CN111304623B - Ultrahigh vacuum sample introduction and sample treatment dual-purpose system and method - Google Patents

Ultrahigh vacuum sample introduction and sample treatment dual-purpose system and method Download PDF

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CN111304623B
CN111304623B CN202010113772.1A CN202010113772A CN111304623B CN 111304623 B CN111304623 B CN 111304623B CN 202010113772 A CN202010113772 A CN 202010113772A CN 111304623 B CN111304623 B CN 111304623B
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substrate
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main cavity
pipe
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CN111304623A (en
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潘毅
吴迪
袁玺惠
闵泰
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Xian Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/568Transferring the substrates through a series of coating stations
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/46Sputtering by ion beam produced by an external ion source
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/52Means for observation of the coating process
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5806Thermal treatment
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/2005Preparation of powder samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20058Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method

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Abstract

The invention discloses an ultrahigh vacuum sample introduction and treatment dual-purpose system and a treatment method, which mainly comprise a main cavity, a sample storage and heating table, a corrugated pipe type linear importer, an observation window, a hand valve, a hot cathode ion gauge, an ion sputtering source, a side angle extraction valve, a gas washing angle valve and a support frame. The main cavity body is provided with a plurality of ultrahigh vacuum tight sealing flange openings which are sequentially connected with a corrugated pipe type linear importer, an observation window, a hand valve, a hot cathode ion gauge, an ion sputtering source, a vacuum air exhaust system and a gas washing system, and a support frame is arranged below the main cavity body. The system can integrate two functions of multi-sample introduction and substrate treatment by using one cavity on the premise of ensuring that the ultra-high vacuum standard is achieved, wherein the substrate treatment mainly adopts a method of inert gas ion sputtering bombardment and annealing, and a film sample with high cleanliness and excellent performance is obtained.

Description

Ultrahigh vacuum sample introduction and sample treatment dual-purpose system and method
Technical Field
The invention relates to the field of ultrahigh vacuum coating, in particular to an ultrahigh vacuum sample introduction and sample treatment dual-purpose system and a treatment method.
Background
The ultrahigh vacuum coating technology refers to the ultrahigh vacuum environment (the pressure is less than 10)-8Pa) and selecting proper base, utilizing physical or chemical means to grow specific film on the surface of the substrate. The technology is widely applied to industries such as microelectronics, semiconductors and the like and scientific research works. The ultrahigh vacuum coating technology mainly comprises the categories of molecular beam epitaxy, laser sputtering deposition and the like. Generally, the preparation process of the ultra-high vacuum thin film sample comprises the following steps: substrate sample introduction, substrate processing, film growth and analysis and characterization. The corresponding ultrahigh vacuum coating equipment comprises a sample introduction cavity, a substrate processing cavity, a coating cavity and an analysis characterization cavity.
To save cost and space and reduce the complexity of the system, it is often necessary to integrate the four chambers. At present, the main mode is to integrate a film growth cavity and a substrate processing cavity into one cavity, namely to carry out pretreatment on a substrate in the ultrahigh vacuum coating cavity. Obviously, the disadvantage of this method is that some impurities inevitably generated during the pretreatment process are adsorbed on the inner wall of the chamber, the sample holder and the evaporation source, and further affect the cleanliness and performance of the sample.
On the other hand, most of the sample injection cavities of the existing ultrahigh vacuum coating equipment are sealed by fluororubber, so that the ultimate vacuum is poor and is about 5 multiplied by 10-6Pa. In the process of transferring the sample with the subsequent cavity, the vacuum degree of the subsequent cavity can be reduced, and pollution is caused. Ideally, in order to obtain a film sample with high cleanliness and excellent performance, each cavity should be kept in a good vacuum degree.
Disclosure of Invention
Aiming at the technical problems of the existing ultrahigh vacuum coating system, the invention mainly provides an ultrahigh vacuum sample introduction and substrate sample treatment dual-purpose system and a treatment method. On the premise of ensuring that the ultrahigh vacuum standard is achieved, the device integrates two functions of sample introduction and substrate sample treatment by using a cavity, wherein the substrate sample treatment mainly adopts a method of inert gas ion sputtering bombardment and annealing.
The invention is realized by the following technical scheme.
An ultrahigh vacuum sample introduction and sample treatment dual-purpose system comprises a main cavity with a T-shaped tube structure; the top wall above the main cavity is respectively and vertically communicated with a corrugated pipe type linear importer and a sample storage and heating table, the lower part of a T-shaped pipe branch pipe of the main cavity is communicated with a side angle extraction valve, and the lower part of a T-shaped pipe main pipe of the main cavity is respectively communicated with an extension pipe and a gas washing angle valve which are distributed in parallel with the T-shaped pipe branch pipe; the front side wall and the rear side wall of the main pipe of the T-shaped pipe of the main cavity are respectively communicated with a hand valve, a second glass observation window and a hot cathode ion gauge, and the rear wall of the main pipe of the T-shaped pipe of the main cavity is provided with a sputtering ion source;
sample ion sputtering bombardment and annealing treatment are realized through a sample storage and heating table, a corrugated pipe type linear introducer and a sputtering ion source;
sample transmission is realized through a hand valve, a corrugated pipe type linear introducer and an extension pipe;
the vacuum degree of 10 is realized by a side angle extraction valve and a hot cathode ion gauge-8Of the order of Pa.
In the system, a main pipe and a branch pipe of a T-shaped pipe of the main cavity are communicated cylindrical cavities, and are formed by welding vacuum pipelines, the main pipe is horizontally arranged, and 9 vacuum flanges capable of being in vacuum connection with other devices are arranged on the side surface of the main pipe of the main cavity; the main cavity is fixed above the support frame.
In the system, the sample storage and heating table comprises a sample rack for fixing a sample substrate, a sample storage rack and a heating table, wherein the sample storage rack extends into the bellows type linear importer, and the heating table is connected to the sample storage rack and is vertical to the horizontal axis of the main cavity body.
In the system, the top wall and the side wall of the main cavity body main pipe are respectively communicated with a first glass observation window and a second glass observation window.
In the system, the lower end of a side pumping angle valve connected below a T-shaped pipe branch pipe of a main cavity body is connected with a side pumping system.
Correspondingly, the invention also provides a processing method of the ultrahigh vacuum sample introduction and sample processing dual-purpose system, which comprises the following steps of sample introduction, sample processing and ultrahigh vacuum film plating:
1) during sample introduction, the hand valve is closed, the extension pipe is disassembled, the bellows type linear importer is shortened to the minimum stroke, the sample storage rack and the heating platform are exposed out of the flange at the bottom of the main cavity body, and the sample rack provided with the substrate is arranged in the sample storage rack or fixed on the heating platform;
extending the bellows type linear importer to enable the sample storage and heating table to be completely returned to the main cavity, reconnecting the extension tube with the main cavity, and exhausting air after sealing to achieve an ultrahigh vacuum condition;
2) when a sample is processed, the stroke of the bellows type linear introducer is adjusted, so that the center of a sample rack on the heating table is positioned on a horizontal axis of the sputtering ion source;
the method is characterized in that two processing means of ion sputtering bombardment and annealing on a substrate are combined for use: sputtering and annealing treatment are carried out on the metal substrate, and annealing treatment is carried out on the insulator and the semiconductor substrate to obtain a clean and flat substrate;
3) during ultrahigh vacuum coating, regulating and controlling the position of a sample shelf in a sample storage and heating table, opening a hand valve, communicating a system and a film growth cavity, and transferring the annealed substrate to the film growth cavity in situ for ultrahigh vacuum coating to obtain a sample;
4) judging whether the growth of the sample film meets the requirements, if not, returning to the step 2) -3) to carry out sample treatment and ultrahigh vacuum coating until the requirements are met.
In the method, during sample treatment, the substrate ions are sputtered and bombarded by communicating a sputtering ion source power supply, filling argon gas and controlling the pressure of a cavity to be maintained at 10-4Pa, the temperature is maintained at normal temperature, the beam energy is not more than 3000eV, and the generated ion beam bombards the surface of the sample under the drive of a high-voltage electric field to achieve the cleanness and the flatness of the substrate.
In the method, when a sample is processed, the substrate on the sample rack is heated and annealed, the heating temperature is 200-1500 ℃, the annealing time is determined according to the sample material and the processing requirement, and the clean and flat substrate is obtained.
In the method, if the film growth of the sample is not ideal, the sample can be transferred into the system by the sample transfer rod, the undesired film is knocked off by the sputtering ion source, and the repeatedly processed substrate is put into the film growth cavity again for growth after ion sputtering bombardment and annealing treatment.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. the invention adopts the T-shaped cavity sealed by the vacuum flange, realizes two procedures of sample injection and substrate sample treatment in one cavity under the ultrahigh vacuum standard, can obtain a film sample with high cleanliness and excellent performance under the condition of ensuring that each cavity is in a good vacuum degree, and avoids pollution caused in the process of transferring the sample by the cavity.
2. The invention can load a plurality of samples simultaneously by opening the cavity each time by utilizing the sample storage and heating table, thereby reducing the times of opening the cavity and the pollution degree to the subsequent cavity.
3. The invention adopts the heating table and the sputtering ion source, realizes the ion sputtering bombardment and the vacuum annealing treatment on the substrate, and is suitable for most of metal, oxide and semiconductor substrates.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is an overall perspective view of the dual-purpose system for ultra-high vacuum sample injection and substrate processing of the present invention;
FIG. 2 is a perspective view of a main chamber of the dual-purpose system for ultra-high vacuum sample injection and substrate processing of the present invention;
FIG. 3 is a partial perspective view of the dual-purpose system for ultra-high vacuum sample introduction and substrate processing of the present invention;
FIG. 4 is a partial cross-sectional view of the dual-purpose system for ultra-high vacuum sample introduction and substrate processing of the present invention.
Reference numerals:
1-sample storage and heating station; 2-bellows type linear importer; 3-hand valve; 4-hot cathode ion gauge; 5-a main cavity; 6, extending a pipe; 7, a support frame; 8-purge angle valve; 9-side angle-drawing valve; 10-a sputtering ion source; 11-a first glass viewing window; 12-a second glass viewing window; 31-sample holder; 32-a sample storage rack; 33- -heating station.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
Referring to fig. 1, the dual-purpose system for ultra-high vacuum sample introduction and sample treatment comprises a main cavity 5, a sample storage and heating table 1, a bellows type linear importer 2, glass observation windows 11 and 12, a hand valve 3, a hot cathode ion gauge 4, a sputtering ion source 10, a side extraction angle valve 9, a gas washing angle valve 8 and a support frame 7. Wherein, each component of the dual-purpose system for ultra-high vacuum sample introduction and substrate treatment comprises a T-shaped main cavity body 5, the top wall above the main cavity body 5 is respectively and vertically communicated with a corrugated pipe type linear importer 2 (the total travel is about 150mm) and a first glass observation window 12 which is obliquely communicated, and a sample storage and heating platform 1 is connected above the corresponding corrugated pipe type linear importer 2; a side angle-drawing valve 9 (connected with a side angle-drawing system) is communicated below the T-shaped pipe branch pipe of the main cavity 5, and an extension pipe 6 and a washing angle valve 8 which are distributed in parallel with the T-shaped pipe branch pipe are respectively communicated below the T-shaped pipe main pipe of the main cavity 5; the front side wall and the rear side wall of the main pipe of the T-shaped pipe of the main cavity 5 are respectively communicated with a hand valve 3, a second glass observation window 12 and a hot cathode ion gauge 4, and the rear wall of the main pipe of the T-shaped pipe of the main cavity 5 is provided with a sputtering ion source 10.
The lower end of a side pumping angle valve 9 connected below the T-shaped pipe branch pipe of the main cavity 5 is connected with a side pumping system.
Fig. 2 is a perspective view of a main cavity of the dual-purpose system for ultra-high vacuum sample injection and substrate processing of the present invention, and as shown in fig. 2, the main cavity 5 belongs to a cylindrical cavity, and is formed by welding vacuum pipelines, the diameter of the main cavity is determined by a flange with the specification of CF35, the main cavity is about 7cm, the length of the main cavity is about 30cm, the weight of the main cavity is about 3.5kg, and 9 vacuum flanges capable of vacuum sealing connection with other devices are arranged on the side surface of the main cavity. The main chamber 5 is fixed above the support frame 7.
The sample heating and annealing functions of the present invention are realized by the sample storage and heating stage 1 and the bellows-type linear introducer 2.
The sample ion sputtering bombardment treatment function of the invention is realized by the sample storage and heating table 1, the bellows type linear introducer 2 and the sputtering ion source 10.
The sample transfer function of the present invention is achieved by a hand valve 3, a bellows-type linear introducer 2 and an extension tube 6.
The observation of the sample substrate of the present invention is achieved by the combination of the first glass observation window 11 and the second glass observation window 12. The two glass observation windows are respectively arranged at the top and the side of the main cavity 5, so that an operator can observe from different angles, and the processing process of the sample substrate and the in-situ transfer process of the ultrahigh vacuum coating system are ensured to be carried out smoothly.
The vacuum condition of the invention is realized by the side angle-drawing valve 9 and the hot cathode ion gauge 4, so that the invention has the vacuum degree of 10 in the operation process-8Of the order of Pa.
The components ensure that the sample substrate can be transferred in situ under ultrahigh vacuum, and the core functions of ion sputtering bombardment and annealing treatment are performed.
The following describes the specific operation flow of the dual-purpose system for ultra-high vacuum sample injection and substrate processing according to the present invention with reference to fig. 3 and 4.
Referring to fig. 3, the present invention is a partial perspective view of the dual-purpose system of ultra-high vacuum sample injection and substrate processing. The sample storage and heating table 1 mainly includes a sample rack 31 for fixing sample substrates, a sample storage rack 32 (capable of storing 3 sample racks 31), and a heating table 33. The sample storage and heating table 1 is vertically arranged, the total length is 43cm, the diameter is determined by a flange CF35 and is about 7cm, and the plane of the heating table 33 is vertical to the horizontal axis of the main cavity body 5; and controls the transmission of the sample frame 31 by means of the bellows type linear introducer 2 and a sample transmission rod (not shown) in the film growth cavity so as to realize the functions of heating annealing, sample introduction and storage of the sample substrate.
When sample introduction is needed, the hand valve 3 is kept closed, the extension pipe 6 on the side wall below the main cavity body 5 is detached, the bellows type linear importer 2 is shortened to the minimum stroke, the sample storage rack 32 and the heating platform 33 are exposed out of the bottom flange of the main cavity body 5, and the prepared sample rack 31 provided with the substrate is arranged in the sample storage rack 32 or fixed on the heating platform 33; and then extending the corrugated pipe type linear introducer 2 to enable the sample storage and heating table 1 to completely return to the main cavity 5, reconnecting the extension pipe 6 to the main cavity 5, and sealing and then exhausting the ultrahigh vacuum sample introduction and substrate treatment dual-purpose system to achieve an ultrahigh vacuum condition.
Referring to fig. 4, the present invention is a partial cross-sectional view of a dual-purpose system for ultra-high vacuum sample injection and substrate processing. When the sample is processed, the stroke of the bellows type linear introducer 2 is adjusted to assist the observation through the first glass observation window 11 and the second glass observation window 12, so that the center of the sample holder 31 on the heating stage 33 is positioned on the horizontal axis of the sputtering ion source 10. The power supply of the sputtering ion source 10 is communicated, the beam energy and the filament current of the sputtering ion source 10 are adjusted, the leakage valve is opened, argon is filled, and the pressure of the cavity is maintained at 10- 4Pa, temperature is maintained at normal temperature, and beam energy is controlledThe quantity (maximum 3000eV) is that the generated ion beam flows through the driving of a high-voltage electric field to bombard the surface of the substrate, and the substrate is subjected to ion sputtering bombardment so as to achieve the aim of cleaning and flattening the sample substrate (substrate). Meanwhile, the sample holder 31 can be heated and annealed on the sample heating stage 33, and the atoms on the surface of the substrate after ion sputtering bombardment are uniformly distributed with energy, so that the substrate is flat. A clean and flat substrate can be obtained by the combined use of two processing means of substrate ion sputtering bombardment and annealing (when the substrate is made of metal, sputtering and annealing treatment are carried out on the metal substrate, and when the substrate is made of insulator and semiconductor, annealing treatment is carried out on the insulator and the semiconductor substrate). And then judging whether the growth of the sample film meets the requirements, if not, returning to the previous step for sample treatment and high vacuum coating until the requirements are met.
After the sample substrate is pretreated by the ultrahigh vacuum sample introduction and substrate treatment dual-purpose system, the position of the sample rack 31 in the sample storage and heating table 1 can be regulated and controlled by a rapid sample transfer rod in the ultrahigh vacuum coating system, and the sample rack 31 can be placed into the sample storage rack 32 for storage; meanwhile, the hand valve 3 can be opened to communicate the ultrahigh vacuum sample introduction and substrate processing dual-purpose system and a film growth cavity (not shown in the figure), and the annealed sample substrate is transferred to the film growth cavity in situ to carry out ultrahigh vacuum coating to obtain a sample.
Particularly, after the film coating of the film growth cavity of the substrate is finished, a Reflection High Energy Electron Diffraction (RHEED) system is adopted to detect a sample in the film growth cavity, whether the sample meets the growth requirement is detected, if the sample does not grow satisfactorily, the sample can be transferred into an ultrahigh vacuum sample introduction and substrate treatment dual-purpose system by means of a sample transfer rod, after the unsatisfactory film is knocked off by means of a sputtering ion source 10, the substrate subjected to repeated treatment is subjected to ion sputtering bombardment again and annealing treatment, and then is placed into the film growth cavity again for growth. Finally, the prepared sample may be placed in a sample holder 32.
The operations above complete the sample injection of the dual-purpose system of ultrahigh vacuum sample injection and substrate treatment, and realize the ion sputtering bombardment and annealing treatment of the sample substrate to obtain a clean and flat sample substrate, and the sample before ultrahigh vacuum coating is subjected to two-step pretreatment of sample injection and substrate treatment, so that the sample requirement of ultrahigh vacuum coating in the film growth cavity is met, and the phenomena of reduced vacuum degree and pollution of the subsequent cavity due to the adsorption of impurities on the inner wall of the cavity, the sample storage rack and the evaporation source are avoided.
In conclusion, the invention designs a small-sized ultrahigh vacuum system with dual purposes of sample introduction and substrate treatment, and combines the sample transfer rod of the film growth cavity, so that the requirements of ion sputtering bombardment and annealing treatment on the sample substrate under the ultrahigh vacuum environment condition can be met on the basis of realizing the core function of in-situ transfer and storage of the sample under the ultrahigh vacuum condition.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.

Claims (9)

1. An ultrahigh vacuum sample introduction and sample treatment dual-purpose system is characterized by comprising a main cavity (5) with a T-shaped tube structure; a corrugated pipe type linear gatherer (2) and a sample storage and heating table (1) are respectively and vertically communicated with the top wall above the main cavity body (5), a side angle drawing valve (9) is communicated below a T-shaped pipe branch pipe of the main cavity body (5), and an extension pipe (6) and a gas washing angle valve (8) which are distributed in parallel with the T-shaped pipe branch pipe are respectively communicated below a T-shaped pipe main pipe of the main cavity body (5); the front side wall and the rear side wall of the main T-shaped pipe of the main cavity (5) are respectively communicated with a hand valve (3), a second glass observation window (12) and a hot cathode ion gauge (4), and the rear wall of the main T-shaped pipe of the main cavity (5) is provided with a sputtering ion source (10);
sample ion sputtering bombardment and annealing treatment are realized through a sample storage and heating table (1), a corrugated pipe type linear introducer (2) and a sputtering ion source (10);
sample transmission is realized through a hand valve (3), a corrugated pipe type linear introducer (2) and an extension pipe (6);
the vacuum degree is realized to reach 10 through a side angle extraction valve (9) and a hot cathode ion gauge (4)-8Of the order of Pa.
2. The dual-purpose system for ultra-high vacuum sample introduction and sample treatment as claimed in claim 1, wherein the main pipe and the branch pipe of the T-shaped pipe of the main cavity (5) are communicated cylindrical cavities, and are formed by welding vacuum pipelines, the main pipe is horizontally placed, and the side surface of the main pipe of the main cavity (5) is provided with 9 vacuum flanges capable of vacuum sealing connection with other devices; the main cavity (5) is fixed above the support frame (7).
3. The dual-purpose system for ultra-high vacuum sample introduction and sample treatment as claimed in claim 1, wherein the sample storage and heating stage (1) comprises a sample holder (31) for fixing the substrate sample, a sample storage holder (32) and a heating stage (33), the sample storage holder (32) extends into the bellows type linear introducer (2), and the heating stage (33) is connected to the sample storage holder (32) and is perpendicular to the horizontal axis of the main pipe of the main cavity (5).
4. The dual-purpose system for ultra-high vacuum sample introduction and sample treatment as claimed in claim 1, wherein the top wall and the side wall of the main tube of the main chamber (5) are respectively communicated with a first glass observation window (11) and a second glass observation window (12).
5. The dual-purpose system for ultra-high vacuum sample introduction and sample treatment as claimed in claim 1, wherein the lower end of the side-pumping angle valve (9) connected below the T-shaped pipe branch of the main chamber (5) is connected with a side-pumping system.
6. The processing method of the dual-purpose system for ultra-high vacuum sample introduction and sample processing as claimed in any one of claims 1 to 5, characterized by comprising the following steps of sample introduction and sample processing:
1) during sample introduction, the hand valve (3) is closed, the extension pipe (6) is detached, the bellows type linear introducer (2) is shortened to the minimum stroke, the sample storage rack (32) and the heating platform (33) are exposed out of the flange at the bottom of the main cavity body (5), and the sample rack (31) provided with the substrate is arranged in the sample storage rack (32) or fixed on the heating platform (33);
extending the bellows type linear introducer (2), enabling the sample storage and heating table (1) to completely return to the main cavity body (5), reconnecting the extension tube (6) with the main cavity body (5), and performing air suction after sealing to achieve an ultrahigh vacuum condition;
2) when a sample is processed, the stroke of the bellows type linear introducer (2) is adjusted, so that the center of a sample rack (31) on a heating table (33) is positioned on the horizontal axis of a sputtering ion source (10);
the method is characterized in that two processing means of ion sputtering bombardment and annealing on a substrate are combined for use: sputtering and annealing treatment are carried out on the metal substrate, and annealing treatment is carried out on the insulator and the semiconductor substrate to obtain a clean and flat substrate;
3) during ultrahigh vacuum coating, regulating and controlling the position of a sample shelf (31) in a sample storage and heating table (1), opening a hand valve (3), communicating a system and a film growth cavity, and transferring the annealed substrate to the film growth cavity in situ for ultrahigh vacuum coating to obtain a sample;
4) judging whether the growth of the sample film meets the requirements, if not, returning to the step 2) -3) to carry out sample treatment and ultrahigh vacuum coating until the requirements are met.
7. The processing method of the dual-purpose system for ultra-high vacuum sample injection and sample processing as claimed in claim 6, wherein during sample processing, the substrate ion sputtering bombardment is performed by connecting a power supply of a sputtering ion source (10), charging argon gas, and controlling the pressure of the chamber to be maintained at 10-4Pa, the temperature is maintained at normal temperature, the beam energy is not more than 3000eV, and the generated ion beam bombards the surface of the sample under the drive of a high-voltage electric field to achieve the cleanness and the flatness of the substrate.
8. The processing method of the dual-purpose system for ultra-high vacuum sample injection and sample processing as claimed in claim 6, wherein during sample processing, the substrate on the sample holder (31) is heated and annealed at a temperature of 200-1500 ℃ to obtain a clean and flat substrate.
9. The processing method of the system for sampling and processing the sample in ultrahigh vacuum as claimed in claim 6, wherein if the film growth of the sample is not ideal, the sample is transferred into the system by a sample transfer rod, the undesired film is removed by a sputtering ion source (10), and the substrate after repeated processing is again subjected to ion sputtering bombardment and annealing treatment and then is placed into the film growth chamber again for growth.
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