CN1982499A - Method and apparatus for growing and forming gas-phase depositing materials - Google Patents

Method and apparatus for growing and forming gas-phase depositing materials Download PDF

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Publication number
CN1982499A
CN1982499A CN 200510132107 CN200510132107A CN1982499A CN 1982499 A CN1982499 A CN 1982499A CN 200510132107 CN200510132107 CN 200510132107 CN 200510132107 A CN200510132107 A CN 200510132107A CN 1982499 A CN1982499 A CN 1982499A
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laser
growth
gas
vacuum chamber
substrate
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CN 200510132107
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曹则贤
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Institute of Physics of CAS
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Institute of Physics of CAS
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Priority to CN 200510132107 priority Critical patent/CN1982499A/en
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Abstract

Method for growing and forming gas-phase depositing material and its apparatus are disclosed. The process is carried out by inducing gas, passing a beam of laser into lining surface to build ionogenic channel, adding positive high-voltage onto pin-hole electrode of light path, determining initial growth position, gas-phase depositing, scanning for columnar discharge by set mode, controlling growth time and operation gas and disposable forming. The apparatus consists of vacuum chamber, substrate table, pinpoint electrode, laser, laser lead-in component and scanning electron microscope. Collimated discharging zone is formed between ion channel and substrate surface along laser beam. It has better film-parameter precision, four-dimensional structure and can be used for after treatment by laser beam.

Description

The method and the device of a kind of gas-phase depositing materials growth and moulding
Technical field
The present invention relates to the method and apparatus of a kind of gas-phase depositing materials growth and structure disposal molding, the method and apparatus of the disposal molding of material growth and structure style is carried out in particularly a kind of laser alignment discharge.
Background technology
Film is the main mode that current material is used, and film gauge uniformity is the key index of film growth techniques.For many existing film growth methods, as adopting the mode of thermal evaporation or ion sputtering, the homogeneity of film thickness is the problem that must take measures to solve always.Usually, thin film growth process can take to rotate sample table, use modes such as a plurality of (multi-angle incident) particle source to make every effort to obtain uniform film, but effect is unsatisfactory.
On the other hand, the main process that film growth is made as micro structural component, the making of identity unit requires film to form certain style (periodically arranged form by undersized unit) on the big area.At present, the method for generally taking is the grow up uniform thin film of area of Mr., covers the last layer mask, and required style utilization exposure is copied on the mask, will pass through chemical etching then, and operations such as cleaning just can obtain required style; Perhaps utilize sweep beam or ionic fluid directly to etch required style.But these methods all have problems such as complex process, time consumption and energy consumption, efficient be low.
People's expectation if the material growth is undertaken by the point-like growth, then scans by the cathode tube imaging mode substrate plane, then is easy to obtain strict film uniformly.Simultaneously, if scan and the control growing time, promptly according to (t) three parameter control material process of growth then can obtain the growth of three-dimensional structure style for x, y according to specific style.Further, in fixed point material process of growth, add the control of composition c again, then can realize (x, y, t, c) disposal molding of four-dimensional structure.This kind growth method will comprise the electron device and following photonic device to being the micro-nano technology and the designed element manufacturing of industry of material foundation with the film, is with a wide range of applications and great economy value.
Summary of the invention
Gas-phase depositing materials is grown and the method for complex construction disposal molding to the purpose of this invention is to provide a kind of brand-new carrying out with dot pattern; Another object of the present invention provides a kind of brand-new material growth method, and ion microbeam directed, that have suitable energy cooperates illumination to provide new material growth method to the reactivation process of growth surface; A further object of the invention is to realize the growth of multiple material structure style on appointed positions neatly.
To achieve these goals, the present invention takes following technical scheme:
The method of a kind of gas-phase depositing materials growth and moulding comprises the steps:
1) in vacuum chamber, feeds the required working gas of growth this kind material;
2) make a laser beam impinge perpendicularly on substrate sample surface on the substrate table in the vacuum chamber, and a needlepoint electrode is placed on the laser optical path;
3) substrate sample on the substrate table places low potential, and needlepoint electrode places noble potential;
4) under the cooperation of surface sweeping Electronic Speculum, find the growth position that will begin; Making alive causes discharge, the beginning vapor deposition processes;
5) discharge of laser alignment is scanned according to the cover half formula with respect to substrate table;
6) growth time on the control specified location is realized desired thickness (t); The component of working gas realizes the adjusting of material chemical composition (c) on the control specified location.
In technique scheme, comprise that also step 7) removes the high pressure on the needlepoint electrode, utilize laser beam to do the aftertreatment of film; Described aftertreatment refers to the annealing taked after film growth finishes, cooling, steps such as radiation modification.
In technique scheme, further, step 3) is taked substrate ground connection, needle point loads positive high-voltage, magnitude of voltage is generally kilovolt (kV) magnitude, depend on working gas and operating air pressure and grow desired particle of concrete material is arrived the energy of growth surface, carry out desired material and be grown to suitable to produce discharge.
In technique scheme, further, step 2) laser beam adopts the ultraviolet laser or the high power pulsed laser of high photon energy; Acting as of laser produces an ionic channel in advance, thus laser beam can ionization employed working gas be basic demand, adopt the ultraviolet laser ionization or the high power pulsed laser ionization mode of high photon energy.
In technique scheme, further, step 2) laser beam adopts optical fiber to import vacuum chamber described in, and the optical fiber that imports laser is integrated with needle point foremost; Optical fiber front end and needle point are made an integral body, make the discharge stability that ionic channel retrained that light beam causes, thereby guarantee that film fixed point mode is grown in (x, y) tolerance range of position in the plane and size.
In technique scheme, further, integrated on same shockproof platform of described substrate table and needle point/fiber port.Can effectively avoid in the process of growth needle point/fiber port with respect to the random motion of substrate like this, (x, y) tolerance range of growth in the plane are provided.
In technique scheme, further, in step 6), also comprise: regulate the diameter of the parameter change ionic channel of laser beam, the change of cooperating gas atmosphere and operating voltage, thereby the diameter of the vegetative point of change pointwise growth pattern.
In technique scheme, further, can cooperate the location of vegetative point and the on-line monitoring of actual growth structure with the scanning electron microscope of electric discharge device non-interference.
A kind of gas-phase depositing materials growth and shaping structures device comprise:
Vacuum chamber 10, this vacuum chamber are provided with conventional introducing port 31 that is used for the required working gas of vapour deposition and export mouth 32; Described introducing port 31 connects the gas source (not shown), and described export mouth 32 is connected with a vacuum pump (not shown); It is characterized in that, also comprise:
Substrate table 11 is in the described vacuum chamber 10, in that (x y) does two-dimentional any-mode and moves in the plane, substrate 12 is fixed on this substrate table 11;
Electrode 13 is in the vacuum chamber 10, is connected with a high-voltage power supply 14, makes described electrode 13 that positive high voltage be arranged; Substrate sample ground connection on the described substrate table 11;
Described electrode 13 has a bracing frame 15, and the distance between support frame as described above 15 and the described substrate table 11 can be regulated;
Laser apparatus 16 is in outside the described vacuum chamber 10;
Laser imports member 17, and the laser that laser apparatus 16 is sent imports vacuum chamber 10 and perpendicular to described substrate 12;
The scanning electron microscope device that electron beam gun 20 and detector 21 are formed;
Described electrode (13) is on the light path of described laser, makes the ionization passage that provides along laser beam between described electrode (13) and described substrate sample (12) surface form a region of discharge (18);
Described electrode 13 is a needlepoint electrode;
In technique scheme, further, described laser imports member 17 and comprises optical fiber, joins with described laser apparatus 16 by the flange on the vacuum chamber, is used for laser beam is imported in the vacuum chamber perpendicular to substrate ground.
The port one 9 of described needlepoint electrode 13 and optical fiber integrates, and the laser output of the another port of optical fiber and laser apparatus 16 is coupled.
In technique scheme, further, the importing of laser can also be adopted another kind of mode, and described laser imports member 17 and comprises: described vacuum chamber has a transparent window, and the laser that described laser apparatus 16 sends sees through the surface that described transparent window impinges perpendicularly on described substrate 12.
In technique scheme, further, described substrate table 11 is done (x, y) two-dimentional any the moving in the plane by stepper-motor or piezoelectric ceramics control.
The present invention utilizes the geseous discharge of collimation, according to the principle of vapor deposition growth, realizes the material growth that pointwise is carried out.Be aided with the two-dimensional scan of substrate and the control of growth time, provide a kind of can direct growth high thickness evenness film or have a kind of like this growth and the forming technique of the material structure of specific four-dimensional style in the big area.It is in the nature plasma auxiliary chemical vapor deposition.
Compared with prior art, the invention has the advantages that:
1) pointwise growth growth pattern has improved the precision of controlling thin film parameter;
2) cooperate the adjusting of scan mode and working gas composition can realize (x, y, t, c) disposal molding of four-dimensional structure;
3) after the material structure growth is finished, can utilize ready-made laser beam to do necessary aftertreatment;
4) can be used for point-like, wire, two-dimentional style, the growth of the various style structures that three-dimensional style that each dot thickness is different and composition variation+aforesaid space style form.
Description of drawings
Fig. 1 represents laser alignment geseous discharge film growth schematic representation of apparatus of the present invention;
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail:
Accompanying drawing 1 is the disclosed schematic diagram that can strengthen growth of chemical vapour deposition material and structure disposal molding technology with the laser alignment geseous discharge that the fixed point mode is grown of invention.Beam of laser incides on the substrate of ground connection along the metal needle point, the very thin plasma body conductive channel that laser ionization working gas forms is used for the discharge process that caused by high pressure between standard needle point and the substrate, make the needle point discharge be limited in very thin column scope, thereby on substrate, realize the film growth of pointwise pattern.Substrate is done in the XY plane accurately according to setting moving of style by electric motor driving.The component that chemical composition changes by change gas precursor realizes.The scanning electron microscope of configuration is used for locating and on-line monitoring in the growth room.
Make a kind of film growth device with reference to Fig. 1, comprising: vacuum chamber 10, this vacuum chamber are provided with conventional introducing port 31 that is used for the required working gas of vapour deposition and export mouth 32; Described introducing port 31 connects the gas source (not shown), and described export mouth 32 is connected with a vacuum pump (not shown); Also comprise: substrate table 11 is in the described vacuum chamber 10, in that (x y) does two-dimentional any-mode and moves in the plane, substrate 12 is fixed on this substrate table 11; Electrode 13 is in the vacuum chamber 10, is connected with a high-voltage power supply 14, makes described electrode 13 that positive high voltage be arranged; Substrate sample ground connection on the described substrate table 11; Described electrode 13 has a bracing frame 15, and the distance between support frame as described above 15 and the described substrate table 11 can be regulated; Laser apparatus 16 is in outside the described vacuum chamber 10; Laser imports member 17 and adopts optical fiber, joins with described laser apparatus 16 by the flange on the vacuum chamber, is used for that laser imported vacuum chamber 10 and perpendicular to described substrate 12; The scanning electron microscope that electron beam gun 20 and detector 21 are formed is used for location and monitoring; Needlepoint electrode 13 is on the light path of described laser, makes the ionization passage that provides along laser beam between described electrode 13 and described substrate sample 12 surfaces form a region of discharge 18; In the present embodiment, the port one 9 of described needlepoint electrode 13 and optical fiber integrates.Described substrate table 11 is done (x, y) two-dimentional any the moving in the plane by step motor control.
In conjunction with said apparatus, with two embodiment material growth of the present invention and structure forming method are described in detail below.
Embodiment 1
According to method provided by the invention, as embodiment, on silicon substrate, be grown to example with the diamond-like style, comprise step specific as follows:
(1) import working gas in vacuum chamber, working gas comprises methane, hydrogen.
(2) import He-Gd laser ionization working gas with optical fiber;
(3) substrate ground connection adds 1 kilovoltage on electrode, the distance between adjusting needle point-substrate and the air pressure of working gas, the electrical discharge zone of acquisition column to substrate from needle point; Quasi-diamond begins growth on substrate; Those skilled in the art know, and under given operating air pressure, can obtain discharge in sizable coupling parameter space of operating distance and operating voltage;
(4) under the scanning electron microscope guiding, needle point is moved to specified growth starting point, keep needle point/substrate relative position motionless, realize the point-like growth; Make needle point/substrate relative position do linear time base sweep, obtain the growth of one-dimentional structure; Make needle point/substrate relative position do two-dimentional continuous sweep, obtain the continuous film of two dimension; Make needle point/substrate relative position do two-dimensional scan, cooperate the control of growth time on the each point, obtain the three-dimensional structure of expectation by the style of setting;
(5) laser beam of Li Yonging carries out aftertreatment to the heating effect of the film that generated to the film pointwise.
Embodiment 2
For the film growth of the structure style that comprises Composition Control, be example with the SiC-Si-C system, concrete steps comprise:
(a) in step (1) working gas of embodiment 1, add silane, carry out step (2)-step (4) of embodiment 1 then;
(b) under the fixed point growth pattern, increase the content of silane gradually and reduce the content of methane, this some place settling then can carry out the transition to pure silicon by SiC.
(c) the various spacescan modes of step 4) among the cooperation embodiment 1 obtain to have added the various structure styles of Composition Control.
It should be noted last that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is had been described in detail with reference to embodiment, those of ordinary skill in the art is to be understood that, technical scheme of the present invention is made amendment or is equal to replacement, do not break away from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of the claim scope of the present invention.

Claims (10)

1, the method for a kind of gas-phase depositing materials growth and moulding comprises the steps:
1) in vacuum chamber, feeds the required working gas of growth material;
2) make a laser beam impinge perpendicularly on substrate sample surface on the substrate table in the vacuum chamber, and a needlepoint electrode is placed on the laser optical path;
3) substrate sample on the substrate table places low potential, and needlepoint electrode places noble potential;
4) under the cooperation of surface sweeping Electronic Speculum, find the growth position that will begin; Making alive causes discharge, the beginning vapor deposition processes;
5) discharge of laser alignment is scanned according to the cover half formula with respect to substrate table;
6) growth time on the control specified location is realized desired thickness (t); The component of working gas realizes the adjusting of material chemical composition (c) on the control specified location.
2, according to the method for described gas-phase depositing materials growth of claim 1 and moulding, comprise that also step 7) removes the high pressure on the needlepoint electrode, utilize laser beam to do the aftertreatment of depositional texture; Described aftertreatment refer to grow annealing, cooling, the radiation modification taked after finishing handled.
3, according to the method for described gas-phase depositing materials growth of claim 1 and moulding, described step 3) is taked substrate ground connection, and needlepoint electrode loads positive high-voltage.
4, laser beam according to the method for growth of the described gas-phase depositing materials of claim 1 and moulding, step 2) adopts the ultraviolet laser of high photon energy or high power pulsed laser to realize the ionization of at least a working gas.
5, according to the method for growth of the described gas-phase depositing materials of claim 1 and moulding, step 2) laser beam described in adopts optical fiber to import vacuum chamber, the optical fiber that imports laser is integrated with needlepoint electrode foremost, and described substrate table and needle point/fiber port are integrated on same shockproof platform.
6, according to the method for each described gas-phase depositing materials growth of claim 1-5 and moulding, it is characterized in that, with the location of the scanning electron microscope realization vegetative point of electric discharge device non-interference and the on-line monitoring of growth structure; When fixing a point to grow, change the working gas composition, realization comprises the growth of the structure style of Composition Control.
7, the device of a kind of gas-phase depositing materials growth and moulding, comprising: vacuum chamber (10), this vacuum chamber are provided with introducing port (31) and the export mouth (32) that is used for the required working gas of vapour deposition; Described introducing port (31) connects gas source, and described export mouth (32) is connected with a vacuum pump; Be in the substrate table (11) in the described vacuum chamber (10); It is characterized in that, also comprise:
Described substrate table moves for planar doing two-dimentional any-mode, and substrate (12) is fixed on this substrate table (11);
Electrode (13) is in the vacuum chamber (10), is connected with a high-voltage power supply (14), makes described electrode (13) that positive high voltage be arranged; Substrate sample ground connection on the described substrate table (11);
Described electrode (13) has a bracing frame (15), and the distance between support frame as described above (15) and the described substrate table (11) can be regulated;
Laser apparatus (16) is in outside the described vacuum chamber (10);
Laser imports member (17), and the laser that laser apparatus (16) is sent imports vacuum chamber (10) and perpendicular to described substrate (12);
The electron-microscope scanning device that electron beam gun (20) and detector (21) are formed;
Described electrode (13) is on the light path of described laser, makes the ionization passage that provides along laser beam between described electrode (13) and described substrate sample (12) surface form a region of discharge (18);
Described electrode (13) is a needlepoint electrode.
8, according to the device of described gas-phase depositing materials growth of claim 7 and moulding, it is characterized in that described laser imports member (17) and comprises optical fiber, be used for laser beam is imported in the vacuum chamber perpendicular to substrate ground; One port (19) of described needlepoint electrode (13) and optical fiber integrates, and the another port of optical fiber and the delivery port of laser apparatus are coupled.
9, according to the device of growth of the described gas-phase depositing materials of claim 7 and moulding, it is characterized in that, described laser imports member (17) and comprising: described vacuum chamber 10 has a transparent window, and the laser that described laser apparatus (16) sends sees through the surface that described transparent window impinges perpendicularly on described substrate (12).
According to the device of each described gas-phase depositing materials growth of claim 7-9 and moulding, it is characterized in that 10, described substrate table (11) is done two dimension by stepper-motor or piezoelectric ceramics control and moved arbitrarily.
CN 200510132107 2005-12-16 2005-12-16 Method and apparatus for growing and forming gas-phase depositing materials Pending CN1982499A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102539200A (en) * 2010-12-14 2012-07-04 中国核动力研究设计院 Preparation technology for irradiated nuclear fuel core electron microscope sample
CN103632912A (en) * 2012-08-21 2014-03-12 B-纳诺有限公司 Electron microscopy imaging system and method
CN114164417A (en) * 2021-11-23 2022-03-11 安徽工业大学 Method for realizing controllable ionization of different particles in vapor deposition by using vacuum ultraviolet light
CN114182212A (en) * 2021-11-23 2022-03-15 安徽工业大学 Method for improving ionization rate in vapor deposition process by using vacuum ultraviolet light

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102539200A (en) * 2010-12-14 2012-07-04 中国核动力研究设计院 Preparation technology for irradiated nuclear fuel core electron microscope sample
CN102539200B (en) * 2010-12-14 2013-08-21 中国核动力研究设计院 Preparation technology for irradiated nuclear fuel core electron microscope sample
CN103632912A (en) * 2012-08-21 2014-03-12 B-纳诺有限公司 Electron microscopy imaging system and method
CN114164417A (en) * 2021-11-23 2022-03-11 安徽工业大学 Method for realizing controllable ionization of different particles in vapor deposition by using vacuum ultraviolet light
CN114182212A (en) * 2021-11-23 2022-03-15 安徽工业大学 Method for improving ionization rate in vapor deposition process by using vacuum ultraviolet light

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