CN219455950U - In-situ Raman test system in plasma environment - Google Patents
In-situ Raman test system in plasma environment Download PDFInfo
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- CN219455950U CN219455950U CN202220342727.8U CN202220342727U CN219455950U CN 219455950 U CN219455950 U CN 219455950U CN 202220342727 U CN202220342727 U CN 202220342727U CN 219455950 U CN219455950 U CN 219455950U
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Abstract
The utility model discloses an in-situ Raman test system in a plasma environment, which comprises: raman test device and material growth apparatus for growing samples in a plasma environment. The Raman test device is used for transmitting pulse optical signals to the material growth equipment and irradiating the pulse optical signals to the sample growing on the material growth equipment, the pulse optical signals excite the sample to generate pulse Raman scattering signals, the Raman test device is used for collecting the pulse Raman scattering signals in a pulse time domain, and a Raman scattering spectrum is obtained through data processing. According to the in-situ Raman test system disclosed by the utility model, the Raman test module is used for transmitting the pulse light signal and receiving the pulse time domain Raman scattering signal excited by the pulse light signal, so that the interference of parasitic light in a plasma environment on Raman spectrum test is reduced.
Description
Technical Field
The application relates to the technical field of online monitoring, in particular to an in-situ Raman test system in a plasma environment.
Background
Carbon materials, such as diamond, diamond-like carbon, graphene, carbon nanotubes, are important multifunctional materials with great application potential and scientific value, and are widely focused as a new material frontier field. The plasma chemical vapor deposition technology is suitable for preparing high-quality films and crystal materials with large area, good uniformity, high purity and good crystal morphology, is an effective means for obtaining high-end carbon materials, and related technological parameters directly influence the vapor growth environment in a reaction chamber so as to influence the quality of the carbon materials. Raman spectroscopy is a necessary means for detecting the structure and quality of the carbon material, and can accurately and rapidly determine the structure, type, defect and impurity conditions of the carbon material, thereby evaluating the quality and property of the material.
In the existing situation, carbon materials are prepared in material growth equipment, plasma luminescence in a reaction cavity is strong, and Raman spectrum testing is disturbed. Therefore, how to eliminate the interference of the parasitic light in the carbon material preparation process to the raman spectrum test has been the subject of research by those skilled in the art.
Disclosure of Invention
The embodiment of the application mainly aims at providing an in-situ Raman test system in a plasma environment, and aims at providing an in-situ Raman test system in a plasma environment, which reduces parasitic light interference in Raman spectrum testing.
In a first aspect, embodiments of the present application provide an in-situ raman test system in a plasma environment, comprising:
a material growth apparatus for growing a sample in a plasma environment;
the Raman test device is used for emitting a pulse optical signal to the material growth equipment and irradiating the pulse optical signal to a sample growing on the material growth equipment, and the pulse optical signal excites the sample to generate a pulse Raman scattering signal; and the method is used for collecting pulse Raman scattering signals in a pulse time domain and obtaining Raman scattering spectra through data processing.
In some embodiments, the raman test device comprises a pulsed laser, the pulsed light signal emitted by the pulsed laser is an ultraviolet pulsed signal, and the wavelength of the pulsed signal is less than 300nm.
In some embodiments, the raman test Device further comprises a photodetector provided with an ICCD (enhanced charge coupled Device) for collecting the raman scattering signal in the pulse time domain of the pulsed raman scattering signal.
In some embodiments, the raman test device further comprises a raman test module comprising a light emitting assembly, a light receiving assembly, a transflective assembly, and a light condensing assembly;
the light receiving assembly transmits the Raman scattering signals to the light detector.
In some embodiments, the raman test module further comprises a light filtering component disposed between the transflective component and the light receiving component;
wherein the light receiving assembly comprises a reflector and a focusing lens;
the focusing lens is arranged between the reflecting mirror and the light detector, the reflecting mirror is used for reflecting the Raman scattering signals so as to transmit the Raman scattering signals to the light detector through the focusing lens, and the transmission direction of the Raman scattering signals reflected by the reflecting mirror is parallel to the light emergent direction of the light emitting component.
In some embodiments, the light receiving component includes a mirror, a focusing lens, and a filtering component;
the reflecting mirror is used for reflecting the Raman scattering signals so as to transmit the Raman scattering signals to the optical detector through the focusing lens, and the transmission direction of the side Raman scattering signals after being reflected by the reflecting mirror is parallel to the light emergent direction of the light emitting component;
the filter component is arranged between the reflecting mirror and the focusing lens or between the reflecting mirror and the transflective component.
In some embodiments, the light emitting component includes a light filter and a collimator lens, where the light filter and the collimator lens are sequentially arranged in a light emitting direction, and a pulse light signal emitted by the pulse laser is converted into ultraviolet monochromatic light after passing through the light filter.
In some embodiments, a material growth apparatus includes a reaction assembly and a seal assembly;
the reaction assembly comprises a main body part and an observation connecting part connected with the main body part, and the main body part is provided with a reaction cavity for providing a growth environment for a sample; the observation connection part is formed with an observation channel which is communicated with the reaction cavity and is provided with an opening; the sealing component is connected with the observation connecting part and is used for sealing the opening of the observation channel and enabling the opening of the observation channel to form a light-transmitting part; the pulse laser signal emitted by the Raman testing device irradiates the sample in the reaction cavity through the observation channel by the light transmission part.
In some embodiments, the in situ raman test system further comprises a transfer assembly for connecting the material growth apparatus with the raman test device;
the switching assembly comprises a first switching piece and a second switching piece, wherein the first switching piece is detachably connected with the observation connecting part and is provided with a through hole corresponding to the light transmission part, and the second switching piece is connected with the first switching piece and is detachably connected with the Raman test module.
In some embodiments, the first adapter comprises a bottom plate, a side plate and an adapter fixing piece, wherein the side plate is annularly arranged on the periphery of the bottom plate, and the through hole is formed in the bottom plate; the curb plate interval is provided with the fixed orifices, and the switching mounting passes through the fixed orifices and surveys connecting portion adaptation to make to survey connecting portion and first adaptor detachable connection.
According to the in-situ Raman test system under the plasma environment, the Raman test module transmits the pulse light signals and excites the sample to generate pulse Raman scattering signals, the pulse Raman signals exciting the sample in one pulse time are stronger than plasma fluorescence of continuous signals, stray light interference accepted by the Raman test module is reduced, and therefore a clearer spectrogram is obtained.
Icon: 10. a material growth apparatus; 11. a reaction assembly; 111. a main body portion; 112. an observation connection portion; 113. a light transmitting portion; 12. a seal assembly; 13. a sample;
20. a raman test device; 21. a housing; 22. a light emitting assembly; 23. a light receiving assembly; 24. a transflector assembly; 25. a light gathering assembly; 26. a light filtering component; 28. a pulsed laser; 222. a light filter; 223. a collimator lens; 231. a reflecting mirror; 232. a focusing lens; 29. a photodetector;
30. a switching component; 31. a first adapter; 32. a second adapter; 321. a first light-transmitting port; 322. a connection hole; 311. a bottom plate; 312. a side plate; 313. a through hole; 314. and a fixing hole.
Drawings
FIG. 1 is a schematic diagram of an explosion structure of an in-situ Raman test system according to the present utility model;
FIG. 2 is a schematic diagram of a Raman testing module optical path of the in-situ Raman testing system according to the present utility model;
FIG. 3 is a schematic diagram of a Raman testing module according to another variation of the in situ Raman testing system according to the present utility model;
fig. 4 is a schematic structural diagram of a switching component of the in-situ raman test system of the present utility model.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
In the description of the present application, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art in a specific context.
At present, materials are prepared in material growth equipment in a plasma environment, plasma luminescence in a reaction cavity is strong, and Raman spectrum testing is disturbed.
In order to solve the above problems, the present utility model provides an in-situ raman test system in a plasma environment.
Some embodiments of the present application will be described in detail below with reference to the accompanying drawings, and the following examples and features of the examples may be combined with each other without conflict.
Referring to fig. 1, fig. 1 is an in-situ raman test system provided in an embodiment of the present application, which includes a material growth apparatus 10 and a raman test device 20.
The material growth apparatus 10 is used to grow a sample 13 in a plasma environment. The raman test device 20 is configured to emit a pulsed light signal to the material growth apparatus 10 and irradiate the sample 13 grown on the material growth apparatus 10, and the pulsed light signal excites the sample 13 to generate a pulsed raman scattering signal. The raman test device 20 is further configured to collect a pulse raman scattering signal in a pulse time domain, and obtain a raman scattering spectrum through data processing.
Illustratively, material growth apparatus 10 grows sample 13 in a plasma environment, and material growth apparatus 10 may be a microwave plasma chemical vapor deposition (MPCVD, microwave Plasma Chemical Vapor Deposition) apparatus or a plasma enhanced chemical vapor deposition (PECVD, plasma Enhanced Chemical Vapor Deposition) apparatus. The grown sample 13 may be diamond or other carbon material, or may be other chemicals that are required for raman spectroscopy testing.
In some embodiments, the material growth apparatus 10 may also be a physical vapor deposition (PVD, physical Vapour Deposition) apparatus that grows the sample 13 in a plasma environment, and the raman test device 20 performs in situ raman spectroscopy on the sample 13.
After the technical scheme is adopted, the Raman testing device 20 emits the pulse optical signal and excites the sample 13 to generate the pulse Raman scattering signal, the pulse Raman signal exciting the sample 13 in one pulse time is stronger than the plasma fluorescence of the continuous signal, and the parasitic light interference received by the Raman testing module 20 is reduced, so that a clearer spectrogram is obtained.
Referring to fig. 2, in some embodiments, the raman test device 20 includes a pulse laser 28, the pulse light signal emitted by the pulse laser is an ultraviolet pulse signal, and the wavelength of the pulse signal is less than 300nm.
Since the ultraviolet raman signal is stronger than the visible and infrared raman signals, the shorter the wavelength, the larger the raman scattering cross-section, and the stronger the raman signal intensity. Under the same conditions, signals with the same intensity are generated, and the laser power required by ultraviolet is smaller. The plasma luminescence spectrum is generally more than 300nm, and the Raman scattering light signal of the laser excitation material below 300nm is below 300nm, so that the ultraviolet Raman detection is less influenced by the interference of the ambient light and the background light, and the interference of the background light caused by the plasma luminescence is avoided, so that a clear spectrogram is obtained.
In some embodiments, the material growth apparatus 10 may also be a hot filament chemical vapor deposition (HFCVD, hot Filament Chemical Vapor Deposition) apparatus, where HFCVD generates a certain plasma and the filament emits a strong light after being heated at high temperature, which greatly interferes with raman spectroscopy testing of the sample 13 being grown. Because the luminescence is mainly visible light, the interference of the filament luminescence to the Raman spectrum test can be effectively avoided by using the ultraviolet Raman test.
Referring to fig. 2, in some embodiments, the raman test device 20 further comprises a light detector 29 provided with an ICCD, the light detector 29 being configured to collect the raman scattering signal in the pulse time domain of the pulsed raman scattering signal.
In some embodiments, the raman test device 20 further comprises a raman test module comprising a light emitting assembly 22, a light receiving assembly 23, a transflective assembly 24, and a light condensing assembly 25.
The transflective component 24 is disposed between the light emitting component 22 and the light condensing component 25, the pulsed light signal emitted by the pulse laser 28 is collimated by the light emitting component 22, and then focused by the transflective component 24 and the light condensing component 25 to irradiate the sample 13 in the material growing device 10, the sample 13 is excited to generate a pulsed raman scattering signal, the pulsed raman scattering signal is reflected by the transflective component 24 to the light receiving component 23, and the raman scattering signal is transmitted by the light receiving component 23 to the light detector 29. Illustratively, the transflective assembly 24 may be a dichroic mirror or a dichroic mirror.
In some embodiments, the raman test module further comprises a filter assembly 26, the filter assembly 26 being disposed between the transflective assembly 24 and the light receiving assembly 23.
Wherein the light receiving assembly 23 comprises a mirror 231 and a focusing lens 232. The focusing lens 232 is disposed between the reflecting mirror 231 and the photodetector 29, and the reflecting mirror 231 is used for reflecting the raman scattering signal, so that the raman scattering signal is transmitted to the photodetector 29 through the focusing lens 232, and the transmission direction of the raman scattering signal reflected by the reflecting mirror 231 is parallel to the light emitting direction of the light emitting component 22. By providing the reflecting mirror 231, the transmission direction of the side raman scattering signal reflected by the reflecting mirror 231 and the light emitting direction of the light emitting assembly 22 are parallel to each other, so that the volume of the raman test device 20 is reduced.
Referring to fig. 2 and 3, the filter assembly 26 is disposed between the mirror 231 and the focusing lens 232, or the filter assembly 26 is disposed between the mirror 231 and the transflective assembly 24.
In some embodiments, the light emitting component 22 includes a light filter 222 and a collimator 223, where the light filter 222 and the collimator 223 are sequentially disposed in the light emitting direction, and the pulse light signal emitted by the pulse laser 28 is converted into ultraviolet monochromatic light after passing through the light filter 222.
Referring to fig. 1, in some embodiments, a material growth apparatus 10 includes a reaction assembly 11 and a seal assembly 12.
The reaction module 11 includes a main body 111 and an observation connection part 112 connected to the main body 111, and the main body 111 is formed with a reaction chamber for providing a growth environment for the sample 13; the observation connection part 112 is formed with an observation channel that communicates with the reaction chamber and has an opening. The sealing assembly 12 is connected to the observation connection part 112 for sealing the opening of the observation path and forming the opening of the observation path into a light-transmitting part 113. The pulsed laser signal emitted from the raman test device 20 is irradiated to the sample 13 in the reaction chamber from the observation channel through the light transmitting portion 113.
Illustratively, the sample 13 is a carbon material, such as diamond, graphene, etc., and the material growth apparatus 10 uses microwave plasma chemical vapor deposition techniques to prepare the carbon material. The sealing assembly 12 comprises a flange and quartz glass, which together seal the opening of the viewing channel and from which light transmission is achieved. It will be appreciated that the seal assembly 12 may be sealed and optically transparent in other ways, and that the viewing interface 112 may be provided in a plurality, not limited thereto.
Referring to fig. 1 and 4, in some embodiments, the in situ raman test system further comprises a pod 30 for coupling the material growth apparatus 10 and the raman test device 20. Wherein the adapter assembly 30 comprises a first adapter 31 and a second adapter 32.
The first adapter 31 is detachably connected to the observation connection part 112 and is provided with a through hole 313 corresponding to the light transmission part 113, and the second adapter 32 is connected to the first adapter 31 and is detachably connected to the housing 21 of the raman test module 20.
The surface of the second adaptor 32 is provided with a first light-transmitting opening 321, a connecting hole 322 is disposed around the first light-transmitting opening 321, an opening (not shown) is disposed on the housing 21, one end of the connecting rod is inserted into the connecting hole 322 of the second adaptor 32, and the other end is inserted into the opening disposed on the housing 21, so as to connect the adaptor assembly 30 and the housing 21. It will be appreciated that the connection of the housing 21 to the adapter assembly 30 may be selected in a number of ways, and is not limited herein.
In some embodiments, the first adaptor 31 includes a bottom plate 311, a side plate 312 surrounding the bottom plate 311, and an adaptor fixture (not shown).
Specifically, the through hole 313 is formed in the bottom plate 311, the side plates 312 are provided with fixing holes 314 at intervals, and the adapting fixing member is adapted to the observation connecting portion 112 through the fixing holes 314, so that the observation connecting portion 112 is detachably connected with the first adapting member 31.
For example, the fixing hole 314 may be provided with threads, and the adaptor fixing may be a screw. The first adapter 31 is sleeved on the observation connecting part 112, and a screw is screwed into the fixing hole 314 under the action of external force, so that the observation connecting part 112 is connected with the first adapter 31. Or the screw is screwed out of the fixing hole 314 under the action of external force, so that the first adapter 31 and the observation connecting part 112 are detached.
When the raman spectrum test needs to be performed on the sample 13, the raman test module 20 can be connected with the observation connection portion 112 of the material growth apparatus 10 through the adapter assembly 30, and the optical signal transmission is realized by the raman scattering signal excited by the sample 13 and the optical signal emitted by the raman test module 20 through the light transmission portion 113, the through hole 313 corresponding to the first adapter 31, and the first light transmission port 321 corresponding to the second adapter 32. When raman spectroscopy is not required, the adaptor assembly 30 may be disconnected from the observation connection unit 112.
It should also be understood that the term "and/or" as used in this specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
While the utility model has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the utility model. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (10)
1. An in-situ raman test system in a plasma environment, comprising:
a material growth apparatus for growing a sample in a plasma environment;
the Raman testing device is used for emitting a pulse optical signal to the material growing equipment and irradiating the sample growing on the material growing equipment, and the pulse optical signal excites the sample to generate a pulse Raman scattering signal; and the method is used for collecting pulse Raman scattering signals in a pulse time domain and obtaining Raman scattering spectra through data processing.
2. The in-situ raman test system according to claim 1, wherein said raman test device comprises a pulsed laser, wherein a pulsed light signal emitted from said pulsed laser is an ultraviolet pulsed signal, and the wavelength of the pulsed signal is less than 300nm.
3. The in situ raman test system according to claim 2, wherein said raman test device further comprises a light detector provided with an enhanced charge coupler for collecting raman scattering signals in a pulse time domain of the pulsed raman scattering signals.
4. The in situ raman test system according to claim 3, wherein said raman test device further comprises a raman test module comprising a light emitting assembly, a light receiving assembly, a transflective assembly, and a light condensing assembly;
wherein the transreflective component is arranged between the light emitting component and the light condensing component, the pulse light signal emitted by the pulse laser is collimated by the light emitting component and then focused by the transreflective component and the light condensing component to irradiate the sample in the material growing equipment, the sample is excited to generate a pulse Raman scattering signal, the transflective assembly reflects the pulse Raman scattering signal to the light receiving assembly, and the light receiving assembly transmits the Raman scattering signal to the light detector.
5. The in situ raman test system according to claim 4, wherein said raman test module further comprises a light filtering assembly disposed between said transflective assembly and said light receiving assembly;
wherein the light receiving assembly comprises a reflector and a focusing lens;
the focusing lens is arranged between the reflecting mirror and the light detector, the reflecting mirror is used for reflecting the Raman scattering signals, so that the Raman scattering signals are transmitted to the light detector through the focusing lens, and the transmission direction of the Raman scattering signals reflected by the reflecting mirror is parallel to the light emergent direction of the light emitting component.
6. The in situ raman test system according to claim 4 wherein said light receiving assembly comprises a mirror, a focusing lens and a filtering assembly;
the reflecting mirror is used for reflecting the Raman scattering signals so as to transmit the Raman scattering signals to the optical detector through the focusing lens, and the transmission direction of the side Raman scattering signals reflected by the reflecting mirror is parallel to the light emergent direction of the light emitting component;
the light filtering component is arranged between the reflecting mirror and the focusing lens or between the reflecting mirror and the transflective component.
7. The in-situ Raman test system according to claim 4, wherein the light emitting assembly comprises a light filter and a collimating lens, the light filter and the collimating lens are sequentially arranged in the light emitting direction, and the pulse light signal emitted by the pulse laser is converted into ultraviolet monochromatic light after passing through the light filter.
8. The in situ raman test system according to claim 4, wherein said material growth apparatus comprises a reaction assembly and a sealing assembly;
the reaction assembly comprises a main body part and an observation connecting part connected with the main body part, wherein the main body part is provided with a reaction cavity for providing a growth environment for a sample; the observation connection part is formed with an observation channel which is communicated with the reaction cavity and is provided with an opening; the sealing component is connected with the observation connecting part and is used for sealing the opening of the observation channel and enabling the opening of the observation channel to form a light transmission part; the pulse laser signal emitted by the Raman testing device irradiates the sample in the reaction cavity from the observation channel through the light transmission part.
9. The in situ raman test system of claim 8, further comprising a transition assembly for connecting the material growth apparatus with the raman test device;
the switching assembly comprises a first switching piece and a second switching piece, wherein the first switching piece is detachably connected with the observation connecting part, a through hole corresponding to the light transmission part is formed in the first switching piece, and the second switching piece is connected with the first switching piece and detachably connected with the Raman test module.
10. The in-situ raman test system according to claim 9, wherein the first adapter comprises a bottom plate, a side plate and an adapter fixing piece, wherein the side plate is annularly arranged on the periphery of the bottom plate, and the through hole is formed in the bottom plate; the side plates are provided with fixing holes at intervals, and the switching fixing piece is matched with the observation connecting part through the fixing holes, so that the observation connecting part is detachably connected with the first switching piece.
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| CN202220342727.8U CN219455950U (en) | 2022-02-18 | 2022-02-18 | In-situ Raman test system in plasma environment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117288740A (en) * | 2023-11-27 | 2023-12-26 | 四方光电股份有限公司 | Raman probe-based battery charge-discharge gas production in-situ test device and test method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117288740A (en) * | 2023-11-27 | 2023-12-26 | 四方光电股份有限公司 | Raman probe-based battery charge-discharge gas production in-situ test device and test method |
| CN117288740B (en) * | 2023-11-27 | 2024-03-19 | 四方光电股份有限公司 | Raman probe-based battery charge-discharge gas production in-situ test device and test method |
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