CN102107847B - Method for preparing three-dimensional micro-nano device - Google Patents
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- CN102107847B CN102107847B CN 200910243010 CN200910243010A CN102107847B CN 102107847 B CN102107847 B CN 102107847B CN 200910243010 CN200910243010 CN 200910243010 CN 200910243010 A CN200910243010 A CN 200910243010A CN 102107847 B CN102107847 B CN 102107847B
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Abstract
The invention discloses a method for preparing a three-dimensional micro-nano device, and relates to the technology of three-dimensional micro-nano devices. The method comprises the following steps of: (1) sample placement and fixation; (2) graphic observation of stick-up micro-nano materials; (3) growth of electrode contact blocks and/or connecting wires in a substrate plane; (4) preparation of three-dimensional electrode contact blocks and connecting wires; (5) removal of residual deposits on the substrate; (6) obtainment of a finished product. The advantages of the invention are that: the process is simple; the device is accurate; micro-nano electrodes and three-dimensional wiring are formed directly and accurately at the free end of the stick-up micro-nano material; the preparation of a real three-dimensional device is realized; and a new process approach is provided to the multifunctional hybrid integration of micro-nano devices.
Description
Technical field
The present invention relates to the three-dimensional micro-nano device technical field, it is the preparation method of stick-up, three-dimensional micro-nano structure, the growth function that is particularly related to a kind of three-dimensional micro-nano structure based on FIB (FIB) is made electrode contact and the distribution that is not positioned in the support substrates plane, forms the form an angle method of mobile three-dimensional micro-nano device of electric current and support substrates plane.
Background technology
Development experience in the past few decades shows, the integrated development of microelectronic device will soon reach physics and/or the limit economically.Nano electron device is the solid electronic device of future generation after microelectronic component, the quantum effect that its main thought is based on nano-functional material designs and prepares the nanometer quantum device, to reach integrated circuit is further reduced, and substitute the ultimate aim of traditional silicon device.In order to break through the limit of traditional microelectronics integrated technique, a large amount of researchers has dropped into increasing manpower and materials and has studied new material, advanced technology and new unit type.One dimension/quasi-one-dimensional nanometer material owing to its unique physical characteristic with and application on the nano-devices such as electronics, photon and bio-sensing receive much concern.Along with the development of size of electronic devices towards small scale, low-dimensional direction, researchers constantly synthesize the three-dimensional nanometer material of the stick-up of the abundant ordered arrangement of pattern.Be fixed on substrate surface for an end, the nanometer entity that the other end freely stretches, such as nano wire, nanotube, how nanometer rods etc. are directly made electrode in its free extended end and are still a technical barrier that needs to be resolved hurrily.Technique based on traditional photoetching technique or electron beam lithography can't address this problem at all.
The material that is not positioned at substrate plane is carried out the characteristic tests such as electricity, common processing method is as follows: at first material is separated from substrate, this comprises that the scraping of nanometer entity is collected, liquid phase is disperseed, the steps such as surface transfer, referring to document " Optical and electrical properties ofZnO nanowires grown on aluminium foil by non-catalytic thermalevaporation ". " Nanotechnology " .2007, Vol.18:175606.In this article, the ZnO nano-wire that at first will grow on the substrate is scraped from substrate through blade, then puts into ethanolic solution and carries out the ultrasonic agglomerate nano wire family separation that makes, and gets afterwards dispersion liquid a small amount of, drips to the substrate surface with insulating thin layer; The method of electron beam exposure or focused ion beam deposition is then adopted in the making of electrode.The weak point of said method is: 1. use blade that the nano material on the substrate is separated easily nano material is caused mechanical damage, and destroyed its original geometry, especially for multi-arm or other complex-shaped nanostructured; 2. have very large randomness when dispersion liquid is got liquid, not only when seeking the single nano material of disperseing, expend time in, also be difficult to the single nano material of paying close attention to is before carried out testing research.Another can overcome above-mentioned some not enough method is to utilize the etching function of FIB, with the stick-up micro-nano material accurately with substrate separation, make it to be positioned at the support substrates plane, then carry out electrode fabrication.After all, the device of these two kinds of method mades, flowing of electric current all is positioned at substrate plane, be a kind of indirectly, the processing method of planar device, changed luv space structure and the position of material, the raising of integrated level is had larger limitation.
Summary of the invention
The object of the invention is to overcome the defective that exists in the prior art, a kind of method for preparing three-dimensional micro-nano device is provided, directly the free end at the stick-up micro-nano material forms micro-nano electrode and three-dimensional wiring accurately, realize the making of three-dimension device truly, new technique approach is provided for the multi-functional mixing of micro-nano device is integrated.
For achieving the above object, technical solution of the present invention is:
A kind of method for preparing three-dimensional micro-nano device, it comprises the following steps:
(1) sample is placed with fixing:
(i) if substrate is the conductive substrates with surface insulation thin layer, be fixed on the sample carrier from substrate back with conductive materials;
(ii) if substrate is to have at the bottom of the electrically insulating substrate of surface conductance layer, after being fixed on sample on the sample carrier, with conductive materials sample surfaces being connected with sample carrier again. the sample that will be fixed on the sample carrier is put on the sample stage of two-beam SEM/FIB or single bundle FIB cavity, then sample stage is carried out the inclination of certain angle, made FIB perpendicular to substrate incident;
(2) figure of the three-D micro-nano material of stick-up observation:
The mobile example platform carries out figure observation with SEM or low line ion current, finds the stick-up micro-nano material and the free-ended position thereof that need to form electrode contact, and measures its size;
(3) growth of electrode contact piece and/or line in the substrate plane:
A) before growth stick-up micro-nano material material, adopt traditional photoetching, electron beam exposure or focused ion beam deposition method to form substrate plane interior large electrode contact block and line;
B) for the front situation without any electrode contact of stick-up micro-nano material growth, according to the position of material, adopt FIB, growth in situ electrode contact piece and contact conductor;
(4) making of three-diemsnional electrode contact and line:
The stick-up micro-nano material is formed three-diemsnional electrode contact and line;
(5) removing of residual deposits on the substrate:
With sample stage certain angle that tilts, make ion beam with certain angle side direction incident, make step 4) in processing three-dimensional structure under fully in the unscreened FIB of the being exposed to visual field; Then set scanning area, the residual deposits of three-dimensional structure below is removed;
(6) get finished product.
The described method for preparing three-dimensional micro-nano device, the a) step in its described step (3), when distant between the free-ended projection of stick-up micro-nano material and contact block, need the Distance Shortened that a connecting line will be between the two of growing with FIB, comprise step: (i) obtain stick-up micro-nano material to be processed and the FIB image of electrode contact piece; (ii) the connecting line figure that utilizes the pattern generator Software Create of equipment to process is determined its position; (iii) introduce metallorganic gaseous molecular source; (iv) open FIB scanning plated metal line, an end of line should be close with the free end projection of stick-up micro-nano material, and the other end connects large electrode contact piece.
The described method for preparing three-dimensional micro-nano device, the b in its described step (3)) step, comprise step: (i) obtain stick-up micro-nano material to be processed and the FIB image of electrode contact piece; (ii) the connecting line figure that utilizes the pattern generator Software Create of equipment to process is determined its position; (iii) introduce metallorganic gaseous molecular source; (iv) open FIB scanning, growth in situ electrode contact piece and contact conductor.
The described method for preparing three-dimensional micro-nano device, its described step (4) realizes respectively by the following method:
(iv) electrostatic displacemen method, set a specific scanning area after, introduce metallorganic gaseous molecular source, beginning FIB scanning and adopt the static bias voltage to ion beam with the continuous yaw displacement of certain speed with the acquisition three-dimensional structure;
(v) graph scanning method is by sweep time and the regional continuous three-dimensional structure of growing of device program control ion-beam scanning;
(vi) accurate Quality control platform displacement method, the continuous moving by sample stage changes the relative position that ion beam scans at substrate, to form three-dimensional structure.
The described method for preparing three-dimensional micro-nano device, its described step (ii), the figure series of utilizing the pattern generator Software Create of equipment to process, according to the growth rate under the particular growth condition, accurately set the overlap coefficient in last graph scanning zone and rear one scan zone in succession and obtain continuous three-dimensional structure sweep time.
The described method for preparing three-dimensional micro-nano device, (i) electrostatic displacemen method of its described step (4) comprises step:
(a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) its position is determined with big or small in the single ion-beam scanning of the pattern generator Software Create graphics field that utilizes equipment; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning, and with certain speed ion beam is carried out yaw displacement, until the 3-dimensional metal line of deposition and the upper end in contact of stick-up micro-nano material;
(ii) graph scanning method comprises step: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) utilize the pattern generator Software Create ion-beam scanning graphical set of equipment, determine particular location and the sweep time of each figure; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning growing three-dimensional structure, form electrode contact;
(iii) accurate Quality control platform displacement method, the manufacturing process of three-diemsnional electrode contact comprises step: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) its position is determined with big or small in the single ion-beam scanning of the pattern generator Software Create graphics field that utilizes equipment; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning, by the mobile growing three-dimensional contact structures of sample stage.
The described method for preparing three-dimensional micro-nano device, it is described when utilizing the metal deposition function of FIB to make electrode, freely upholds the growth of the direct-connected connecting line of end with material, and line≤20pA is hanged down in employing.
The described method for preparing three-dimensional micro-nano device in its described step (5), to the residual deposits around the three-dimensional structure, adopts vertically or other incident angle removal residual deposits; When utilizing FIB that residual deposits is removed, line is that pA is to the nA magnitude.
The described method for preparing three-dimensional micro-nano device, its described sample not only is the single nanostructured of nanometer rods, nanotube or nano wire, also comprises the three-dimensional micro-nano structure of free extended end unobstructed stick-up on the locus; Material can be the assembly of metal, semiconductor, organic matter, heterocomplex, dielectric material or different materials, but the charge accumulated that its electric conductivity will can avoid ion-beam scanning to cause; Between the free extended end of three-dimensional material and substrate plane certain angle of inclination is arranged, the span of this angle is between 0 °＜φ≤90 °.
The described method for preparing three-dimensional micro-nano device, its described metallorganic gaseous molecular source can be mixture single or various metals organic matter gaseous molecular source, and the three-dimensional structure that requires to generate is conducted electricity.
The inventive method and existing an end is fixed on the substrate, the micro-nano material that the other end freely stretches carries out electrode processing method to be compared, and advantage is:
1. the FIB (FIB) of low line deposition is a kind of direct writing technology that breaks away from mask and resist, the graphics resolution that forms can be comparable with the dimension of picture that electron beam exposure is made, more outstanding is FIB can grow electric conductivity preferably, the 3 D complex graphic structure of nanoscale, this technology makes the making of the integrated line of three-dimensional hybrid become possibility.
2. make nano-electrode based on the growth of ion beam chemical gaseous phase three-dimensional material, avoided the space structure of nano material and destruction and the mechanical damage of position, what form is the three-dimension device structure, the area of active area is very little, electric current and substrate surface have a certain degree mobile, are conducive to improve device density.
3. for the three-dimensional material that grows between the electrode contact figure that processes in advance, the formation of electrode contact and device can be in SEM/FIB or single bundle FIB system once property finish, have time and cost advantage; Flexibility, integrality and accuracy to the nano material electrode structure fabrication have further been guaranteed.
4. utilize FIB to the fixed point selective etch function of material, low line etching is combined with the growth phase of material, when effectively removing residual deposits, can also carry out the original position reparation to device or circuit.
Description of drawings
Fig. 1 is in a kind of method for preparing three-dimensional micro-nano device of the present invention, the electrostatic displacemen growth schematic diagram of three-dimensional structure, wherein, substrate 11, ion-beam scanning zone 12, electrostatic displacemen step-length are to be that Δ t, vertical arrow indication are the ion-beam scanning zone in the Δ t time of staying of Δ r, ion beam, lateral arrows indication ion-beam scanning electrostatic displacemen direction, the overhanging portion of three-dimensional structure and the angle of substrate are θ;
Fig. 2 a-c is the SEM side-looking picture that the upper end to perpendicular to the tungsten nanometer rods of substrate growth of the embodiment of the invention 1 forms the nanometer contact: a, perpendicular to the tungsten nanometer rods of substrate growth; B utilizes the upper end of FIB nanometer rods in a to form three-dimensional manometer electrode contact and distribution; C, the FIB etching is removed 3-D nano, structure below residual deposits among the b.Wherein substrate 21, and the Au electrode contact is fast 22, the tungsten connecting line 23 of FIB growth, tungsten nanometer rods 24, the upper end 25 of tungsten nanometer rods; The 3-D nano, structure part 26,27,28,29 of FIB growth, the scanning area 30 of FIB when residual deposits is removed.
Fig. 3 a-d be the embodiment of the invention 2 make the vertical electronic device flow chart at the multi-layer film structure substrate: a, NbN/MgO/NbN/MgO/SiO
2/ Si multi-layer film structure; B utilizes FIB in a growth tungsten nanometer rods; C is to forming the sandwich nano pole structure behind the b dry etching; D, FIB growing three-dimensional structure forms space electrode and distribution, then utilizes the FIB etching to remove residual deposits.Wherein 31 is Si (substrate)/SiO
2(200nm)/the MgO part, 32 and 33 parts are respectively NbN and MgO, 34 is the tungsten nanometer rods, the sandwich nano dot structure comprises 34 belows (32-33-32), the contact of NbN/ (W-Ga-C-O) nanometer is comprised of 32 and 34 of 33 tops, 35 is the three-diemsnional electrode distribution, and 36 is the contact electrode piece.
The specific embodiment
As shown in Figure 1, the method schematic diagram for preparing three-dimensional micro-nano device for the present invention is a kind of, wherein, substrate 11, ion-beam scanning zone 12, electrostatic displacemen step-length are to be that the overhanging portion of Δ t, three-dimensional structure and the angle of substrate are θ the time of staying of Δ r, ion beam.
Method of the present invention comprises step:
(1) sample is placed with fixing
The own micro-nano material of standing can be grown on the different support substrates, type according to support substrates, fixing means is as follows: if (i) substrate is the conductive substrates with surface insulation thin layer, available conductive materials is fixed on the sample carrier from substrate back.(ii) at the bottom of the electrically insulating substrate with surface conductance layer, be fixed on sample on the sample carrier after, with conductive materials sample surfaces is connected with sample carrier again, so that conductive channel to be provided.The sample that will be fixed on the sample carrier is put on two-beam SEM/FIB or the single bundle FIB cavity sample stage, then sample stage is carried out the inclination of certain angle.
(2) figure of stick-up micro-nano material observation:
The mobile example platform carries out figure observation with SEM or low line ion current, finds the stick-up micro-nano material and the free-ended position thereof that need to form electrode contact, measures its size.
(3) growth of electrode contact piece and/or line in the substrate plane:
The making of electrode contact piece and line has two schemes substantially in the substrate plane: one, before growth stick-up micro-nano material, adopt traditional methods such as photoetching, electron beam exposure or focused ion beam deposition to form substrate plane interior large electrode contact block and line.For this substrate that has had large electrode contact block figure and/or line, when distant between the free-ended projection of stick-up micro-nano material and contact block, need the Distance Shortened that a connecting line will be between the two of growing with FIB, process comprises: (i) obtain stick-up micro-nano material to be processed and the FIB image of electrode contact piece; (ii) the connecting line figure that utilizes the pattern generator Software Create of equipment to process is determined its position; (iii) introduce metallorganic gaseous molecular source; (iv) open FIB scanning plated metal line.One end of line should be close with the free end projection of stick-up micro-nano material, and the other end connects large electrode contact piece.The second is for the front situation without any electrode contact of stick-up micro-nano material growth, then according to the position of material, adopt FIB, go on foot growth in situ electrode contact piece and contact conductor by above-mentioned (i)-(ii)-(iii)-(iv).
(4) making of three-diemsnional electrode contact and line:
Adopt the process program of FIB-CVD growth in situ three-dimensional structure substantially to have three kinds: (i) electrostatic displacemen method, after namely setting a specific scanning area, introduce metallorganic gaseous molecular source, beginning FIB scanning and adopt the static bias voltage to ion beam with the continuous yaw displacement of certain speed to obtain three-dimensional structure, the growth schematic diagram is as shown in Figure 1; (ii) graph scanning method, in this method, the sweep time by device program control ion-beam scanning and the zone three-dimensional structure of growing.This method is repeated, controllability is good, but requires high to experimental design.The figure series that need to utilize the pattern generator Software Create of equipment to process, according to the growth rate under the particular growth condition, accurately set the overlap coefficient in last graph scanning zone and rear one scan zone in succession and obtain continuous three-dimensional structure sweep time; (iii) accurate Quality control platform displacement method, namely the continuous moving by sample stage changes ion beam and forms three-dimensional structure at the relative position that substrate scans.The deficiency of the method is the operability that it is relatively poor.
Corresponding with above three kinds of growth patterns, can there be three kinds of methods to come the stick-up micro-nano material is formed electrode contact and line.Corresponding to scheme (i), the manufacturing process of three-diemsnional electrode contact comprises: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) its position is determined with big or small in the single ion-beam scanning of the pattern generator Software Create graphics field that utilizes equipment; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning, and with certain speed ion beam is carried out yaw displacement, until the 3-dimensional metal line of deposition and the upper end in contact of stick-up material.Corresponding to scheme (ii), the manufacturing process of three-diemsnional electrode contact comprises: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) utilize the pattern generator Software Create ion-beam scanning graphical set of equipment, determine particular location and the sweep time of each figure; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning growing three-dimensional structure, form electrode contact.Corresponding to scheme (iii), the manufacturing process of three-diemsnional electrode contact comprises: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) its position is determined with big or small in the single ion-beam scanning of the pattern generator Software Create graphics field that utilizes equipment; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning, by the mobile growing three-dimensional contact structures of sample stage.
The removing of (5) residual deposits on the substrate ((residue deposition))
With sample stage certain angle that tilts, make ion beam with certain angle side direction incident, make step 4) in processing three-dimensional structure under fully in the unscreened FIB of the being exposed to visual field.Then set scanning area, the residual deposits of three-dimensional structure below is removed.To the residual deposits around the three-dimensional structure, can adopt vertically or other incident angle.
Distance affects between the micro-nano material that one end freely stretches and the included angle of substrate and nano material and substrate top electrode contact block the position of three-dimensional structure growth and the angle that growth needs tilts.If apart from too far away, it is good at a distance of 0.5-5 μ m that the connecting line that then needs to grow in advance makes both.Distance is too large, simultaneously the height of space material again hour, required growth angle of inclination and span be very large three-dimensional structure all, this has increased the technology difficulty of three dimensional growth.Distance is too little, then in the process of Material growth, may have deposition to occur at spatial entities, changes in a way its original performance.
When utilizing FIB metal deposition function to make electrode, (≤20pA) growth, other connecting line and electrode contact piece then adopt larger line to finish to hold the suitable employing of growth of direct-connected connecting line to hang down line with the exhibition of freely upholding of stick-up micro-nano material.The residual deposits that produces outside setting surface area that produces owing to factors such as beam profile distribution characteristics (beam profile) and secondary electron scatterings when low line Energy Deposition is well avoided line scanning, serious residual deposits can cause interelectrode short circuit or form extra conductive channel around nano micro-material; Low line can make because Ions Bombardment is down to minimum on the impact of stick-up micro-nano material even is not had simultaneously.Larger line can obtain larger sedimentation rate substantially, thereby saves time.The key of three-dimensional material growth to the velocity of displacement of ion beam, too slow then overhanging portion depart from vertical direction the angle of inclination (90 °-θ) too little, span is little, the time that links to each other with space structure on the technique is longer.In addition, large velocity of displacement can't to highly little, contact with the free extended end formation of the stick-up micro-nano material that the connecting line distance is large on the substrate at all.And too fast velocity of displacement can make the residual deposits on the substrate increase, and increased accordingly the time that residual deposits is removed.
When utilizing FIB that the etching function of material is removed residual deposits, the removing of three-dimensional structure material below can adopt pA to the line of nA magnitude.Large line can increase etching speed, saves time; And low line can reduce the impact on three-dimensional structure.
[embodiment 1]:
Form vertical electrode at the free end perpendicular to the tungsten nanometer rods of substrate, may further comprise the steps:
1) image observation of tungsten nanometer rods.Shown in Fig. 2 a, diameter is that the tungsten nanometer rods (24) of 150nm is positioned at SiO
2(200nm)/left end on tungsten connecting line (23) surface on the Si substrate (21).The Au on the left side (22) contact block is with it at a distance of about 1 μ m.The other end of connecting line links to each other with Au/Cr (50nm/10nm) electrode contact piece on the substrate.This substrate utilization conduction carbon ribbon is fixed on the sample carrier, sends in the SEM/FIB cavity and be fixed on the sample stage.Used system FIB incident direction and horizontal plane angle are 38 °; Open electron gun (5kV beam voltage, the electron beam diaphragm of 30 μ m) and ion gun (30kV ion beam accelerating potential, the ion beam line of 1pA), it is the 5mm place that sample stage is risen to working depth, and the inclination sample stage makes ion beam perpendicular to substrate plane incident; The nanometer rods image is focused on and other parameter adjustment.
2) heating of metal organic matter gaseous molecular source import system (Precursor gas injectionsystem).The metallorganic gaseous molecular source that makes in the present embodiment is W (CO)
6
3) growth of three-dimensional manometer electrode.The growth schematic diagram is seen Fig. 1 (disproportionate among the figure), step is as follows: (i) the nanometer rods graph position determines and dimensional measurement, nanometer rods and electrode connecting line are moved on to field of view center, utilize SEM to measure distance (～1 μ m) between its height (～4.5 μ m) and nanometer rods and left side Au contact block; Then switch to the FIB imaging pattern and collect a FIB image; (ii) growth of root vertical component (such as 26 parts among Fig. 2 b), adopting pattern generator definition size is the ion-beam scanning zone of 80nm * 80nm, and this figure being placed into the edge of the golden contact block that nanometer rods faces, setting sweep time is 30s.The gas conduit in metallorganic gaseous molecular source is drawn as to substrate surface, open the gas conduit valve, select the ion beam line of 1pA and start ion-beam scanning, it highly is about 0.5 μ m; (iii) growth of suspension three-dimensional distribution, these part minute three sections compositions are (such as 27,28 among Fig. 2 b, shown in 29), the angle that 27 parts depart from vertical direction is 7 °, is respectively 3.3 and 0.4 μ m in the growth of Z direction and directions X, and electrostatic displacemen speed and the time of use are respectively 2nms
-1With 4min, the angle that 28 parts depart from vertical direction is 18 °, is respectively 0.6 and 0.2 μ m in the growth of Z direction and directions X, and electrostatic displacemen speed and the time of use are respectively 4nms
-1With 1min; The angle that 29 parts depart from vertical direction is 26 °, is respectively 0.4 and 0.3 μ m in the growth of Z direction and directions X, and electrostatic displacemen speed and the time of use are respectively 6nms
-1With 1min, the three-dimension device structure is seen Fig. 2 b.
4) removal of residual deposits.Sample stage is tilted 45 °, and the angle between FIB and substrate is 7 ° at this moment, then adopts pattern generator to form scanning area shown in the white dashed line (30) among Fig. 2 c, and the line etching of usefulness 5pA 2 minutes is removed residual deposits.
In step 1 of the present invention) in, the included angle of tungsten nanometer rods and substrate only is exemplary, the span that can be used for the φ of the inventive method can be between 0 °＜φ≤90 °; In addition, the tungsten nanometer rods can also be the micro nano structure of other materials and shape.Described nanostructured includes but not limited to the single nanostructured such as nanometer rods, nanotube or nano wire, and described material comprises metal, semiconductor, organic matter, heterocomplex (composite), medium and their assembly.Pt for example, Au, Co, Cu, Ni, Si, GaN, InP, ZnO, C, Pt-W-Ga-C, SiO
2Deng.
Silicon substrate of the present invention only as schematically for example, should be appreciated that for a person skilled in the art, and the stick-up micro-nano material that is used for forming vertical devices can be grown on the different substrates.Therefore, the present invention correspondingly adopts following fixing means according to the type of substrate:
(i) if substrate is the conductive substrates with surface insulation layer, available conductive materials is fixed on the sample carrier from substrate back.Described insulating barrier comprises SiO
2, Si
3N
4, Al
2O
3Or its combination etc., and thickness should make substrate when electron beam ion beam imaging without charge accumulated but can reach the substrate surface electric insulating effect; Described conductive substrates comprises Si, GaAs, GaN, InP or metal etc.; In addition, also can there be the substrate of thin dielectric film to make metal contact pattern and be substrate with it long with ordinary optical photoetching-metal deposition-stripping technology;
(ii) if substrate is the dielectric substrate with surface conductance layer, can be fixed on sample on the sample carrier after, with conductive materials sample surfaces and sample carrier are coupled together again.Wherein, described conductive layer comprises that described metal comprises Au such as the metal conductive oxide of ito thin film or individual layer or multilayer, Ni, Cr, Cu or Al etc.; Described dielectric substrate comprises glass, quartz or sapphire insulation material;
Described conductive materials comprises conductive silver glue, conduction carbon ribbon, copper strips etc.
In step 2 of the present invention) in, employed metallorganic gaseous molecular source also is exemplary, can grow electric conductivity preferably other single presomas of three-dimensional structure or a plurality of precursors combination all can, comprise WF
6, PtC
7H
17, Al (CH
3)
3, Au C
7H
7F
6O
2Or their combination etc.
In step 3 of the present invention) in the line that adopts of three-dimensional structure growth only for exemplary, its scope is approximately 20pA and following magnitude.Also will be according under specific growth conditions to the electrostatic displacemen speed (Δ r/ Δ t) that ion beam is taked, the speed of nanostructured vertical component growth, the distance that needs to form between contact block on the height of material of Three-Dimensional contact and it and the substrate or the connecting line is come calmly.During CVD growing three-dimensional structure, the growth of sloping portion is accompanied by vertical direction and the growth that is parallel to substrate usually, and this inevitably also has subsidiary growth on substrate.Larger velocity of displacement correspondence (90 °-θ)～(1/ Δ t), also cause more residual deposits on substrate simultaneously at larger inclination angle.When the three-dimensional structure height shorter, and and connecting line between distance when larger, need to adopt relatively large ion beam velocity of displacement, otherwise, should adopt less ion beam velocity of displacement, with the reduction residual deposits.The growing method that adopts also is exemplary, can also adopt graph scanning, the methods such as the accurate movement of sample stage.In addition, should be appreciated that for the person of ordinary skill of the art, the present invention adopts the SEM/FIB double-beam system, yet this method can be used in single bundle or other FIB systems equally; Except using SEM, the present invention can also use low line ion current to needs form three-diemsnional electrode the micro-nano material of stick-up carry out figure observation, the unnecessary bombardment that low line ion current can avoid gallium ion that material is caused in imaging process; And, also can use the multi beam ion beam, electron beam carries out the growth of three-dimensional structure.In addition, in FIB growth, utilize SEM to carry out the real-time monitored growth course, change in real time the ion beam velocity of displacement, with the position of adjusting contact point etc.
In step 4 of the present invention) in, residual deposits, the employed ion current size of the removal of pollution is exemplary, its scope is approximately pA to the nA magnitude, when the residual deposits of three-dimensional structure below will can be removed with ion beam in the angle of inclination of sample stage, scanning was not stopped by it and gets final product.
[embodiment 2]:
At multilayer film Si (substrate)/SiO
2(200nm)/and make vertical nano-device on MgO (cushion)/NbN (260nm)/MgO/NbN (220nm) structure, may further comprise the steps:
1) isolation of active area: adopt photoetching technique to form the resist graphics field at the multilayer film substrate, then use dry etching: RIE (reacting gas CF
4) and ICP (reacting gas BCl
3/ Ar), active area being divided into independently unit, Fig. 3 a is depicted as the substrate active area schematic diagram after the processing, and 31 is Si (substrate)/SiO
2(200nm)/and the MgO part, 32 and 33 parts are respectively NbN and MgO layer.
2) growth tungsten nanometer rods: utilize conductive silver glue to be fixed on the sample carrier substrate that processes in the step (1), send in the SEM/FIB cavity and be fixed on the sample stage; Sample stage is tilted 52 ° clockwise, make substrate surface vertical with the ion beam incident direction.Tungsten source (the W (CO) of heating GIS
6), open the electron beam ion beam, select the ion beam line of 1pA, adjust working depth and equipment state.Employing equipment pattern generator arranges the ion-beam scanning zone in the active area centre position and is of a size of 80nm * 80nm, rear importing metallorganic gaseous tungsten source, and setting the ion-beam scanning time is 10min.Gallium ion decomposes the metallorganic molecule of tungstenic, forms the tungsten nanometer rods (34) perpendicular to sample surfaces, shown in Fig. 3 b.Nanorod growth is closed tungsten source valve and generalized information system is return original off-position after finishing.
3) making of nano dot structure.Utilize the nanometer rods of FIB growth among Fig. 3 b as the mask of etching, adopt RIE and ICP, dry etching is thick to the NbN of lower floor and the surplus 100nm that has an appointment, form sandwich nano dot structure (32-33-32) and NbN/ (W-Ga-C-O) the nanometer contact (being formed by 32 and 34 of 33 tops) of 34 belows, shown in Fig. 3 c.
4) formation of three-diemsnional electrode distribution (35).Process is as the step 3 among the embodiment 1), the direction of displacement that just ion beam is applied is opposite.
5) formation of contact electrode piece (36).Adopt the FIB line of 10pA, be set with the consistent scanning area of source region width the NbN layer of three-dimensional structure below is carved thoroughly, make it to be divided into two, then the thick NbN of the remaining 100nm of lower floor can be used as large electrode contact piece, the final vertical nanostructured of SIS, device schematic structure such as Fig. 3 d of realizing.
As preferred embodiment of the present invention, said method is given prominence to and has been embodied the mask that the present invention makes as nano dot structure in the nano material perpendicular to substrate that adopts the FIB growth, and the while is as the excellent part of vertical electrode.Yet, for it should be appreciated by those skilled in the art, the more general implementation of another kind of the present invention is at first according to requirement on devices, in the process of Material growth, the suitable skin-material thin layer of growing forms the sandwich construction with specific knot contact performance, then growth of vertical in the nano material of substrate plane as mask, rear employing dry method or wet etching form the nano dot functional structure, and sharp FIB-CVD growing three-dimensional distribution is finished element manufacturing.
To multi-layer film material, the conducting nanowires of the other materials kind that the nanometer rods of FIB growth or other modes are grown, nanometer rods etc. both can be used as etching mask, form the function nano point, after finishing, etching also can be used as the vertical component of electrode, utilize FIB-CVD, then can the growing three-dimensional distribution, make it to be connected with large contact block.The vertical devices that this method forms, the area of active area is very little.
Step 1 at the present embodiment) in, employed multi-layer film structure only is exemplary, can also be other multilayer film or single-layer membrane structure, such as p+GaN/InGaN/GaN (MQW)/n+GaN multi-quantum pit structure.The isolation of active area also can be finished with other equipment and reacting gas, or adopts wet etching, the method that wet method is combined with dry method.
In addition, in the step 2 of the present embodiment) in, the nanometer rods perpendicular to substrate surface of FIB growth also can be replaced by other figures, as square, triangle, loop configuration, or the larger figure of area of growing first is fast, and then growth thereon has the nanometer rods of certain altitude etc.Scanning size also can freely design.
In addition, in the step 5 of the present embodiment) in, adopt the FIB etching that the remaining NbN layer of bottom is carved when thoroughly separating, also the place to go residual deposits during three dimensional growth, the NbN of bottom can be used as two contact electrode pieces simultaneously, has reduced the element manufacturing operation.And the vertical nano-device that said method is made is self aligned, and the area of active area can be done very littlely, and its side do not stop, this advantage on luminescent device, surface device, manufacturing of the fiber grating sensors is more obvious.
Although the present invention is made specific descriptions with reference to the above embodiments; but for the person of ordinary skill of the art; should be appreciated that and can make amendment or improve based on content disclosed by the invention, and these modifications and improve all should be within the protection domain of claim of the present invention.
Claims (8)
1. a method for preparing three-dimensional micro-nano device is characterized in that: comprise the following steps:
(1) sample is placed with fixing:
(i) if substrate is the conductive substrates with surface insulation thin layer, be fixed on the sample carrier from substrate back with conductive materials; If substrate is to have at the bottom of the electrically insulating substrate of surface conductance layer, be fixed on sample on the sample carrier after, with conductive materials sample surfaces is connected with sample carrier again;
The sample that (ii) will be fixed on the sample carrier is put on the sample stage of two-beam SEM/FIB or single bundle FIB cavity, then sample stage is carried out the inclination of certain angle, makes FIB perpendicular to substrate incident;
(2) figure of the three-D micro-nano material of stick-up observation:
The mobile example platform carries out figure observation with SEM or low line ion current, finds the stick-up micro-nano material and the free-ended position thereof that need to form electrode contact, and measures its size;
(3) growth of electrode contact piece and/or line in the substrate plane, this growth are to carry out before the micro Nano material growth of stick-up or after growing, wherein:
When a) before the micro Nano material growth of stick-up, in substrate plane, growing electrode contact piece and/or line, adopt traditional photoetching, electron beam exposure or focused ion beam deposition method to form substrate plane interior large electrode contact block and/or line;
B) when in substrate plane, growing electrode contact piece and/or line after the micro Nano material growth of stick-up, according to the position of material, adopt focused ion beam equipment, growth in situ electrode contact piece and/or contact conductor;
(4) making of three-diemsnional electrode contact and line:
The stick-up micro-nano material is formed three-diemsnional electrode contact and line;
(5) removing of residual deposits on the substrate:
With sample stage certain angle that tilts, make ion beam with certain angle side direction incident, make step 4) in processing three-dimensional structure under fully in the unscreened FIB of the being exposed to visual field; Then set scanning area, the residual deposits of three-dimensional structure below is removed;
(6) get finished product.
2. the method for preparing three-dimensional micro-nano device as claimed in claim 1, it is characterized in that: a) step in the described step (3), when distant between the free-ended projection of stick-up micro-nano material and contact block, need the Distance Shortened that a connecting line will be between the two of growing with FIB, comprise step: (i) obtain stick-up micro-nano material to be processed and the FIB image of electrode contact piece; (ii) the connecting line figure that utilizes the pattern generator Software Create of focused ion beam equipment to process is determined its position; (iii) introduce metallorganic gaseous molecular source; (iv) open FIB scanning plated metal line, an end of line should be close with the free end projection of stick-up micro-nano material, and the other end connects large electrode contact piece.
3. the method for preparing three-dimensional micro-nano device as claimed in claim 1 is characterized in that: the b in the described step (3)) step, comprise step: (i) obtain stick-up micro-nano material to be processed and the FIB image of electrode contact piece; (ii) the connecting line figure that utilizes the pattern generator Software Create of focused ion beam equipment to process is determined its position; (iii) introduce metallorganic gaseous molecular source; (iv) open FIB scanning, growth in situ electrode contact piece and/or contact conductor.
4. the method for preparing three-dimensional micro-nano device as claimed in claim 1 is characterized in that: described step (4) realizes respectively by the following method:
(i) electrostatic displacemen method, set a specific scanning area after, introduce metallorganic gaseous molecular source, beginning FIB scanning and adopt the static bias voltage to ion beam with the continuous yaw displacement of certain speed with the acquisition three-dimensional structure;
(ii) graph scanning method is by sweep time and the regional continuous three-dimensional structure of growing of focused ion beam equipment programme-control ion-beam scanning;
(iii) accurate Quality control platform displacement method, the continuous moving by sample stage changes the relative position that ion beam scans at substrate, to form three-dimensional structure.
5. the method for preparing three-dimensional micro-nano device as claimed in claim 4, it is characterized in that: described step (ii), the figure series of utilizing the pattern generator Software Create of focused ion beam equipment to process, according to the growth rate under the particular growth condition, accurately set the overlap coefficient in last graph scanning zone and rear one scan zone in succession and obtain continuous three-dimensional structure sweep time.
6. the method for preparing three-dimensional micro-nano device as claimed in claim 1, it is characterized in that: (i) electrostatic displacemen method of described step (4) comprises step:
(a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) its position is determined with big or small in the single ion-beam scanning of the pattern generator Software Create graphics field that utilizes focused ion beam equipment; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning, and with certain speed ion beam is carried out yaw displacement, until the 3-dimensional metal line of deposition and the upper end in contact of stick-up micro-nano material;
(ii) graph scanning method comprises step: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) utilize the pattern generator Software Create ion-beam scanning graphical set of focused ion beam equipment, determine particular location and the sweep time of each figure; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning growing three-dimensional structure, form electrode contact;
(iii) accurate Quality control platform displacement method, the manufacturing process of three-diemsnional electrode contact comprises step: (a) collect stick-up micro-nano material to be processed and reach adjacent with it connecting line or the FIB image of contact electrode piece; (b) its position is determined with big or small in the single ion-beam scanning of the pattern generator Software Create graphics field that utilizes focused ion beam equipment; (c) introduce metallorganic gaseous molecular source; (d) open FIB scanning, by the mobile growing three-dimensional contact structures of sample stage.
7. the method for preparing three-dimensional micro-nano device as claimed in claim 1, it is characterized in that: when the method is made electrode in the metal deposition function of utilizing focused ion beam equipment, freely uphold the growth of holding direct-connected connecting line with material, adopt low line≤20pA.
8. the method for preparing three-dimensional micro-nano device as claimed in claim 1 is characterized in that: in the described step (5), to the residual deposits around the three-dimensional structure, adopt vertically or other incident angle removal residual deposits; When utilizing FIB that residual deposits is removed, line is that pA is to the nA magnitude.
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| CA2568789A1 (en) * | 2004-04-13 | 2005-10-27 | Riber | Method of three-dimensional microfabrication and high-density three-dimensional fine structure |
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| CN101207137A (en) * | 2006-12-22 | 2008-06-25 | 中国科学院物理研究所 | Material with metal silicide nanostructure and method for making the same |
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