CN102173376A - Preparation method for small silicon-based nano hollow array with orderly heights - Google Patents
Preparation method for small silicon-based nano hollow array with orderly heights Download PDFInfo
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- CN102173376A CN102173376A CN2011100456985A CN201110045698A CN102173376A CN 102173376 A CN102173376 A CN 102173376A CN 2011100456985 A CN2011100456985 A CN 2011100456985A CN 201110045698 A CN201110045698 A CN 201110045698A CN 102173376 A CN102173376 A CN 102173376A
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Abstract
The invention relates to a preparation method for a small silicon-based nano hollow array with orderly heights, belonging to the technical field of nano-structure preparation. The preparation method employs large-diameter polystyrene nano-spheres which are self-mounted into a single-layer nano-sphere film serving as masks on a Si substrate. After going through multiple technical procedures such as reaction ion lithography, direct current sputtering metal films, selective corrosion and the like, the mask is converted into a small inverted-pyramidal nano-hollow array, which is a two-dimensional hexagonal dot array. The cycle of the nano-hollow arrays is determined by the diameters initially selected for the polystyrene nano-spheres. The invention is likely to be used in fields of growth of controllable quantum structures, photonic crystal manufacturing, quantum logic operation, magnetic storage media, etc.
Description
Technical field
The invention belongs to the nanostructured preparing technical field, be specifically related to the preparation method of a kind of small size silicon-based nano hole array.
Background technology
In recent years, along with the continuous development and the maturation of various semiconductor integrated techniques, the preparation of semiconductor low-dimension nano material has also obtained tremendous development with sign, and has progressively entered practicability.Semiconductor low-dimensional quantum structure (as quantum dot, quantum wire, Quantum Rings etc.) is owing to having the quantum limitation effect that low spatial dimension and very small dimensions cause, present the physical characteristic of a lot of novelties, become one of the research focus in current low-dimensional nano structure field.Yet utilize the quantum structure of self-assembling technique growth, its spatial distribution, pattern and size etc. generally all is difficult to accurate control, has limited its application in devices field.In order to realize that low-dimensional quantum structure can control growth, the researcher has proposed the multiple method that realizes the quantum structure controllable growth on the substrate with orderly distribution nanometer hole or nano-pore.The common method for preparing ordered nano hole (or nano-pore) structure has electron beam lithography (EBL), focused ion beam technology etching (FIB) and X-ray holographic lithography etc.These methods are at first accurately to etch the nano-scale mask on the substrate of photoresist scribbling, and utilize lithographic technique then, etch structures such as nanometer hole or nano-pore.This class ordered nano-structure preparation method's advantage is the accuracy height, and the size of its spatial distribution and quantum structure etc. all is easy to accurate control.But its apparatus expensive, the technology complexity, the production cost height is also introduced defective easily after the etching.
Utilize the nanosphere self-assembling technique to prepare the nano material preparation technology that orderly graphic array is a kind of low-cost high production.Early stage work mainly is exploration prepares the ordered nano-structure array in semiconductor or metal surface method.Along with the development of this technology, people utilize the ordered nano ball array to prepare magnetic ordered nano particle film, ordered nano line etc., and have found their new physical characteristic.These new materials with ordered nano-structure have obtained application in fields such as feds, infrared photon crystal, phase transition storage and solar cells, have shown their important use and have been worth.The relevant report that utilizes pipe/polyhenylethylene nano ball self-assembling technique to prepare nanometer hole starts from 2009.But the nanometer hole size that reaches described in this report is bigger, and uncontrollable.This is unfavorable for the research to its Quantum Properties.The method for preparing nanometer hole that this invention proposed can be regulated and control the cycle and the size of nanometer hole simultaneously.Prepared nanometer hole is arranged high-sequential, and size only is a tens nanometer.With this nanometer hole can make the extremely small quantum structure of size.This explores new physical characteristic for their quantum effect of research, and it will be very favourable improving using value.
Summary of the invention
The purpose of this invention is to provide a kind of method of using the small size silicon-based nano hole array of the preparation high-sequential that equipment is simple, technological operation convenient, cost of manufacture is cheap.
The method of the small size silicon-based nano hole array of the preparation high-sequential that the present invention proposes, be to utilize the self-assembling technique of major diameter pipe/polyhenylethylene nano ball on silicon substrate, through multiple etching, sputter, technologies such as selective corrosion are prepared the nanometer hole array on monocrystalline substrate.The equipment that uses mainly contains culture dish, the syringe of 20 microlitre capacity, slide, and the concrete steps of preparation are:
1, will lie against the culture dish bottom through the silicon substrate that cleans, being positioned in the culture dish with certain angle of inclination through the slide that cleans, the downside of slide is seen shown in Figure 2 facing to silicon substrate; In culture dish, inject deionized water.
2, utilize self-assembling technique, cover individual layer pipe/polyhenylethylene nano ball in surface of silicon.Its method is as follows: with methanol solution and diameter is that (pipe/polyhenylethylene nano ball latex suspension is for buying gained from commercial company, and the nanosphere density of particle is 1.05g/cm for the pipe/polyhenylethylene nano ball latex suspension of 400-800nm
3, particle concentration is 10% solids by weight in the latex suspension) evenly mix according to the ratio of volume ratio 1:1; Drop on the slide with the pipe/polyhenylethylene nano ball methyl alcohol mixed solution of syringe then, allow this solution slowly flow in the water the 4-6 microlitre; After 4-6 minute, deionized water is slowly extracted out with syringe.At this moment, on silicon substrate, promptly obtain the individual layer pipe/polyhenylethylene nano ball film (consulting Fig. 3) that two-dimentional hexagonal lattice is arranged.
3, surface coverage there is the sample of pipe/polyhenylethylene nano ball carry out the reactive ion etching processing to reduce the size of nanosphere.The remaining size of pipe/polyhenylethylene nano ball after the etching is by the size decision of the nanometer hole of desire preparation.Its method is as follows: utilize reactive ion etching (RIE) technology, carry out etching in oxygen atmosphere.Oxygen during etching is pressed and is 9-10Pa, and oxygen gas flow rate is 20-40sccm, uses power to be 25-35W; After the etching, make the pipe/polyhenylethylene nano structure be class taper (consulting Fig. 4).Etch period is by the remaining size decision of desired pipe/polyhenylethylene nano ball.
4, deposit last layer gold film on the pipe/polyhenylethylene nano ball sample surfaces after the etching.Its method is as follows: use the d.c. sputtering technology, at sample surfaces sputter last layer gold film.The operating voltage of d.c. sputtering is 900V-1000V, and sputtering current is 35-45mA, and working gas is an argon gas, and the ar pressure during sputter remains on 10
-3About Torr (as 10
-3--200～10
-3+ 200Torr).Sputtering time is 1-2 minute.The golden film thickness that is deposited on sample surfaces after the sputter is 1-3nm.
5, the pipe/polyhenylethylene nano ball on the sample surfaces of the rapid preparation of removal previous step.Its method is as follows: sample is put into organic solvent tetrahydrofuran (C
4H
8O) in the solution, and do ultrasonic processing.Ultrasonic time 15-25 minute, polystyrene film is dissolved in the organic solvent.Then, sample is placed the ultrasonic processing of ethanol 2--4 minute.Use deionized water rinsing at last, dry.The pipe/polyhenylethylene nano ball of sample surfaces and the golden film on these nanospheres all are removed after this handles.The golden film that is covered in sample surfaces is network structure.Pipe/polyhenylethylene nano ball after mesh size and the etching is measure-alike.
6, the sample to the rapid preparation of previous step carries out selective etching.Its method is as follows: it is the KOH solution of 15-25% that sample is placed weight concentration.The net metal film that utilizes sample surfaces is as mask, under 25-35 ℃ of temperature, and ultrasonic processing 2-5 minute.Silicon in the etching off mesh.Because KOH solution is for the corrosion rate difference of silicon at different crystal orientations, thereby obtain the nanometer hole of inverted pyramid shape.
7, remove the golden film of the sample surfaces of the rapid preparation of previous step.Its method is as follows: it is KI:I that sample is placed on proportioning
2: H
2O=(8-12) g:(2-3) the interior ultrasonic processing of g:100ml corrosive liquid is 25-35 minute.Ultrasonic processing back continues to soak 9-11 hour.Sample is used deionized water rinsing after taking out.Promptly obtain having the small size nanometer hole array of arranging by two-dimentional hexagonal lattice.Nanometer hole is inverted pyramid shape structure.Nanometer hole is arranged high-sequential (consulting Fig. 5) on a large scale.
Among the present invention, the program of described cleaning silicon substrate is as follows: deionized water rinsing 1-3 minute, and the ultrasonic 3-7 of acetone minute, the ultrasonic 4-6 of methyl alcohol minute.Deionized water rinsing 4-6 minute.At H
2SO
4: H
2O
2After boiling 6-4 minute in the=2:1 solution, continue to soak 6-4 minute.Deionized water rinsing 2-4 minute.Then at HF:H
2Flood 40-80 second in the O=1:9 solution, to remove oxide layer.Use deionized water rinsing 50-80 after second at last, dry with getting rid of the sheet machine.
Among the present invention, the program of described cleaning slide is: deionized water rinsing 1-3 minute, and the ultrasonic 4-6 of acetone minute, the ultrasonic 4-6 of methyl alcohol minute, deionized water rinsing 4-6 minute.Then at H
2SO
4: H
2O
2After boiling 4-6 minute in the=2:1 solution, continue to soak 6-4 minute.After using deionized water rinsing 2-4 minute at last, oven dry.
Characteristics of the present invention are as follows:
1. made nanometer hole array sizes is little, and it arranges high-sequential, the controlling cycle system of array in the large tracts of land scope.
2. the technology easy operating control of preparation nanometer hole array, and with the process compatible of traditional silicon-based devices.
3. can on the large tracts of land substrate, make, produce in batches.
4. the equipment price and the cost of manufacture of development use are all very cheap.
The ordered nano hole array of the present invention's preparation is applicable to the growth of controlled amounts minor structure, can be widely used in fields such as photonic crystal manufacturing, quantum logic computing and magnetic medium storage.
Description of drawings
Fig. 1. the main technique flow chart of preparation nanometer hole array.
Fig. 2. the pipe/polyhenylethylene nano ball is carried out the experimental provision that self assembly is arranged on silicon substrate.
Fig. 3. be covered in the atomic force microscope images of the pipe/polyhenylethylene nano ball on the silicon substrate film.The upper right corner is the nanosphere image that amplifies.
Atomic force microscope images on Fig. 4 silicon substrate after the pipe/polyhenylethylene nano ball warp RIE etching.The upper right corner is nanosphere enlarged image after etching.
Fig. 5. utilize the atomic force microscope images of the prepared nanometer hole array of this invention.Nanometer hole is the inverted pyramid shape, arranges by two-dimentional hexagonal lattice.The upper right corner is the nanometer hole image that amplifies.
Number in the figure:
Culture dish,
The syringe of capacity 20 μ L,
Slide,
Silicon substrate,
Deionized water.
The specific embodiment
1, substrate is Si (a 001) single-chip.Carry out following cleaning: deionized water rinsing 2 minutes, ultrasonic 5 minutes of acetone, ultrasonic 5 minutes of methyl alcohol.Deionized water rinsing 5 minutes.At H
2SO
4: H
2O
2After=2:1 solution boils 5 minutes, continue to soak 5 minutes.Using deionized water rinsing after 3 minutes, being placed on proportioning is HF:H
2Dipping is 60 seconds in the O=1:9 solution, to remove the oxide layer of silicon chip surface.Use deionized water rinsing after 60 seconds at last, dry with getting rid of the sheet machine.
2,, set up device as Fig. 2 for to cover individual layer pipe/polyhenylethylene nano ball on the silicon substrate.The culture dish material is a polystyrene.Be of a size of 100mm * 20mm.
3, slide used in the device shown in Figure 2 is made cleaning by following program: deionized water rinsing 2 minutes, ultrasonic 5 minutes of acetone, ultrasonic 5 minutes of methyl alcohol, deionized water rinsing 5 minutes.At H
2SO
4: H
2O
2After boiling 5 minutes in the=2:1 solution, continue to soak 5 minutes.Use deionized water rinsing after 3 minutes at last, oven dry.
4, according to position of sound production shown in Figure 2 wherein with the silicon chip that cleans up and slide.Inject the 50ml deionized water then.
5, deposit individual layer pipe/polyhenylethylene nano ball on silicon substrate.Process is as follows: with methanol solution and diameter is that (pipe/polyhenylethylene nano ball latex suspension is from good (the Duke China Scientific of high molecular particle Science and Technology Ltd. of Du You for the pipe/polyhenylethylene nano ball latex suspension of 430nm, Inc.) buy, product type is 5043A) evenly mix according to the ratio of volume ratio 1:1.Then as shown in Figure 2, with the syringe of one 20 microlitre,, and allow this solution slowly flow in the water at the pipe/polyhenylethylene nano ball methanol solution that drips 5 microlitres on the slide.After 5 minutes, water is slowly extracted out with syringe.At this moment, will be coated with the individual layer nanosphere film that two-dimentional hexagonal lattice is arranged on Si (001) substrate, the cycle of nanosphere dot matrix is that 430nm(consults Fig. 3).Pipe/polyhenylethylene nano bulb diameter wherein can be selected arbitrarily in 400-800nm.
6,, adopt the dry plasma etch technology to reduce the size of pipe/polyhenylethylene nano ball with the Si substrate that is coated with individual layer pipe/polyhenylethylene nano ball film of step 5 preparation.Technology is as follows: sample is put into the vacuum chamber of reactive ion etching equipment (model SAMCO 10-NR), carry out etching in oxygen atmosphere.Oxygen during etching is pressed and is 10Pa, and oxygen gas flow rate is 30sccm.Etching power is 30W, and etch period is 10 minutes and 40 seconds.After finishing, etching obtains cone-shaped pipe/polyhenylethylene nano structure.(consulting Fig. 4).
7, on the sample surfaces of 6 preparations set by step, utilize sputtering technology deposit last layer gold film.Technology is as follows: use the d.c. sputtering technology, at sample surfaces sputter last layer gold film.The d.c. sputtering platform model of using is Lecia EM SCD-005.The operating voltage of sputter is 1000V, and sputtering current is 40mA, and working gas is an argon gas, and the Ar Pressure during sputter remains on 10
-3About Torr.Sputtering time is 1 minute.The golden film thickness of sample surfaces deposit is 2nm after the sputter.
8, the pipe/polyhenylethylene nano ball film on the sample of removing step 7 preparation.Process is as follows: with the tetrahydrofuran solution that places of the sample of Au film in the sputter, do ultrasonic processing 20 minutes.Then, place the ultrasonic processing of ethanol 3 minutes.Use deionized water rinsing after 3 minutes at last, dry.After this handled, the pipe/polyhenylethylene nano ball of sample surfaces and the golden film above the nanosphere were all removed fully, have only stayed netted golden film on the surface.Pipe/polyhenylethylene nano ball after mesh size and the etching is measure-alike.
9. use mesh gold film as mask, the sample with step 8 preparation etches nanometer hole.Technology is as follows: it is that 20% the KOH aqueous solution carries out selective corrosion that sample is placed concentration.To place temperature be 30 ℃ water bath with thermostatic control to container during corrosion.Etching time is 4 minutes.After corrosion finishes, take out sample., dry after 3 minutes with deionized water rinsing.Because KOH solution is for the corrosion rate difference of silicon at different crystal orientations, thereby the nanometer hole that is corroded into inverted pyramid shape of the silicon in the mesh of golden film.
10, remove the golden film of the sample surfaces of step 9 preparation.Technology is as follows: it is KI:I that sample is placed proportioning
2: in the solution of H2O=10g:2.5g:100ml, ultrasonic processing 30 minutes.After ultrasonic the disposing, in original solution, continue to soak 10 hours.Take out sample, after 3 minutes, dry with deionized water rinsing.Promptly on Si (001) substrate, obtain the nanometer hole array that two-dimentional hexagonal lattice is arranged.Its arrangement cycle is 430nm.Nanometer hole is inverted pyramid shape structure.The length of side of nanometer hole bottom surface is between 75nm-85nm.The degree of depth is between 55nm-65nm.As shown in Figure 5.
Claims (3)
1. the small size silicon-based nano of high-sequential is cheated the preparation method of array, it is characterized in that concrete steps are:
(1) will lie against the culture dish bottom through the silicon substrate that cleans, being positioned in the culture dish with certain angle of inclination through the slide that cleans, the downside of slide is facing to silicon substrate; In culture dish, inject deionized water;
(2) utilize self-assembling technique, cover individual layer pipe/polyhenylethylene nano ball in surface of silicon, its method is as follows: with methanol solution and diameter is that the pipe/polyhenylethylene nano ball latex suspension of 400-800nm evenly mixes according to the ratio of volume ratio 1:1, wherein, the nanosphere density of particle is 1.05g/cm in the described pipe/polyhenylethylene nano ball latex suspension
3, the particulate weight concentration is 10% in the latex suspension; Drop on the slide with the pipe/polyhenylethylene nano ball methyl alcohol mixed solution of syringe then, allow this solution slowly flow in the water the 4-6 microlitre; After 4-6 minute, deionized water is slowly extracted out with syringe; At this moment, on silicon substrate, promptly obtain the individual layer pipe/polyhenylethylene nano ball film that two-dimentional hexagonal lattice is arranged;
(3) surface coverage there is the sample of pipe/polyhenylethylene nano ball carry out the reactive ion etching processing to reduce the size of nanosphere, its method is as follows: utilize reactive ion etching technology, in oxygen atmosphere, carry out etching, oxygen during etching is pressed and is 9-10Pa, oxygen gas flow rate is 20-40sccm, uses power to be 25-35W; After the etching, make the pipe/polyhenylethylene nano structure be the class taper;
(4) deposit last layer gold film on the pipe/polyhenylethylene nano ball sample surfaces after the etching, its method is as follows: use the d.c. sputtering technology, at sample surfaces sputter last layer gold film; The operating voltage of d.c. sputtering is 900V-1000V, and sputtering current is 35-45mA, and working gas is an argon gas, and the Ar Pressure during sputter remains on 10
-3--200～10
-3+ 200Torr, sputtering time are 1-2 minute; The golden film thickness that is deposited on sample surfaces after the sputter is 1-3nm;
(5) the pipe/polyhenylethylene nano ball on the sample surfaces of the rapid preparation of removal previous step, its method is as follows: sample is put into organic solvent tetrahydrofuran solution, and do ultrasonic processing, ultrasonic time 15-25 minute, polystyrene film is dissolved in the organic solvent, then, sample is placed the ultrasonic processing of ethanol 2--4 minute; Use deionized water rinsing at last, dry; The pipe/polyhenylethylene nano ball of sample surfaces and the golden film on these nanospheres all are removed after this handles, and the golden film that is covered in sample surfaces is network structure;
(6) sample to the rapid preparation of previous step carries out selective etching, its method is as follows: it is the KOH solution of 15-25% that sample is placed weight concentration, the netted golden film that utilizes sample surfaces is as mask, under 25-35 ℃ of temperature, ultrasonic processing 2-5 minute, silicon in the etching off mesh obtains the nanometer hole of inverted pyramid shape;
(7) remove the previous step golden film of the sample surfaces of preparation suddenly, its method is as follows: it is KI:I that sample is placed on proportioning
2: H
2O=(8-12) g:(2-3) the interior ultrasonic processing of g:100ml corrosive liquid is 25-35 minute, and ultrasonic processing back continues to soak 9-11 hour, and sample is used deionized water rinsing after taking out, and promptly obtains having the small size nanometer hole array by two-dimentional hexagonal lattice arrangement.
2. preparation method according to claim 1, the program that it is characterized in that cleaning silicon substrate is as follows: deionized water rinsing 1-3 minute, the ultrasonic 3-7 of acetone minute, the ultrasonic 4-6 of methyl alcohol minute; Deionized water rinsing 4-6 minute; At H
2SO
4: H
2O
2After boiling 6-4 minute in the=2:1 solution, continue to soak 6-4 minute; Deionized water rinsing 2-4 minute, then at HF:H
2Flood 40-80 second in the O=1:9 solution, to remove oxide layer; Use deionized water rinsing 50-80 after second at last, dry with getting rid of the sheet machine.
3. preparation method according to claim 1 is characterized in that the program of cleaning slide is: deionized water rinsing 1-3 minute, and the ultrasonic 4-6 of acetone minute, the ultrasonic 4-6 of methyl alcohol minute, deionized water rinsing 4-6 minute; Then at H
2SO
4: H
2O
2After boiling 4-6 minute in the=2:1 solution, continue to soak 6-4 minute; After using deionized water rinsing 2-4 minute at last, oven dry.
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