CN216337944U - Nano film preparation equipment - Google Patents
Nano film preparation equipment Download PDFInfo
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- CN216337944U CN216337944U CN202122640181.2U CN202122640181U CN216337944U CN 216337944 U CN216337944 U CN 216337944U CN 202122640181 U CN202122640181 U CN 202122640181U CN 216337944 U CN216337944 U CN 216337944U
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Abstract
The utility model relates to the technical field of film preparation, in particular to a nano film preparation device.A first reaction source is continuously introduced into a reaction chamber, a second reaction source is introduced into the reaction chamber in a pulse mode to react with the first reaction source, so that a film is deposited on a substrate, the pulse frequency ratio of the second reaction source is adjusted to accurately control the component ratio of different elements in a multi-component film, the thickness of the multi-component film can be controlled by an over-cycle number, and the reaction chamber can be heated to a higher temperature, so that the thickness of the film can be accurately controlled in an atomic scale, and the purposes of preparing the film at a high temperature and controlling the crystallinity and the thickness of the film are achieved.
Description
Technical Field
The utility model relates to the technical field of film preparation, in particular to a nano film preparation device.
Background
Prior art thin film formation techniques are primarily Atomic Layer Deposition (ALD) and Chemical Vapor Deposition (CVD).
(1) Atomic Layer Deposition (ALD) is a technological process for forming thin films by alternately passing pulses of vapor phase precursors into a reaction chamber and causing chemisorption reactions on the substrate surface (as shown in fig. 1), featuring self-limiting and self-saturation. The ALD technology has the advantages of excellent three-dimensional shape retention, large-area uniformity and accurate thickness controllability, and is particularly suitable for gap-filling growth of complex surface shapes and high-depth-width structures; the film thickness is accurately and simply controlled, and the thickness of the grown film is controlled by the reaction cycle times; and a lower deposition temperature is used, and a specific process can be carried out even at room temperature; is suitable for interface modification and preparation of a nano-scale multi-component laminated structure. But the method has a stable temperature growth window, and the deposition process is insensitive to the change of factors such as temperature, precursor metering, gas flow and the like in the temperature range. The temperature of the film deposited by the ALD method is relatively low, generally below 400 ℃, the deposited film is mostly in an amorphous state, and a small amount of the deposited film is in a single crystal state, so that the ALD method is difficult to obtain the single crystal film with controllable atomic scale. While most organometallic reaction sources decompose spontaneously at high temperatures, thus limiting the temperature of the ALD reaction.
(2) Chemical Vapor Deposition (CVD) is a vapor deposition method of thin films in which a reaction source is simultaneously delivered to a reaction chamber under carrier gas transport, as shown in fig. 2. The reaction temperature of the method can reach higher temperature, and the method can be used for depositing the single crystal film. The CVD deposition film is mainly controlled by parameters such as reaction time control, reaction temperature and the like, the method cannot accurately control the film thickness in an atomic scale, and accurate control of the components of the ternary film is not easy to realize.
Disclosure of Invention
Aiming at the problems in the prior art, the utility model provides a nano film preparation device, wherein a first reaction source is continuously introduced into a reaction chamber, a second reaction source is introduced into the reaction chamber in a pulse mode to react with the first reaction source, so that a film is deposited and formed on a substrate, the pulse frequency ratio of the second reaction source is adjusted, the component ratio of different elements in a multi-component film can be accurately controlled, the thickness of the multi-component film can be controlled by an overcycling number, and the reaction chamber can be heated to a higher temperature, so that the purposes of preparing the film at a high temperature and controlling the thickness of the film are achieved.
In order to solve the technical problems, the utility model adopts the following technical scheme: a nano-film preparation device comprises a frame, and a pulse reaction source device, a reaction chamber and a vacuum device which are all arranged on the frame, wherein an outlet of the pulse reaction source device is communicated with the reaction chamber, and the vacuum device is used for keeping the vacuum state in the reaction chamber; the device comprises a reaction chamber, a pulse reaction source device and a control device, wherein a continuous reaction source device is arranged at an inlet of the reaction chamber and is used for introducing a first continuous gas-phase reaction source into the reaction chamber, a substrate is placed in the reaction chamber, the pulse reaction source device comprises a plurality of reaction source bottles, a second reaction source is arranged in each reaction source bottle, and the reaction source bottles are used for alternately introducing a pulse-type second reaction source into the reaction chamber; the periphery of the reaction chamber is provided with a reaction heating device which is used for heating the reaction chamber, so that the pulse type second reaction source in the reaction chamber reacts with the first reaction source and forms a nano film on the substrate.
Preferably, the continuous reaction source device includes a solid first reaction source, a reaction pipeline for placing the solid first reaction source, and a first heater installed on the periphery of the reaction pipeline, the first heater is used for heating the reaction pipeline to vaporize the fixed first reaction source, the reaction pipeline is communicated with both the pulse reaction source device and the reaction chamber, the outlet of the reaction pipeline is hermetically connected with the inlet of the reaction chamber, and the inlet of the reaction pipeline is hermetically connected with the outlet of the pulse reaction source device.
Preferably, the pulse reaction source device further comprises a pulse carrying assembly, the pulse carrying assembly comprises a second heater and a transmission pipeline arranged on the second heater, an outlet of the transmission pipeline is communicated with the reaction chamber, and an inlet of the reaction chamber is hermetically sleeved on the transmission pipeline; the pulse type second reaction source generated by the reaction source bottle is introduced into the transmission pipeline after passing through the second heater, the transmission pipeline introduces the second reaction source into the reaction chamber, and the second heater is used for heating the generated second reaction source.
Preferably, the outer periphery of the conveying pipeline is provided with a third heater, and the third heater is used for heating the conveying pipeline.
Preferably, the outlets of the reaction source bottles reach the inlet of the reaction chamber at equal distances.
Preferably, the frame is further provided with a position adjusting device for adjusting the position of the reaction chamber.
Preferably, the position adjusting device comprises a slide rail mounted on the frame and a slide block slidably connected with the slide rail, and the reaction chamber is detachably connected with the slide block.
Preferably, the vacuum device comprises a vacuum measuring instrument, CvAn adjustable flapper valve and a vacuum pump, the outlet of the reaction chamber being in communication with the vacuum pump, CvAn adjustable flapper valve installed between the vacuum pump and the reaction chamber, CvAn adjustable flapper valve is used to adjust the pressure of the reaction chamber, and the vacuum measurement instrument is used to measure the pressure of the reaction chamber.
Preferably, the reaction chamber is a quartz tube.
Preferably, the reaction chamber is provided integrally with the reaction conduit.
The utility model has the beneficial effects that:
according to the nano film preparation equipment provided by the utility model, a first reaction source is continuously introduced into a reaction chamber, and a second reaction source is introduced into the reaction chamber in a pulse mode to react with the first reaction source, so that a film is deposited on a substrate; if a plurality of second reaction sources exist, the second reaction sources with a certain pulse number ratio are circularly and alternately introduced into the reaction chamber, and different second reaction sources react with the first reaction source to form the multi-component film. The utility model can accurately control the component ratio of different elements in the multi-component film by adjusting the pulse frequency ratio of the second reaction source, the thickness of the multi-component film can be controlled by the overcycling number, and the reaction chamber can be heated to a higher temperature, thereby realizing the purposes of preparing the film at a high temperature and controlling the thickness of the film.
Drawings
FIG. 1 illustrates a prior art atomic layer deposition method;
FIG. 2 illustrates a prior art CVD method;
FIG. 3 is a first schematic structural diagram of the present invention;
FIG. 4 is a second schematic structural view of the present invention;
FIG. 5 is a cross-sectional view of the present invention;
FIG. 6 is a third schematic structural view of the present invention;
FIG. 7 illustrates the deposition of a binary film according to the present invention;
FIG. 8 illustrates the deposition of a ternary film according to the present invention.
The reference numerals in fig. 1 to 8 include:
1-frame, 2-pulse reaction source device, 3-reaction chamber, 5-reaction source bottle, 6-reaction heating device, 7-second heater, 8-transmission pipeline, 9-third heater, 10-reaction pipeline, 11-first heater, 12-slide rail, 13-slide block, 14-vacuum measuring instrument, 15-CvAdjustable flapper valve, 16-vacuum pump.
Detailed Description
In order to facilitate understanding of those skilled in the art, the present invention will be further described with reference to the following examples and drawings, which are not intended to limit the present invention. The present invention is described in detail below with reference to the attached drawings.
Referring to fig. 3 to 6, the apparatus for preparing a nano-film according to the present embodiment includes a frame 1, and a pulse reaction source device 2, a reaction chamber 3, and a vacuum device, all mounted on the frame 1, wherein an outlet of the pulse reaction source device 2 is communicated with the reaction chamber 3, and the vacuum device is used for maintaining a vacuum state in the reaction chamber 3; a continuous reaction source device is arranged at an inlet of the reaction chamber 3 and used for introducing a first continuous gas-phase reaction source into the reaction chamber 3, a substrate is placed in the reaction chamber 3, the pulse reaction source device 2 comprises a plurality of reaction source bottles 5, a second reaction source is arranged in each reaction source bottle 5, and the reaction source bottles 5 are used for alternately introducing a pulse-type second reaction source into the reaction chamber 3; the periphery of the reaction chamber 3 is provided with a reaction heating device 6, and the reaction heating device 6 is used for heating the reaction chamber 3, so that the pulse type second reaction source in the reaction chamber 3 reacts with the first reaction source and forms a nano film on the substrate.
In this embodiment, a thin film is formed by a chemical reaction and surface adsorption by means of pulse-type chemical vapor deposition (P-CVD). Specifically, as shown in fig. 6 and 7, the reaction chamber 3 is continuously filled with a first reaction source, such as a reaction source C shown in fig. 7 (hereinafter, the reaction source C is referred to as the first reaction source), the number of the second reaction sources may be one or more, and the reaction shown in fig. 7 is described here, where, for example, the second reaction source in fig. 7 is a precursor a, and an outlet of the reaction source bottle 5 is provided with a pulse diaphragm valve, so that after the reaction source bottle 5 is heated, a pulse-type precursor a can be generated through the pulse diaphragm valve, and a manner of generating the pulse-type reaction source is the prior art, which is not described herein again; then, the pulse-type precursor a generated by the reaction source bottle 5 is introduced into the reaction chamber 3, reacts with the reaction source C, and is adsorbed on the substrate by the action of chemical bonds, van der waals force and the like to deposit and form the binary film ACx. In this embodiment, the thickness of the deposited film can be precisely controlled at atomic level by adjusting the pulse frequency of the reaction source a, the thickness of the film grown by a single pulse is constant within a certain temperature range, and the crystallinity and other quality parameters of the deposited film can be adjusted by adjusting parameters such as carrier gas flow, precursor a pulse width, vapor pressure of the reaction source C, pressure of the reaction chamber 3, and temperature of the reaction chamber 3. In this embodiment, by combining two modes of atomic layer deposition and chemical vapor deposition, the reaction chamber 3 can be heated to a higher temperature, and then the thickness of the thin film can be accurately controlled by adjusting the pulse frequency of the pulse-type precursor a, which can be realized no matter how thin or how thick, thereby realizing the purposes of preparing the thin film at a high temperature and controlling the thickness of the thin film.
When a plurality of reaction source bottles 5 are provided with different second reaction sources, multi-component film deposition can be realized, as shown in fig. 8, which is deposition of a ternary film ABwCz, and the following figure is taken as an example to illustrate deposition of a multi-component film. FIG. 8 shows the upper left and lower left views of the deposition of two binary films, ACx and ABy, respectively, by P-CVD. By combining the left binary film growth method, the precursor A, B of the reaction source is alternately introduced into the reaction chamber 3 at a certain pulse number ratio to react with the co-reaction source C and deposit a film on the substrate. FIG. 8 shows that the pulse number ratio of A/B is 2/1, the composition ratio of the A/B element in the ternary film ABwCz can be accurately controlled by adjusting the pulse number ratio of A/B, the thickness of the ternary film can be controlled by the number of over cycles, and thus the problem that the ternary film is difficult to prepare by the traditional chemical vapor deposition CVD is solved.
Referring to fig. 5 and 6, a continuous reaction source device of a first reaction source for generating a gas phase includes a solid first reaction source, a reaction pipe 10 for placing the solid first reaction source, and a first heater 11 installed at the periphery of the reaction pipe 10, where the first heater 11 is used to heat the reaction pipe 10 to vaporize the fixed first reaction source, the reaction pipe 10 is communicated with both the pulse reaction source device 2 and the reaction chamber 3, an outlet of the reaction pipe 10 is hermetically connected to an inlet of the reaction chamber 3, and an inlet of the reaction pipe 10 is hermetically connected to an outlet of the pulse reaction source device 2. In addition, the pulse reaction source device 2 further comprises a pulse transmission assembly, the pulse transmission assembly comprises a second heater 7 and a transmission pipeline 8 arranged on the second heater 7, an outlet of the transmission pipeline 8 is communicated with the reaction chamber 3, and an inlet of the reaction chamber 3 is hermetically sleeved on the transmission pipeline 8; the pulse type second reaction source generated by the reaction source bottle 5 passes through the second heater 7 and then is introduced into the transmission pipeline 8, the transmission pipeline 8 introduces the second reaction source into the reaction chamber 3, and the second heater 7 is used for heating the generated second reaction source.
Specifically, the reaction tube 10 is mainly used for placing the reaction source C of the solid, and the reaction tube 10 is integrally provided with the reaction chamber 3, and preferably a quartz tube is used. The reaction source C is arranged in a vacuum quartz tube between the pulse reaction source device 2 and the reaction chamber 3, the temperature of the region is lower than that of the reaction region, namely the reaction chamber 3, and higher than that of the pulse reaction source device 2, the reaction source C can be gasified in the temperature region to obtain a gas phase reaction source C, and the reaction chamber 3 is filled with the reaction source C under the action of carrier gas and free diffusion. The pulsed reaction source device 2 can deliver the second reaction source A, B, D, E in fig. 6 to the reaction chamber 3 to react with the reaction source C to form a thin film. The reaction source C is arranged at the front end of the reaction chamber 3, so that the structure is simpler, and the simplified structure can better ensure the vacuum characteristic in the reaction chamber 3. The front end of the pulse reaction source is connected with an independent pulse reaction source pipeline, each pulse reaction source pipeline comprises a pulse diaphragm valve and a reaction source bottle 5 with a manual valve, the reaction source bottles 5, the pulse diaphragm valves and a transmission pipeline 8 are heated in real time, as shown in fig. 6, a pulse second reaction source generated by the reaction source bottles 5 is continuously heated at a second heater 7, a third heater 9 is also arranged on the periphery of the transmission pipeline 8 to prevent the second reaction source from being cooled in the transmission pipeline 8 and ensure that pulse type second reaction source steam smoothly enters the reaction chamber 3, so that the temperature distribution of the whole nano film preparation equipment is gradually increased from the reaction source bottles 5, the pulse diaphragm valves, the pulse transfer component and a first heater 11 of the reaction source C to the reaction chamber 3.
Further, the outlets of the reaction source bottles 5 of the present embodiment reach the inlets of the reaction chambers 3 at equal distances. Therefore, the reaction of different second reaction sources can be prevented from being influenced by the interference of the path, and the accuracy and precision of film deposition can be further improved.
In the nano-film manufacturing apparatus provided in this embodiment, as shown in fig. 3, the frame 1 is further provided with a position adjusting device for adjusting a position of the reaction chamber 3, the position adjusting device includes a slide rail 12 installed on the frame 1 and a slide block 13 slidably connected to the slide rail 12, and the reaction chamber 3 is detachably connected to the slide block 13.
In particular, different reactants can be adapted by adjusting the position of the reaction chamber 3, and the application range is wider. The position of the reaction chamber 3 can be adjusted by manually pushing the reaction chamber 3, and the purpose of automatically adjusting the position of the reaction chamber 3 can be achieved by arranging a corresponding driving motor or driving an air cylinder.
In the apparatus for preparing a nano-film provided in this embodiment, as shown in fig. 5 and 6, the vacuum device of this embodiment includes a vacuum measuring instrument 14, CvAn adjustable flapper valve 15 and a vacuum pump 16, the outlet of the reaction chamber 3 being in communication with the vacuum pump 16, CvAn adjustable flapper valve 15 is installed between the vacuum pump 16 and the reaction chamber 3, CvAn adjustable flapper valve 15 is used to adjust the pressure of the reaction chamber 3 and the vacuum measuring instrument 14 is used to measure the pressure of the reaction chamber 3. Wherein the vacuum measuring instrument 14, CvThe adjustable flapper valve 15 and the vacuum pump 16 are prior art in their own right.
Specifically, the outlet of the reaction chamber 3 is connected with a vacuum pump 16, and a C is connected between the vacuum pump 16 and the reaction chamber 3vAn adjustable flapper valve 15 and a vacuum measuring instrument 14, the pressure of the reaction chamber 3 can be adjusted by adjusting the carrier gas flow and the C of the flapper valvevThe values are adjusted to form different deposited film crystallinity and other quality parameters.
Although the present invention has been described with reference to the above preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the utility model as defined by the appended claims.
Claims (10)
1. A nanometer film preparation equipment is characterized in that: the device comprises a rack, and a pulse reaction source device, a reaction chamber and a vacuum device which are all arranged on the rack, wherein an outlet of the pulse reaction source device is communicated with the reaction chamber, and the vacuum device is used for keeping the vacuum state in the reaction chamber;
the device comprises a reaction chamber, a pulse reaction source device and a control device, wherein a continuous reaction source device is arranged at an inlet of the reaction chamber and is used for introducing a first continuous gas-phase reaction source into the reaction chamber, a substrate is placed in the reaction chamber, the pulse reaction source device comprises a plurality of reaction source bottles, a second reaction source is arranged in each reaction source bottle, and the reaction source bottles are used for alternately introducing a pulse-type second reaction source into the reaction chamber;
the periphery of the reaction chamber is provided with a reaction heating device which is used for heating the reaction chamber, so that the pulse type second reaction source in the reaction chamber reacts with the first reaction source and forms a nano film on the substrate.
2. The nano-film manufacturing apparatus according to claim 1, wherein: the continuous reaction source device comprises a solid first reaction source, a reaction pipeline for placing the solid first reaction source and a first heater arranged on the periphery of the reaction pipeline, the first heater is used for heating the reaction pipeline to enable the fixed first reaction source to be vaporized, the reaction pipeline is communicated with the pulse reaction source device and the reaction chamber, an outlet of the reaction pipeline is hermetically connected with an inlet of the reaction chamber, and an inlet of the reaction pipeline is hermetically connected with an outlet of the pulse reaction source device.
3. The nano-film manufacturing apparatus according to claim 1, wherein: the pulse reaction source device also comprises a pulse transmission component, the pulse transmission component comprises a second heater and a transmission pipeline arranged on the second heater, an outlet of the transmission pipeline is communicated with the reaction chamber, and an inlet of the reaction chamber is hermetically sleeved on the transmission pipeline; the pulse type second reaction source generated by the reaction source bottle is introduced into the transmission pipeline after passing through the second heater, the transmission pipeline introduces the second reaction source into the reaction chamber, and the second heater is used for heating the generated second reaction source.
4. The apparatus for preparing nano thin film according to claim 3, wherein: and the periphery of the conveying pipeline is provided with a third heater, and the third heater is used for heating the conveying pipeline.
5. The nano-film manufacturing apparatus according to claim 1, wherein: the outlets of the reaction source bottles reach the inlet of the reaction chamber at equal distances.
6. The nano-film manufacturing apparatus according to claim 1, wherein: the frame is also provided with a position adjusting device for adjusting the position of the reaction chamber.
7. The nano-film manufacturing apparatus according to claim 6, wherein: the position adjusting device comprises a slide rail arranged on the frame and a slide block connected with the slide rail in a sliding manner, and the reaction chamber is detachably connected with the slide block.
8. The nano-film manufacturing apparatus according to claim 1, wherein: the vacuum device comprises a vacuum measuring instrument and a vacuum measuring device CvAn adjustable flapper valve and a vacuum pump, the outlet of the reaction chamber being in communication with the vacuum pump, CvAn adjustable flapper valve installed between the vacuum pump and the reaction chamber, CvAn adjustable flapper valve is used to adjust the pressure of the reaction chamber, and the vacuum measurement instrument is used to measure the pressure of the reaction chamber.
9. The nano-film manufacturing apparatus according to claim 1, wherein: the reaction chamber is a quartz tube.
10. The nano-film manufacturing apparatus according to claim 2, wherein: the reaction chamber and the reaction pipeline are integrally arranged.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122640181.2U CN216337944U (en) | 2021-10-29 | 2021-10-29 | Nano film preparation equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122640181.2U CN216337944U (en) | 2021-10-29 | 2021-10-29 | Nano film preparation equipment |
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| CN216337944U true CN216337944U (en) | 2022-04-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202122640181.2U Active CN216337944U (en) | 2021-10-29 | 2021-10-29 | Nano film preparation equipment |
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| CN (1) | CN216337944U (en) |
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- 2021-10-29 CN CN202122640181.2U patent/CN216337944U/en active Active
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