CN104555911A - Method for manufacturing nanowire - Google Patents
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- CN104555911A CN104555911A CN201510028655.4A CN201510028655A CN104555911A CN 104555911 A CN104555911 A CN 104555911A CN 201510028655 A CN201510028655 A CN 201510028655A CN 104555911 A CN104555911 A CN 104555911A
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Abstract
The invention provides a method for machining and manufacturing a small-size nanowire through broad-beam electron beams on the basis of the electron beam induction and sedimentation principle with organic gas or metal compounds serving as a gas source and raw materials. Through the gradient effect and the margin effect of the intensity distribution inside beam spots of te broad-beam electron beams and an electron beam position control method, the manufacturing in the mode that the set-length and set-diameter direct reading and writing are conducted on nanowire materials at set positions is achieved.
Description
Technical field
The present invention relates to one utilizes volatility source of the gas for raw material, the method of nano wire is prepared based on the processing of e-beam induced deposition principle, particularly relating to a kind of use utilizes wide-beam electronic bundle to prepare the method for small size nano wire, belongs to technical field prepared by sophisticated semiconductor material.
Background technology
In recent years, along with going deep into of scientific research, nano-material has more and more been applied to electronic device manufacture, high performance material, the fields such as common consumer product.Especially, manufacture field at advanced semi-conductor electronic device, nano wire may be used for manufacturing undersized semi-conducting material to obtain excellent device performance.And the position usually needing nano wire to be positioned to determine when using nano wire to build semi-conductor electronic device is to realize being electrically connected or certain functional characteristic.Now, a kind of means directly preparing nano wire at assigned address can preferably be had.These means preferably can be good location, and to realize nanowire diameter, length, the control of the characteristics such as shape.At present, one of most effective method that can realize this function is the method that e-beam induced deposition (EBID) prepares nano thread structure.The general principle utilizing e-beam induced deposition to prepare nano wire is that the organic molecule utilizing high-power electron beam to make to be adsorbed in substrate surface under low pressure environment decomposes, carbon in its Middle molecule or metallic element are deposited on substrate surface in solid form, but not carbon composition then forms volatilization is pulled away mutually.It is generally acknowledged, the live width of the nano wire using e-beam induced deposition to prepare is directly relevant to the bundle spot size of electron beam.Due to the dispersion effect of electron beam and matter interaction, the live width of the nano wire obtained generally is greater than the diameter of electron beam spot.For this reason, in order to obtain the nano wire of little live width, the electron beam that bundle spot is less must be used.At present, use good instrument and equipment, the bundle spot of electron beam may be contracted to the level of sub-nanometer scale.But due to the dispersion effect that electronics and material surface effect produce obtain live width generally in the magnitude of ten nanometers.And will obtain this live width, supporting electron beams converge system needs to spend huge cost.
Under As-Is, in most of application scenario, the live width of tens nanometer is acceptable, but still needs the beam spot diameter, of nanometer scale, and its cost is still higher.Because the size of the electron beam spot that may reach directly determines the cost of electron-optical system, therefore, finding a kind of method preparing little live width under large beam spot condition must reduce costs greatly, the development of great aspect related direction.
As previously mentioned, based on the principle of routine, due to the dispersion effect that electron beam and material effects produce, the live width of nano wire must be greater than the diameter of used electron beam.The electron beam of large beam spot is used to prepare undersized nano wire seemingly impossible.And this principle seems to also limit the nano thread structure that method small size nano wire being prepared by e-beam induced deposition is applied to low cost prepares aspect.The present invention analyzes by experiment, confirms the feasibility using the electron beam of large beam spot to prepare undersized nano wire.This method, based on new e-beam induced deposition mechanism, can reduce the cost of related fields greatly, be conducive to the development of related industry.
Summary of the invention
Goal of the invention: the present invention proposes a kind of use organic gas or metallic compound is raw material as source of the gas, uses wide-beam electronic bundle, prepares the method for small size nano wire based on the processing of e-beam induced deposition principle.Utilizing Gradient Effect and its edge effect of intensity distribution in wide-beam electronic bundle bundle spot, by controlling the method for electron-beam position, realizing nano-material carries out the direct read/write mode formulating length and diameter preparation in formulation position.
Technical scheme of the present invention is: a kind of method preparing nano wire, and concrete steps are as follows:
(1) by needing the substrate of grow nanowire to put into vacuum chamber, vacuumizing, controlling pressure in vacuum tank 10
-3-10
-6pa, passes into source of the gas, and controlling to pass into the indoor pressure of source of the gas final vacuum is 10
-1-10
-4pa;
(2) unlocking electronic bundle after source of the gas is stable, regulate the focus state of electron beam, make electron beam in beam spot diameter, the mean intensity of electron beam is greater than 10
2e/nm
2/ s; And regulate the intensity distribution situation at electron beam edge, make intensity have uneven distribution along edge, namely it is greater than 10 from bundle spot edge along the spatial variations rate in beam spot diameter, direction
2e/nm
2/ s/100nm; The diameter of electron beam spot is 2-1000 times of the nanowire diameter of required preparation;
(3) the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material, point cantact between described substrate location and bundle spot edge, and contact point grows nanostructured after contact at once, afterwards with certain speed counter substrate mobile electron bundle, in moving process, by controlling its translational speed and focal position makes the edge of electron beam spot be positioned at the tip of the nanostructured newly grown all the time, form nano wire; Also the growth top of nano wire is namely kept to extend along with the edge of electron beam; The speed of electron beam counter substrate movement is the speed of nanowire growth;
The decision method of the speed v of described electron beam counter substrate movement is as follows:
Obtain the deposition rate z of source of the gas under step (2) described electron beam in step (1) by experiment, the diameter D of nano wire and electron beam counter substrate movement speed v linear correlation:
wherein, L is the length that nano wire grows within the t time, and it is v=L/t with the pass of electron beam counter substrate movement speed v, so
namely, when deposition rate z and the nanowire diameter D that need prepare are certain, electron beam movement speed v can be obtained;
(4) close electron beam after terminating the growth of nano wire, obtain the nano thread structure of required preparation.
Further, described in step (3), the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material; Concrete: when being the edges of substrate of thickness below 500 nanometers when needing the substrate location of growing nano wire material, by the bundle spot edge of electron beam and the EDGE CONTACT of substrate, other end does not all contact.
Further, described in step (3), the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material; Concrete: when need the substrate location of growing nano wire material be substrate flat surfaces on a some time, first at the growing point that this some place's deposit is protruded, change the relative position of substrate and electron beam afterwards, contacted with the growing point of described protrusion by the bundle spot edge of electron beam, other end does not all contact.
Further, the preparation method of described growing point is: use semiconductor technology to prepare a bulge-structure, or uses the method for inclination substrate to use e-beam induced deposition to prepare a bulge-structure needing the substrate location of growing nano wire material.
Further, in step (3) in electron beam and substrate relative movement thereof, in position stop or change the relative movement direction of electron beam and substrate, the former can produce bamboo knot shaped structure, the latter produces bending carbon nanocoils, and the uneven meeting of translational speed makes nano wire there is different diameters.
Further, step (1) described source of the gas is organic gas, for growing carbon nanocoils; Or metallic compound, for growing metal nano wire.
Beneficial effect of the present invention: use wide-beam electronic bundle, the method of small size nano wire is prepared based on the processing of e-beam induced deposition principle, utilize Gradient Effect and its edge effect of intensity distribution in wide-beam electronic bundle bundle spot, by controlling the method for electron-beam position, realize nano-material carries out the direct read/write mode formulating length and diameter preparation in formulation position.
1., without the need to the electron beam of converged state, greatly reduce cost.As introduced above, great majority use the method reducing bundle spot at present, need very high one-tenth originally to improve electron-optical system.And the present invention does not need.
2. high accuracy, adjustable point.Whole process is undertaken by the position controlling electron beam, and current reasonable its positioning precision of electron beam irradiation system can control at sub-nanometer level.Therefore the method can realize the preparation of high-precision fixed point.
3. catalyst-free.Do not need in whole process to use catalyst.And the method preparing nano wire at present needs to use catalyst mostly.This method decreases the possible pollution that catalyst brings.
4. room temperature can be carried out, without the need to high temperature, and preparation technology easily.The fabricate of nanowires many at present needs to use hot conditions, is unfavorable for energy-conservation and reduces costs.
5. the diameter of nano wire, length, the control that the direction of growth etc. can be good, can also use the method to prepare the nano wire of multiple bending or curved shape.The direction of growth of nano wire is the direction of relative movement along electron beam and substrate all the time, and and beam spot radial parallel.Prepared nano wire can be vertical with substrate surface or angled, depends on the relative orientation of substrate and electron beam and the direction of both relative motions.
6. can realize the preparation of multiple material nano wire.Its material that can prepare only depends on used source of the gas.As long as there is suitable source of the gas just can realize the preparation of corresponding nano-material.
7. prepare fast, EBID preparation process growing nano linear velocity is comparatively large, can reach hundreds of nanometer even speed of micron per minute.Conventional physical vapour deposition (PVD), the methods such as chemical vapour deposition (CVD) are difficult to reach this speed.
Accompanying drawing explanation
Fig. 1: the intensity distribution in electron beam spot.Top is bundle spot irradiation intensity distribution schematic diagram in the plane, and wherein dotted line is the edge of electron beam, the region that black part is divided into intensity large.Bottom is the intensity distribution along beam spot diameter, direction.The dotted line separated region of double-head arrow instruction represents the region that electron beam intensity changes greatly.These regions are conducive to the deposit of the electron beam-induced based on edge effect.
Fig. 2: schematic diagram of the present invention, the deposition process of material within the scope of electron beam spot.Wherein solid black lines region is electron beam irradiation region, the edge shape that black dotted lines painting material is expanded gradually in electron beam spot.On figure, D1 is depicted as a smaller deposition size, and D2 is the diameter through deposit forming shape after a period of time, and D3 is the shape that material is formed within the scope of bundle spot after the longer time.White dashed line is shown as the material shape edges that deposit is formed within the scope of bundle spot after the long enough time.In order to reach the nano wire obtaining and be significantly less than Electron Beam spot size, the situation being less than D3 should be used to carry out the fabricate of nanowires as far as possible.During actual preparation, electron beam contacts the nanostructured that can grow up to D1-D3 situation with substrate one.
Fig. 3: schematic diagram of the present invention.A: nano thread structure.B: electron beam spot.C: nanowire growth end, its growing end is positioned at the bundle spot edge of electron beam.The arrow signal moving direction of electron beam and the direction of growth of nano wire.
Fig. 4: use the inventive method to prepare carbon nano-structured process.The growth leading portion of figure upward arrow instruction carbon nanocoils.On figure, border circular areas is the wide-beam electronic bundle for growing carbon nanocoils.The position of electron beam is fixed.Can see and mainly grow (figure a-e) along the radial direction of electron beam at the initial stage of nanowire growth, this growth pattern makes its length increase.In the later stage (figure f-h) of growth, carbon nanocoils is obvious along the growth in diameter itself direction, causes the increase of nanowire diameter.
Fig. 5: carbon nanowire structures prepared by embodiment 1.On figure, scale is 50 nanometers.
Fig. 6: carbon nanowire structures prepared by embodiment 2.On figure, scale is 100 nanometers.
Fig. 7: the schematic diagram using the present invention's grow nanowire on edges of substrate.Wherein D is substrate, and B is electron beam, and A is the nano wire grown.In figure: the position of substrate and electron beam during (a) initial growth state.C () is top view corresponding during initial growth state; (b) in nanowire growth process, nano wire, the position of substrate and electron beam.D () is top view corresponding in nanowire growth process.Electron beam moving direction is from left to right.
Fig. 8: use the present invention at the schematic diagram of a substrate flatness point grow nanowire on the surface.Wherein: E is substrate, F is the growing point of the protrusion of deposit, and B is electron beam, and A is the nano wire grown.The position of substrate and electron beam during (a) initial growth state; (b) in nanowire growth process, nano wire, the position of substrate and electron beam.
Detailed description of the invention
When electron beam irradiation is at material surface and when causing EBID, the intensity distribution in the deposit of material and electron beam irradiation region is closely related.In the present invention, material can start deposit and progressively extend to electron beam center at the edge of electron beam.Due to the intensity distribution feature (as shown in Figure 1) of electron beam spot, in this process, grow up (as shown in Figure 2) gradually in the region of deposition materials.If electron beam is moved in the process, then the deposit place of material can be followed the movement of electron beam and move.By the intensity distribution of conservative control electron beam, the kind of EBID gas and concentration, the size of vacuum, translational speed and direction etc. the technological parameter of electron beam can realize dissimilar, size, the preparation of the nano-material of shape.Process based on this " edge deposit " principle does not need the electron beam focused on through precise hard_drawn tuhes, only uses wide-beam electronic bundle.
Embodiment 1:
Prepare a method for nano wire, concrete steps are as follows:
(1) by needing the substrate of grow nanowire to put into vacuum chamber, vacuumizing, controlling pressure in vacuum tank 10
-5pa, passes into the volatile organism of trace, and heating makes it slowly volatilize in vacuum chamber, and it is 10 that source of the gas stablizes the indoor pressure of final vacuum
-4pa;
(2) unlocking electronic bundle, regulates the focus state of electron beam, makes the mean intensity of electron beam in beam spot diameter, be 10
4e/nm
2/ s, bundle spot size is 300 nanometers.And regulate the intensity distribution situation at electron beam edge, make intensity have uneven distribution along edge, namely have a comparatively precipitous Strength Changes edge, it is greater than 10 from bundle spot edge along the spatial variations rate in beam spot diameter, direction
3e/nm
2/ s/100nm; Wherein the size of electron beam spot significantly should be greater than the diameter of the nano wire of required preparation, generally gets the 2-1000 of the nanowire diameter of required preparation doubly.Generally speaking, as long as electron beam spot has the edge of a Strength Changes, the spatial variations rate from bundle spot edge along beam spot diameter, direction is greater than 10
2e/nm
2/ s/100nm, the present invention can implement.
(3) the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material, as shown in Figure 7, when being the edges of substrate of thickness below 500 nanometers when needing the substrate location of growing nano wire material, by the bundle spot edge of electron beam and the EDGE CONTACT of substrate, grow nanostructured, afterwards with certain speed mobile electron bundle (moving substrate also can reach identical effect, only needs final relative movement as shown in Figure 3).As shown in Figure 8, when the substrate location needing growing nano wire material is a point on flat surfaces, first at the growing point that this some place's deposit is protruded, afterwards the bundle spot edge of electron beam is contacted with the growing point of described protrusion, grow nanostructured, afterwards with certain speed mobile electron bundle.The preparation method of described growing point is: use semiconductor technology to prepare a bulge-structure, or uses the method for inclination substrate to use e-beam induced deposition to prepare a bulge-structure needing the substrate location of growing nano wire material.
That is: distinguish to some extent at little pointed edge with in the growth of large flat surfaces.This can grow along the moving direction of electron beam because principle of the present invention determines nano wire.And except the growing point of nano wire in the region of electron beam irradiation, there is not deposition of materials in other places.Otherwise other shapes can be grown to serve as, also the principle of discontented foot breadth Shu Shengchang minor diameter nano wire.
In electron beam moving process, by controlling its translational speed and focal position makes the edge of electron beam spot be positioned at the tip of grown nano wire; Also the growth top of nano wire is namely kept to extend along with the edge of electron beam; The speed of electron beam movement is the speed of nanowire growth.
The decision method of the speed v of described electron beam movement is as follows:
Obtain the deposition rate z of source of the gas under electron beam by experiment, the diameter D of nano wire and electron beam movement speed v linear correlation:
wherein, L is the length that nano wire grows within the t time, and it is v=L/t with the pass of electron beam movement speed v, so
namely, when deposition rate z and the nanowire diameter D that need prepare are certain, electron beam movement speed v can be obtained;
Wherein: the decision method of deposition rate z is as follows: assuming that electron beam intensity is x (electron number/unit are/unit interval), partial pressure is expressed as y (molecular number/unit volume), the deposition rate of gas under electron beam during specified temp is z (unit volume/unit interval), and electron beam translational speed is v (unit distance/unit interval).Generally speaking, under uniform temperature and barometric information, for specific gas material, deposition rate is relevant to electron beam intensity and partial pressure.Can be assumed to be z=f (x, y), wherein, function f needs to be determined by concrete experiment.And electron beam intensity is higher, partial pressure is larger, and the speed of deposit is larger, and in any case speed can reach capacity namely no longer with electron beam intensity and partial pressure increase and increase.
In the present embodiment: obtaining the deposition rate z of source of the gas under electron beam is by experiment 13000nm
2/ min, the nanowire diameter D that need prepare are 40nm, then electron beam movement speed v is about 10nm/min.It should be noted that, under uniform temperature and barometric information, for specific gas material, and electron beam intensity and partial pressure certain when, deposition rate z immobilizes, and now only need adjust electron beam translational speed, can obtain the nano wire of different-diameter.When electron beam intensity and partial pressure change, deposition rate changes, and during experiment, first need calculate the deposition rate of used source of the gas under electron beam, then the nanowire diameter prepared as required, determines electron beam translational speed.
(4) close electron beam after terminating the growth of nano wire, obtaining diameter is the nano thread structure of about 40nm, as shown in Figure 5.Achieve and use wide-beam electronic Shu Jiagong to prepare small size nano wire.
Further, step (1) described source of the gas is organic gas, for growing carbon nanocoils; Or metallic compound, for growing metal nano wire.Such as: the material of described source gas is: acrylic acid, PEG, diallyl dimethyl ammoniumchloride, Fe (CO)
5, W (CO)
6, WF
6, Pt (PF
3)
4, D
2gaN
3or (CH
3)
3cH
3c
5h
4pt.
Embodiment 2:
As shown in Figure 6, a kind of method preparing nano wire, concrete steps as described in Example 1, but in electron beam moving process, in position stop or change the relative movement direction of electron beam and substrate, the former can produce bamboo knot shaped structure, and the latter produces bending carbon nanocoils, and the uneven meeting of translational speed makes nano wire there is different diameters.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these change and convert the protection domain that all should belong to claims of the present invention.
Claims (6)
1. prepare a method for nano wire, it is characterized in that: concrete steps are as follows:
(1) by needing the substrate of grow nanowire to put into vacuum chamber, vacuumizing, controlling pressure in vacuum tank 10
-3-10
-6pa, passes into source of the gas, and controlling to pass into the indoor pressure of source of the gas final vacuum is 10
-1-10
-4pa;
(2) unlocking electronic bundle after source of the gas is stable, regulate the focus state of electron beam, make electron beam in beam spot diameter, the mean intensity of electron beam is greater than 10
2e/nm
2/ s; And regulate the intensity distribution situation at electron beam edge, make intensity have uneven distribution along edge, namely it is greater than 10 from bundle spot edge along the spatial variations rate in beam spot diameter, direction
2e/nm
2/ s/100nm; The diameter of electron beam spot is 2-1000 times of the nanowire diameter of required preparation;
(3) the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material, point cantact between described substrate location and bundle spot edge, and contact point grows nanostructured after contact at once, afterwards with certain speed counter substrate mobile electron bundle, in moving process, by controlling its translational speed and focal position makes the edge of electron beam spot be positioned at the tip of the nanostructured newly grown all the time, form nano wire; Also the growth top of nano wire is namely kept to extend along with the edge of electron beam; The speed of electron beam counter substrate movement is the speed of nanowire growth;
The decision method of the speed v of described electron beam counter substrate movement is as follows:
Obtain the deposition rate z of source of the gas under step (2) described electron beam in step (1) by experiment, the diameter D of nano wire and electron beam counter substrate movement speed v linear correlation:
wherein, L is the length that nano wire grows within the t time, and it is v=L/t with the pass of electron beam counter substrate movement speed v, so
namely, when deposition rate z and the nanowire diameter D that need prepare are certain, electron beam movement speed v can be obtained;
(4) close electron beam after terminating the growth of nano wire, obtain the nano thread structure of required preparation.
2. a kind of method preparing nano wire according to claim 1, is characterized in that: described in step (3), the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material; Concrete: when being the edges of substrate of thickness below 500 nanometers when needing the substrate location of growing nano wire material, by the bundle spot edge of electron beam and the EDGE CONTACT of substrate, other end does not all contact.
3. a kind of method preparing nano wire according to claim 1, is characterized in that: described in step (3), the bundle spot edge of electron beam is placed in the substrate location needing growing nano wire material; Concrete: when need the substrate location of growing nano wire material be substrate flat surfaces on a some time, first at the growing point that this some place's deposit is protruded, change the relative position of substrate and electron beam afterwards, contacted with the growing point of described protrusion by the bundle spot edge of electron beam, other end does not all contact.
4. a kind of method preparing nano wire according to claim 3, it is characterized in that: the preparation method of described growing point is: use semiconductor technology to prepare a bulge-structure, or use the method for inclination substrate to use e-beam induced deposition to prepare a bulge-structure needing the substrate location of growing nano wire material.
5. a kind of method preparing nano wire according to claim 1, it is characterized in that: in step (3) in electron beam and substrate relative movement thereof, in position stop or change the relative movement direction of electron beam and substrate, the former can produce bamboo knot shaped structure, the latter produces bending carbon nanocoils, and the uneven meeting of translational speed makes nano wire there is different diameters.
6. a kind of method preparing nano wire according to claim 1, is characterized in that: step (1) described source of the gas is organic gas, for growing carbon nanocoils; Or metallic compound, for growing metal nano wire.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113798712A (en) * | 2021-09-06 | 2021-12-17 | 清华大学 | Nano material connection method and super strong nano tube structure |
| CN115448251A (en) * | 2022-09-29 | 2022-12-09 | 中国科学院合肥物质科学研究院 | Nanowire preparation method |
Citations (2)
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|---|---|---|---|---|
| CN102053180A (en) * | 2010-11-26 | 2011-05-11 | 天津大学 | Method for reinforcing lateral rigidity of hanging nanotube device through electron beam induced metal deposition |
| CN103011064A (en) * | 2012-12-25 | 2013-04-03 | 东南大学 | Method for preparing substructure less than 10 nanometers on nanometer material surface |
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2015
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| CN102053180A (en) * | 2010-11-26 | 2011-05-11 | 天津大学 | Method for reinforcing lateral rigidity of hanging nanotube device through electron beam induced metal deposition |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113798712A (en) * | 2021-09-06 | 2021-12-17 | 清华大学 | Nano material connection method and super strong nano tube structure |
| CN115448251A (en) * | 2022-09-29 | 2022-12-09 | 中国科学院合肥物质科学研究院 | Nanowire preparation method |
| CN115448251B (en) * | 2022-09-29 | 2023-12-12 | 中国科学院合肥物质科学研究院 | Nanowire preparation method |
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