CN110965041B - Insertable gas-phase cluster soft deposition method - Google Patents

Insertable gas-phase cluster soft deposition method Download PDF

Info

Publication number
CN110965041B
CN110965041B CN201911273496.9A CN201911273496A CN110965041B CN 110965041 B CN110965041 B CN 110965041B CN 201911273496 A CN201911273496 A CN 201911273496A CN 110965041 B CN110965041 B CN 110965041B
Authority
CN
China
Prior art keywords
gas
sample
cavity
soft deposition
soft
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201911273496.9A
Other languages
Chinese (zh)
Other versions
CN110965041A (en
Inventor
骆智训
黄奔奔
杨梦周
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Chemistry CAS
Original Assignee
Institute of Chemistry CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Chemistry CAS filed Critical Institute of Chemistry CAS
Priority to CN201911273496.9A priority Critical patent/CN110965041B/en
Publication of CN110965041A publication Critical patent/CN110965041A/en
Application granted granted Critical
Publication of CN110965041B publication Critical patent/CN110965041B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
    • C23C16/463—Cooling of the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/54—Apparatus specially adapted for continuous coating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention relates to an insertable gas cluster soft deposition device and a method, comprising the following steps: the vacuum module and the gas distribution module are communicated with the sample cavity; a mass spectrometer is arranged in the soft deposition cavity and used for carrying out mass spectrometry on the gas-phase clusters; the sample cavity and the soft deposition cavity are divided or communicated through a gate valve arranged at the joint of the sample cavity and the soft deposition cavity, a sample table capable of reciprocating is arranged in the sample cavity, and a deposition substrate is arranged on the sample table; the vacuum module vacuumizes the soft deposition cavity and the sample cavity; and the gas distribution module is used for introducing inert gas into the vacuumized soft deposition cavity and the sample cavity. The device combines the mass spectrometry device of the gas phase cluster with the soft deposition experimental device, can conveniently use the soft deposition function in the mass spectrometry experimental process, and monitors the deposition amount of the gas phase cluster in real time in the soft deposition process, thereby ensuring that the deposited gas phase cluster can be sufficiently used for subsequent experiments.

Description

Insertable gas-phase cluster soft deposition method
Technical Field
The invention relates to an insertable gas-phase cluster soft deposition method, belonging to the technical field of cluster preparation and detection.
Background
Clusters are relatively stable microscopic or submicroscopic aggregates consisting of several or even thousands of atoms, molecules or ions bound by physical or chemical bonds, the physical and chemical properties of which vary with the number of atoms contained. The clustering is widely existed in the natural world and in practical activities of human beings, and involves many substance movement processes and phenomena, such as catalysis, combustion, crystal growth, nucleation and solidification, phase change, sol, film formation and sputtering, etc., so the research aiming at the clustering is the research hotspot in the material science at present.
The characterization means of the cluster comprises a far infrared multi-photon dissociation spectrum, a photoelectron spectrum, a trapped cluster electron diffraction spectrum and the like, and information such as the structure, energy, track and the like of the cluster can be obtained through the characterization means. However, the above characterization means cannot perform direct morphological research and performance characterization on the gas-phase clusters. Therefore, the obtained gas-phase cluster needs to be subjected to soft deposition operation, but the traditional soft deposition device has the defects of complex structure, complex operation and simple function, and the accurate quality of the gas-phase cluster is difficult to accurately obtain before deposition. In addition, how to couple a convenient low-temperature substrate isolation system on a soft deposition system is also a key technical difficulty at present.
Disclosure of Invention
In view of the above problems, the present invention provides an insertable vapor cluster soft deposition method, which integrates a soft deposition system and a mass spectrometer detection system to obtain a vacuum environment of a soft deposition chamber and realize a low temperature substrate isolation function.
In order to achieve the purpose, the invention adopts the following technical scheme: the invention provides an insertable gas cluster soft deposition device, which comprises: the vacuum module and the gas distribution module are communicated with the sample cavity; a mass spectrometer is arranged in the soft deposition cavity and used for carrying out mass spectrometry on the gas-phase clusters; the sample cavity and the soft deposition cavity are divided or communicated through a gate valve arranged at the joint of the sample cavity and the soft deposition cavity, a sample table capable of reciprocating is arranged in the sample cavity, and a deposition substrate is arranged on the sample table; the vacuum module vacuumizes the soft deposition cavity and the sample cavity when the gate valve is opened; and the gas distribution module is used for introducing inert gas into the vacuumized soft deposition cavity and the sample cavity.
Further, the mass spectrometer comprises a quadrupole mass analyzer and an electron multiplier which are arranged at the same height, and a space region between the quadrupole mass analyzer and the electron multiplier and at the same height with the quadrupole mass analyzer and the electron multiplier is a detection region.
Further, the sample platform connects gradually sample telescopic link and driver, and the length of sample telescopic link is controlled to the driver to drive sample platform reciprocating motion.
Furthermore, a graduated scale is arranged on one side of the sample telescopic rod or the sample telescopic rod; all be equipped with the observation window on the lateral wall in soft deposit chamber and the lateral wall in sample chamber, ensure through scale and observation window that the sample platform is in the detection area of mass spectrograph.
Further, a cooler is arranged on the sample stage and is used for cooling the sample stage by utilizing liquid nitrogen or a low-temperature cooling stage.
Furthermore, the inert gas introduced into the gas distribution module is SF6Matrix gas for forming fluorinated monolayer film substrate with the deposition substrate, vacuum gauges arranged on the soft deposition chamber and the sample chamber, and SF controlled by observing vacuum gauge readings of the soft deposition chamber and the sample chamber6The flow rate of the matrix gas.
Further, the gas distribution module comprises original SF6Gas delivery pipe, dilution gas delivery pipe, gas mixing chamber and SF6A substrate gas delivery tube; gas mixing chamber is respectively connected with original SF6The gas delivery pipe, the dilution gas delivery pipe are communicated with each other, and the original SF6The gas and the diluent gas are mixed in the gas mixing chamber to form SF with preset content6A matrix gas, and passing SF6Transporting SF by substrate gas6Matrix gas is passed into the sample chamber.
Furthermore, the soft deposition cavity comprises an ion lens group, and the kinetic energy of the gas-phase cluster ions charged into the soft deposition cavity is adjusted by applying different direct-current voltages to each ion lens in the ion lens group.
The invention also discloses an insertable gas cluster soft deposition method, which adopts any one of the insertable gas cluster soft deposition devices to carry out soft deposition of the gas clusters; the gas phase cluster soft deposition method comprises the following steps: s1, opening the gate valve, vacuumizing the soft deposition cavity and the sample cavity to a preset vacuum degree, and closing the gate valve; s2, filling the soft deposition cavity with the gas-phase clusters, and performing mass spectrometry on the gas-phase clusters; s3, opening the gate valve, extending the sample telescopic rod, and placing the sample table into the soft deposition cavity; s4 filling SF into the sample cavity6A matrix gas forming a fluorinated monolayer film substrate; s5 carrying out gas phase cluster soft deposition, after the gas phase cluster soft deposition is finished, shortening the sample telescopic rod, closing the gate valve, closing the vacuum module and the gas distribution module, opening the observation window, taking out the sampleAnd (5) preparing the product.
Further, in the step S5, when performing the soft deposition of the gas cluster, the mass spectrometer performs mass spectrometry on the gas cluster in real time, calculates the flux of the gas cluster according to the mass spectrum peak intensity obtained by the mass spectrometry, and determines the soft deposition time so that the obtained sample amount meets the requirement of the subsequent detection.
Due to the adoption of the technical scheme, the invention has the following advantages: 1. the mass spectrum experimental device of the gas phase cluster is combined with the soft deposition experimental device, the soft deposition function can be conveniently used in the mass spectrum experimental process, the deposition amount of the gas phase cluster is monitored in real time in the soft deposition process, the deposited gas phase cluster is ensured to be sufficient for subsequent experiments, and the problem that repeated experiments are needed due to insufficient deposition amount is avoided. 2. The mass range of the deposited clusters can be determined or a selective soft deposition can be performed. 3. High vacuum can be achieved by coupled vacuum pre-pumping and matrix gas distribution systems, or by injecting formulated SF6The matrix gas is used as a monolayer film substrate to realize low-temperature matrix isolation, and the cluster soft deposition efficiency and the sample quality are improved. 4. The glass observation window can observe the descending position of the soft deposition rod and can conveniently sample after the test is realized.
Drawings
FIG. 1 is a front view of an insertable vapor cluster soft deposition apparatus according to an embodiment of the present invention;
FIG. 2 is a side view of an insertable vapor cluster soft deposition apparatus in accordance with an embodiment of the present invention;
FIG. 3 is a top view of an insertable vapor cluster soft deposition apparatus according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a vacuum module and a gas distribution module according to an embodiment of the present invention.
Reference numerals:
1-a soft deposition chamber; 2-a sample chamber; 3-a gate valve; 4-sample stage; 5-quadrupole mass analyser; 6-electron multiplier; 7-ion lens group; 8-sample telescoping rod; 9-a driver; 10-a bellows; 11-a graduated scale; 12-a viewing window; 13-a bellows; 14-a first shut-off valve; 15-a mechanical pump; 16-a molecular pump; 17-vacuumCounting; 18-a second stop valve; 19-original SF6A gas delivery pipe; 20-a dilution gas delivery pipe; 21-a gas mixing chamber; 22-SF6A substrate gas delivery tube.
Detailed Description
The present invention is described in detail below with reference to the attached drawings. It is to be understood, however, that the drawings are provided solely for the purposes of promoting an understanding of the invention and that they are not to be construed as limiting the invention. In describing the present invention, it is to be understood that the terminology is used for the purpose of description only and is not intended to be interpreted as indicating or implying any relative importance.
The present embodiment provides an insertable vapor cluster soft deposition apparatus, as shown in fig. 1 to 3, including: the device comprises a soft deposition cavity 1, a sample cavity 2, a vacuum module and a gas distribution module, wherein the soft deposition cavity 1 and the sample cavity 2 are sequentially connected, and the vacuum module and the gas distribution module are communicated with the sample cavity 2; a mass spectrometer is arranged in the soft deposition cavity 1 and used for carrying out mass spectrometry on the gas-phase clusters; the sample cavity 2 and the soft deposition cavity 1 are divided or communicated through a gate valve 3 arranged at the joint of the sample cavity and the soft deposition cavity, a sample table 4 capable of reciprocating is arranged in the sample cavity 2, and a deposition substrate is arranged on the sample table 4; when the gate valve 3 is opened, the vacuum module vacuumizes the soft deposition cavity 1 and the sample cavity 2; and the gas distribution module introduces inert gas into the vacuumized soft deposition cavity 1 and the vacuumized sample cavity 2. The device in the embodiment combines the mass spectrum experimental device of the gas cluster with the soft deposition experimental device, can conveniently use the soft deposition function in the mass spectrum experimental process, monitors the deposition amount of the gas cluster in real time in the soft deposition process, ensures that the deposited gas cluster can be sufficiently subjected to subsequent experiments, and avoids the problem that repeated experiments are needed due to insufficient deposition amount.
Wherein, the soft deposition chamber 1 comprises a mass spectrometer and an inlet for charging the gas-phase clusters. The mass spectrometer comprises a pair of quadrupole mass analyzer 5 and electron multiplier 6 arranged at the same height, and the space region between the quadrupole mass analyzer 5 and the electron multiplier 6 at the same height is the detection region. The charged gas-phase clusters enter the detection area of the mass spectrometer. And the mass spectrometer performs mass spectrometry on the gas phase clusters to generate corresponding spectrograms. An ion lens group 7 is further arranged at the inlet of the gas-phase cluster, and different direct-current voltages are applied to the ion lenses in the ion lens group 7 to adjust the kinetic energy of the gas-phase cluster ions filled in the soft deposition cavity 1, so that the gas-phase cluster ions meet the requirements of subsequent soft deposition experiments.
Including sample platform 4 in the sample chamber 2, sample platform 4 connects gradually sample telescopic link 8 and driver 9, and driver 9 controls sample telescopic link 8 flexible to decide the length of sample telescopic link 8, the length change through sample telescopic link 8 drives sample platform 4 reciprocating motion. The driver 9 may be manually driven, for example, a rotating disc may be used to rotate and adjust the length of the sample telescopic rod 8, or may be used to mechanically and automatically adjust the length of the telescopic rod. For example, a power device such as an electric motor and a hydraulic cylinder is adopted to drive the sample telescopic rod 8 to move up and down or left and right. The reciprocating motion here means a state in which it can be extended or shortened, and does not require the sample expansion link 8 to be extended or shortened at a certain frequency all the time. It should be noted that, in fig. 1 to 3, the sample expansion link 8 is vertically moved, the drawings are only exemplary, and the sample expansion link 8 may also horizontally reciprocate. In order to protect the sample telescopic rod 8 and avoid the damage of the sample telescopic rod, the sample telescopic rod 8 is also sleeved with a telescopic corrugated pipe 10 which can be extended or shortened along with the sample telescopic rod 8. In addition, in order to guarantee that the length of sample telescopic link 8 accords with the experimental requirement, guarantee that sample telescopic link 8 sends sample platform 4 into in the detection area promptly, so be equipped with scale 11 on 8 one side of sample telescopic link or the sample telescopic link 8. The scale 11 provided on the sample expansion link 8 side is a scale 11 that is fixed in length and cannot expand and contract, that is, a scale 11 that is fixed in length. The graduated scale 11 of setting on sample telescopic link 8 is the scale of carving on sample telescopic link 8, is about to sample telescopic link 8 extension or shorten to certain length, and this length value can be shown to this graduated scale 11. The side wall of the soft deposition chamber 1 and the side wall of the sample chamber 2 are both provided with an observation window 12, and the position of the sample stage 4 can be seen through the observation windows 12. The sample stage 4 is secured within the detection region of the mass spectrometer by the scale 11 and the viewing window 12. In addition, the observation window 12 can be used as a door for taking in a sample and taking out the sample after completion of the experiment.
In order to meet the requirement of soft deposition, the sample stage 4 is also provided with a cooler which utilizes liquid nitrogen or a low-temperature cooling stage to cool the sample stage 4.
The vacuum module comprises a bellows 13, one end of which bellows 13 communicates with the sample chamber 2 through a first shut-off valve 14 provided at a side wall of the sample chamber 2. The other end of the bellows 13 is connected to a mechanical pump 15 or a molecular pump 16. Firstly, the sample cavity 2 and the soft deposition cavity 1 are vacuumized by the mechanical pump 15, and then the sample cavity 2 and the soft deposition cavity 1 are vacuumized by the molecular pump 16, so that the vacuum degree of the sample cavity 2 and the soft deposition cavity 1 is ensured to be in a preset vacuum degree in the whole experiment process. Vacuum gauges 17 are arranged in the sample cavity 2 and the soft deposition cavity 1, and the vacuum gauges 17 monitor the vacuum degrees in the sample cavity 2 and the soft deposition cavity 1 in real time. Meanwhile, the vacuum gauge 17 can also monitor the amount of inert gas introduced into the gas distribution module in real time, so that the introduction amount of the inert gas can be adjusted at any time.
The gas distribution module communicates with the sample chamber 2 via a second shut-off valve 18 arranged above the sample chamber 2. The inert gas introduced in this example is SF6A matrix gas. SF here6The matrix gas is SF gas containing a predetermined amount6For distinguishing pure SF6Gas or originally introduced SF6Higher gas content. Introduction of SF6The matrix gas is used to form a fluorinated monolayer film with the deposition substrate. This is because the common deposition substrate can mechanically collide with the substrate when the vapor cluster is deposited, so that the morphology of the vapor cluster is changed. And the existence of the fluorinated monolayer film has a buffering effect on the cluster, so that the kinetic energy of the cluster is reduced, and the change of the morphology of the cluster caused by mechanical collision is avoided.
As shown in fig. 4, the distribution module specifically includes an original SF6 Gas delivery tube 19, diluent gas delivery tube 20, gas mixing chamber 21 and SF6A substrate gas transport pipe 22; the gas mixing chamber 21 is respectively connected with the original SF6A gas delivery pipe 19, a dilution gas delivery pipe 20, and raw SF6The gas and the diluent gas are mixed in the gas mixing chamber 21 to a predetermined amount of SF6A matrix gas, and passing SF6The substrate gas delivery tube 22 delivers SF6Matrix gas is passed into the sample chamber 2.
The invention also discloses an insertable gas cluster soft deposition method, which adopts any one of the insertable gas cluster soft deposition devices to perform gas cluster soft deposition; the gas phase cluster soft deposition method comprises the following steps: s1, opening the gate valve 3, vacuumizing the soft deposition cavity 1 and the sample cavity 2 to a preset vacuum degree, and closing the gate valve 3; s2, filling the gas-phase clusters into the soft deposition cavity 1, and carrying out mass spectrometry on the gas-phase clusters; s3, opening the gate valve 3, extending the sample telescopic rod 8, and placing the sample table 4 into the soft deposition cavity 1; s4 filling SF into the sample cavity 26A matrix gas forming a fluorinated monolayer film base, SF being controlled by a vacuum gauge 17 observing the soft deposition chamber 1 and the sample chamber 26A flow rate of the matrix gas; s5, carrying out gas phase cluster soft deposition, after the gas phase cluster soft deposition is finished, shortening the sample telescopic rod 8, closing the gate valve 3, closing the vacuum module and the gas distribution module, opening the observation window 12, and taking out the sample.
In step S5, when performing the soft deposition of the gas cluster, the mass spectrometer performs mass spectrometry on the gas cluster in real time, and after the mass spectrometry, the soft deposition system can screen out the clusters with a specific mass range or a specific mass number for the soft deposition. Or calculating the flux of the gas phase cluster through mass spectrum peak intensity obtained by mass spectrum analysis, and determining the soft deposition time to ensure that the obtained sample amount meets the requirements of morphology research and material performance characterization.
The above embodiments are only used for illustrating the present invention, and the structure, connection mode, manufacturing process, etc. of the components may be changed, and all equivalent changes and modifications performed on the basis of the technical solution of the present invention should not be excluded from the protection scope of the present invention.

Claims (9)

1. An insertable vapor cluster soft deposition method comprising: the device comprises a soft deposition cavity, a sample cavity, a vacuum module and a gas distribution module, wherein the soft deposition cavity and the sample cavity are sequentially connected; a mass spectrometer is arranged in the soft deposition cavity and used for carrying out mass spectrometry on the gas-phase clusters; the sample cavity and the soft deposition cavity are divided or communicated through a gate valve arranged at the joint of the sample cavity and the soft deposition cavity, a sample table capable of reciprocating is arranged in the sample cavity, and a deposition substrate is arranged on the sample table; the vacuum module vacuumizes the soft deposition cavity and the sample cavity when the gate valve is opened; the gas distribution module is used for introducing inert gas into the vacuumized soft deposition cavity and the vacuumized sample cavity, and is characterized by comprising the following steps:
s1, opening the gate valve, vacuumizing the soft deposition cavity and the sample cavity to a preset vacuum degree, and closing the gate valve;
s2, filling gas-phase clusters into the soft deposition cavity, regulating kinetic energy of gas-phase cluster ions by applying different direct-current voltages to an ion lens group, and performing mass spectrometry on the gas-phase clusters;
s3, opening the gate valve, extending the sample telescopic rod, and placing the sample table into the soft deposition cavity;
s4 filling SF into the sample cavity6A matrix gas forming a fluorinated monolayer film substrate;
s5, carrying out gas phase cluster soft deposition, after the gas phase cluster soft deposition is finished, shortening the sample telescopic rod, closing the gate valve, closing the vacuum module and the gas distribution module, opening the observation window, and taking out the sample.
2. The insertable vapor cluster soft deposition method of claim 1, wherein the mass spectrometer comprises a quadrupole mass analyzer and an electron multiplier which are arranged at the same height, and a spatial region between the quadrupole mass analyzer and the electron multiplier and at the same height as the quadrupole mass analyzer and the electron multiplier is a detection region.
3. The insertable gas cluster soft deposition method of claim 1, wherein the sample stage is connected with a sample telescopic rod and a driver in sequence, and the driver controls the length of the sample telescopic rod so as to drive the sample stage to reciprocate.
4. The insertable gas cluster soft deposition method of claim 2, wherein a graduated scale is arranged on one side of the sample telescopic rod or the sample telescopic rod; and the side wall of the soft deposition cavity and the side wall of the sample cavity are both provided with observation windows, and the sample platform is ensured to be positioned in the detection area of the mass spectrometer through the graduated scale and the observation windows.
5. The insertable gas cluster soft deposition method of any one of claims 1 to 4, wherein a cooler is arranged on the sample stage, and the cooler cools the sample stage by using liquid nitrogen or a cryogenic cooling stage.
6. The pluggable vapor cluster soft deposition method according to any one of claims 1-3, wherein the inert gas introduced into the gas distribution module is SF6A matrix gas for forming a fluorinated monolayer film substrate with the deposition substrate, vacuum gauges arranged on the soft deposition chamber and the sample chamber, and SF control by observing vacuum gauge readings of the soft deposition chamber and the sample chamber6The flow rate of the matrix gas.
7. The pluggable vapor cluster soft deposition method of claim 6, wherein the gas distribution module comprises raw SF6Gas delivery pipe, dilution gas delivery pipe, gas mixing chamber and SF6A substrate gas delivery tube; gas mixing chamber is respectively connected with original SF6The gas delivery pipe, the dilution gas delivery pipe are communicated with each other, and the original SF6The gas and the diluent gas are mixed in the gas mixing chamber to form SF with preset content6A matrix gas, and passing SF6A substrate gas delivery pipe for delivering the SF6Matrix gas is passed into the sample chamber.
8. The insertable vapor cluster soft deposition method of any one of claims 1 to 4, wherein the soft deposition chamber comprises an ion lens set, and the kinetic energy of the vapor cluster ions charged into the soft deposition chamber is adjusted by applying different direct current voltages to each ion lens in the ion lens set.
9. The insertable vapor cluster soft deposition method according to claim 1, wherein in step S5, during the vapor cluster soft deposition, the mass spectrometer performs mass spectrometry on the vapor cluster in real time, calculates the flux of the vapor cluster from the mass spectrum peak intensity obtained by the mass spectrometry, and determines the soft deposition time so that the obtained sample amount meets the requirement of the subsequent detection.
CN201911273496.9A 2019-12-12 2019-12-12 Insertable gas-phase cluster soft deposition method Active CN110965041B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911273496.9A CN110965041B (en) 2019-12-12 2019-12-12 Insertable gas-phase cluster soft deposition method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911273496.9A CN110965041B (en) 2019-12-12 2019-12-12 Insertable gas-phase cluster soft deposition method

Publications (2)

Publication Number Publication Date
CN110965041A CN110965041A (en) 2020-04-07
CN110965041B true CN110965041B (en) 2021-04-06

Family

ID=70034044

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911273496.9A Active CN110965041B (en) 2019-12-12 2019-12-12 Insertable gas-phase cluster soft deposition method

Country Status (1)

Country Link
CN (1) CN110965041B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111733392A (en) * 2020-07-01 2020-10-02 中国科学院化学研究所 Gas-phase cluster reaction device, reaction system and method
CN114324083B (en) * 2022-01-06 2023-09-05 北京航空航天大学合肥创新研究院(北京航空航天大学合肥研究生院) Nano cluster beam integrated deposition on-line test system
CN115290738B (en) * 2022-07-26 2024-06-07 中国科学院化学研究所 Cluster rich-pressure reaction and large-flux mass-selection soft deposition device and method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1853255A (en) * 2003-06-21 2006-10-25 莱克公司 Multi-reflecting time-of-flight mass spectrometer and a method of use

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9484220B2 (en) * 2013-03-15 2016-11-01 International Business Machines Corporation Sputter etch processing for heavy metal patterning in integrated circuits

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1853255A (en) * 2003-06-21 2006-10-25 莱克公司 Multi-reflecting time-of-flight mass spectrometer and a method of use

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"An energy-filtering device coupled to a quadrupole mass spectrometer for soft-landing";A. Bodin等;《Review of Scientific Instruments》;20130930(第84期);095104 *
"Soft landing of bare nanoparticles with controlled size, composition, and morphology";Grant E.Johnson等;《NANOSCALE》;20150119;第7卷(第8期);第3494页右栏第29行-3495左栏第9行，图1 *

Also Published As

Publication number Publication date
CN110965041A (en) 2020-04-07

Similar Documents

Publication Publication Date Title
CN110965041B (en) Insertable gas-phase cluster soft deposition method
CN2837831Y (en) Ultra-high vacuum in-situ growth, characterization and test system
MLZ KWS-2-small angle scattering diffractometer
CN103295873B (en) A kind of method and apparatus producing analysis ion under low pressure
CN102312224B (en) Beam-induced deposition at cryogenic temperatures
Larsen Diffraction studies of crystals at low temperatures–crystallography below 77 K
US10994256B2 (en) High-throughput combinatorial materials experimental apparatus for in-situ synthesis and real-time characterization and related methods
US20160123847A1 (en) Micromanipulator for a cryomicrotome
CN109075016B (en) Package for an open ionizing ion source
US8816274B2 (en) Mass spectrometer
CN102156116A (en) Graphene sheet intercalation compound preparation method and in situ microRaman representation system
US9996090B2 (en) Preparation of high pressure BF3/H2 mixtures
CN106814095B (en) Freezing sample preparation device for scanning electron microscope
CN111549339A (en) Method for enhancing bonding fastness of graphene and base material
CN106637114B (en) Cluster beam experimental device and preparation method of nanocluster
Moore et al. Size-dependent dynamics of a quantum solvent: Laser spectroscopy of HCN–(HD) n grown in helium nanodroplets
Maryott et al. Effective collision numbers for angular momentum relaxation from nuclear relaxation studies of simple liquids
Claassen et al. Matrix‐Isolation Raman and Infrared Spectra, Molecular Structure, and Force Constants for XeO3F2
CN110988107B (en) Sublimation-recrystallization mass spectrometry imaging matrix precipitation device and method with controllable crystallization temperature
CN113655078A (en) Sample vacuum preparation cavity
CN217361499U (en) Adjusting mechanism of ionization device
CN106996942B (en) A kind of optical path switching system
CN109569432A (en) Chemical reaction method in a kind of vacuum
Pye et al. α-Gallium oxide deuteriohydroxide: A powder neutron diffraction investigation
CN102818799A (en) In situ microscopic Raman characterization system

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant