flange, one end face of the first flange is provided with three second interfaces 31, the three second interfaces 31 are CF interfaces, the three second interfaces 31 are respectively and correspondingly provided with the source placing component 2, the three second interfaces 31 are all in an inclined shape of 1.5 degrees and are uniformly distributed on the outer end face of the first flange 3, the outer end face of the first flange 3 is also provided with an optical observation window, the structural design can be used for expanding an integrated on-line optical detection device, three sets of source placing components 2 are arranged on the end face of the first flange 3, and the device can provide independent carrier gas flow rate, positioning and temperature measurement and control for three molecular sources, wherein the molecular source positioning travel range is 0-800 mm, and the carrier gas flow rate control range is 5-200 sccm.
Preferably, the surface of the second flange plate 5 is radially distributed with four vacuum KF interfaces, the four vacuum KF interfaces are respectively connected with a vacuum gauge, a vacuum valve, a cold trap and a vacuum pump 10, the structural design is adopted, the second flange plate 5 can be used for carrying out parameter detection and control equipment such as installation pressure, temperature, air flow and the like, the surface of the second flange plate 5 is provided with an optical observation window, and the structural design is adopted, so that the integrated online optical detection device can be used for expanding.
In the embodiment, high-purity argon is used as shielding gas, the high-purity argon is output by a gas flow controller 1 to generate micro-flow gas with adjustable volume flow of 5-200sccm, the high-purity argon is output by three channels of the gas flow controller 1 and then input to a first interface 21 through a polytetrafluoroethylene gas pipe, the polytetrafluoroethylene gas pipe is fixedly connected with the first interface 21 through a clamping sleeve vacuum joint, the shielding gas enters a source-placing quartz pipe, then enters an air inlet interface flange plate, enters a quartz pipe 4 of a tube furnace through the air inlet interface flange plate, and finally is discharged from an air outlet interface flange plate.
Preferably, one end of the source placing tube 22 penetrates through the vacuum corrugated tube and is fixed in the telescopic vacuum corrugated tube by adopting a double-O rubber ring, one end of the temperature measuring tube 24 is inserted into the source placing tube from the first interface 21, the temperature measuring tube 24 is fixed at the first interface 21 by the double-O rubber ring, the outlet end (accommodated in the source placing quartz tube) of the temperature measuring tube 24 is a closed end, the K-type thermocouple temperature measuring wire 8 is inserted into the temperature measuring tube 24, and the thermometer 9 is connected outside the inlet end.
Before each chemical vapor deposition growth, the second flange plate 5 is firstly disassembled, then two reaction molecule sources are arranged in the source placing tube 22 and are contacted with the closed end of the temperature measuring tube 24, a substrate is arranged in a heating area in the quartz tube 4 of the tube furnace, the second flange plate 5 is reinstalled, the whole device is pumped to high vacuum, the quartz tube 4 of the tube furnace is heated and is introduced with carrier gas, after the air flow pressure and temperature are stable, the telescopic tube 23 is controlled by the control system 7 to drive the source placing tube 22 to move into the heating area of the quartz tube 4 of the tube furnace for heating, and the molecule sources are continuously and stably evaporated until the growth deposition is finished.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should understand that the embodiments as a whole may be combined as appropriate to form other embodiments understood by those skilled in the art.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. The utility model provides a vacuum tube furnace device is fixed a position to source which characterized in that includes:
the gas flow controller (1), the said gas flow controller (1) is used for outputting the gas with the volume flow of 5-200 sccm;
the source placing assembly (2), the source placing assembly (2) comprises a first interface (21), a source placing pipe (22), an extension pipe (23) and a temperature measuring pipe (24), the source placing pipe (22) and the gas flow controller (1) are communicated with each other through the first interface (21), the extension pipe (23) is sleeved outside the source placing pipe (22), and one end of the temperature measuring pipe (24) penetrates through the first interface (21) and is accommodated in the source placing pipe (22);
the device comprises a first flange plate (3), wherein one end face of the first flange plate (3) is provided with a plurality of second interfaces (31), and the plurality of second interfaces (31) are connected with a plurality of source placing components (2) in a one-to-one corresponding mode;
one end of the tube-type furnace quartz tube (4) is fixedly arranged on the first flange plate (3);
and the second flange plate (5) is detachably mounted at the other end of the tube furnace quartz tube (4).
2. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: still include step motor (6) and control system (7), step motor (6) are used for the drive flexible pipe (23) carry out concertina movement, control system (7) with step motor (6) electric connection, control system (7) are used for controlling step motor's (6) step speed and step number.
3. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: the temperature measuring device is characterized by further comprising a temperature measuring line (8) and a temperature measuring meter (9), wherein one end of the temperature measuring line (8) is inserted into the temperature measuring pipe (24), and the other end of the temperature measuring line (8) is connected to the temperature measuring meter (9).
4. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: the telescopic pipe (23) is provided with at least two sections, the length of the telescopic pipe (23) is 1000-1200 mm, and the maximum compressible stroke of the telescopic pipe (23) is 800 mm.
5. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: the second interface (31) is a CF interface.
6. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: and four vacuum KF interfaces are radially distributed on the surface of the second flange plate (5), and are respectively connected with a vacuum gauge, a vacuum valve, a cold trap and a vacuum pump (10).
7. The source-splitting positioning vacuum tube furnace device of claim 6, wherein: the first flange plate (3) and the second flange plate (5) are both provided with optical observation windows.
8. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: the first flange plate (3), the tube furnace quartz tube (4) and the second flange plate (5) are fixedly connected through a vacuum double-O rubber ring.
9. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: one end of the temperature measuring tube (24) is a closed end, and the closed end is accommodated in the source placing tube (22).
10. The source-splitting positioning vacuum tube furnace device of claim 1, wherein: the first interface (21) and the source placing pipe (22) are fixedly connected through a vacuum KF25 quick-release clamp, and the first interface (21) is provided with at least two KF16 reserved vacuum connecting ports along the radial direction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110586714.5A CN113355657B (en) | 2021-05-27 | 2021-05-27 | Source-dividing positioning vacuum tube furnace device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110586714.5A CN113355657B (en) | 2021-05-27 | 2021-05-27 | Source-dividing positioning vacuum tube furnace device |
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| CN113355657A true CN113355657A (en) | 2021-09-07 |
| CN113355657B CN113355657B (en) | 2022-10-28 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400760A (en) * | 2013-08-05 | 2013-11-20 | 电子科技大学 | Method and device for growing bismuth selenide single crystal film on silicon substrate |
| US20150368831A1 (en) * | 2014-06-18 | 2015-12-24 | King Abdullah University Of Science And Technology | Systems and methods for automated production of multi-composition nanomaterial |
| CN208653665U (en) * | 2018-05-31 | 2019-03-26 | 洛阳八佳电气科技股份有限公司 | A kind of low-temperature measurement device of intermediate frequency high temperature furnace |
| CN111074234A (en) * | 2019-12-31 | 2020-04-28 | 上海理工大学 | Device and method for growing two-dimensional material based on push-pull trolley mode |
| CN212988619U (en) * | 2020-11-05 | 2021-04-16 | 山东晶升电子科技有限公司 | Temperature measuring device of crucible descending method growth furnace |
-
2021
- 2021-05-27 CN CN202110586714.5A patent/CN113355657B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400760A (en) * | 2013-08-05 | 2013-11-20 | 电子科技大学 | Method and device for growing bismuth selenide single crystal film on silicon substrate |
| US20150368831A1 (en) * | 2014-06-18 | 2015-12-24 | King Abdullah University Of Science And Technology | Systems and methods for automated production of multi-composition nanomaterial |
| CN208653665U (en) * | 2018-05-31 | 2019-03-26 | 洛阳八佳电气科技股份有限公司 | A kind of low-temperature measurement device of intermediate frequency high temperature furnace |
| CN111074234A (en) * | 2019-12-31 | 2020-04-28 | 上海理工大学 | Device and method for growing two-dimensional material based on push-pull trolley mode |
| CN212988619U (en) * | 2020-11-05 | 2021-04-16 | 山东晶升电子科技有限公司 | Temperature measuring device of crucible descending method growth furnace |
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| CN113355657B (en) | 2022-10-28 |
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