CN102320566B - Method for preparing three-dimensional nano space electrode by adopting self-alignment forming - Google Patents
Method for preparing three-dimensional nano space electrode by adopting self-alignment forming Download PDFInfo
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Abstract
The invention discloses a method for preparing a three-dimensional nano space electrode by adopting self-alignment forming. The method comprises the following steps of: fixing a sample on a substrate, fixing the substrate on a sample support, and placing the sample support fixed with the sample and the substrate on a sample table in a vacuum cavity of electron beam/ ion beam double-beam equipment; finding a specific nano structure in the sample by adopting an electron microscope, and then growing a platinum nano wire for forming a certain included angle with the substrate on the sample by adopting a focusing ion beam/ electron beam assisted deposition technology; performing deformation operation on the prepared platinum nano wire by adopting a thermal annealing mode; and growing an electrode contact block or a connecting wire, and thus obtaining the three-dimensional nano space electrode. The preparation method for preparing a micro/nano structure not in a substrate supporting plane based on the phenomenon of regular deformation of the focusing ion beam/ electron beam assisted deposition thermally-annealed platinum nano wire has the characteristics of good flexibility and high controllability.
Description
Technical field
The present invention relates to the three-dimensional micro-nano device preparing technical field, the deformation that is particularly related to a kind of Pt nanowires of or electron beam assistant depositing growth auxiliary to the FIB of stick-up based on thermal annealing handles to prepare the method for three-dimensional bending micro-nano structure,, in the situation that do not destroy original internal structure, be specially adapted to the preparation of three-dimensional nano space electrode.
Background technology
Development along with nanometer technology, research to the low-dimensional materials physical property is more and more extensive, particularly the research of one-dimensional nano line launched on a large scale, article about various nano wire emerges in an endless stream,, for nano wire being applied to the circuit of micro-nano size, about the measurement of nano wire electrical properties, be absolutely necessary.For the nano wire that is in mesoscopic size,, because its size is very little, make the measurement research to its electrical properties become very difficult, measurement means is very limited.
The method of existing measurement nano wire electrical properties can be divided into two large classes: one. the in site measurement method.In this method, the microscopical conducting probes such as AFM, STM, SPM are used to be used as one of them contact electrode of nanotube, and to observation and the manipulation of nanotube, the realization that electrically contacts and electrical measurement are all carried out in the microscope chamber.The method have a series of shortcomings such as: to nanotube carry out alternating temperature, add outfield, electricity transport property research and comparison difficulty in the situation such as ventilation body.Wherein maximum shortcoming is exactly the research that the method can only be used for carrying out the nano wire physical property, can not be applied in actual circuit large-scale production.
Two. will prepare electrode and electrical properties and measure the method for separately carrying out.This kind method adopts modern micro-processing technology, utilizes the means such as beamwriter lithography, ion beam assisted depositing metal to make electrode, with macroscopical contact electrode on the nanometer pipe racks that is dispersed on dielectric substrate, and its electrology characteristic of measurement that then just can be easier.But the method inevitably pollutes and destroys nano wire.Therefore be badly in need of finding a kind of preparation method that can overcome the three-dimensional former potential electrode of above shortcoming.
In addition, along with device develops towards miniaturization, people are devoted to improve device density, are one of approach that improves device density to the structure of three-dimension device.The manufacture method of finding the controlled space nanostructured of a kind of three-dimensional has caused more and more people's concern.
Summary of the invention
The technical problem that (one) will solve
In view of this, main purpose of the present invention is to provide a kind of method that adopts self-alignment forming to prepare three-dimensional nano space electrode,, to solve the problem of present 3-D nano, structure electrode preparation method shortage, reach the purpose for preparing the 3-D nano, structure electrode on the basis of not damaging original 3-D nano, structure.
(2) technical scheme
For achieving the above object, the invention provides a kind of method that adopts self-alignment forming to prepare three-dimensional nano space electrode, comprising:
Sample is fixed on substrate, and substrate is fixed on sample carrier, and the sample carrier that is fixed with sample and substrate is positioned on sample stage in FIB/SEM double-beam system vacuum chamber;
Adopt electron microscope to find particular nanostructure on sample, then adopt the Pt nanowires that FIB or electron beam assistant depositing technology are grown on sample and substrate forms an angle;
Adopt the thermal annealing mode to carry out the deformation operation to the Pt nanowires for preparing; And
Growth electrode contact piece or line, obtain three-dimensional nano space electrode.
In such scheme, described sample is fixed on substrate, substrate is fixed on sample carrier, comprising: if substrate face is insulating barrier, the back side is conductive layer, this substrate back conductive layer is contacted with sample carrier, and with conductive materials, substrate is fixed on sample carrier; If substrate face is conductive layer, the back side is insulating barrier, this substrate back insulating barrier is contacted with sample carrier, and with conductive materials, the substrate face conductive layer is connected with sample carrier after being fixed in sample on sample carrier again.
In such scheme, described employing electron microscope is after finding particular nanostructure on sample, also comprise: the position of selected Pt nanowires growth and the relative position in Pt nanowires and platinum precursor source, and the relative position in Pt nanowires and platinum precursor source is regulated.In the described step that the relative position in Pt nanowires and platinum precursor source is regulated, the control of this relative position realizes by specimen rotating holder.described employing FIB or electron beam assistant depositing technology comprise at growth on sample and the Pt nanowires that substrate forms an angle: adopt electron microscope after finding particular nanostructure on sample, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, start the point-scan mode of ion beam or electron beam in the position of selected Pt nanowires growth, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby form the deposition of pt atom at the scanning position place, and the metal organic molecule can continue to be adsorbed on substrate surface, and due to the invariant position of scanning element, so deposition can occur in identical position and the pt atom layer height of deposition constantly increases, the control of Pt nanowires height is to control by the time that control point is scanned, the diameter of Pt nanowires is that the adjustment of focusing is controlled by the choosing of line, because height of deposition is incident direction along ion beam or electron beam, the orientation of the nano-pillar that therefore deposits is determined by the incident direction of ion beam or electron beam, by the incline direction of adjusting sample stage, ion beam or electron beam are incided on sample stage with certain angle, thereby can control the Pt nanowires that growth and substrate form an angle.The length of described Pt nanowires is controlled by sedimentation time, and the diameter of Pt nanowires is determined by the line of the focus level in when growth and electron beam/ion beam used; The Pt nanowires diameter that adopts less than 3 microns and draw ratio greater than 1: 1, by annealing to regulate and control to make its deformation crooked.
In such scheme, described employing thermal annealing mode is carried out the deformation operation to the Pt nanowires for preparing and comprised: the sample that will be prepared with Pt nanowires is positioned in the annealing furnace body of wall, selective annealing temperature, annealing time, and annealing atmosphere anneals, and makes Pt nanowires crooked; Wherein the angle of Pt nanowires bending is relevant with annealing time, annealing temperature and annealing atmosphere, realizes the angle of nano-pillar bending by the control to these three parameters.Described in these three parameters of annealing time, annealing temperature and annealing atmosphere are controlled to realize the process of nano-pillar angle of bend, adopt the combination of various temperature, time, atmosphere to realize identical bending effect.The combination of described employing various temperature, time, atmosphere realizes that identical bending effect comprises: annealing is 1 minute under the atmosphere of 900 ℃ of nitrogen, perhaps anneals 4 hours under the atmosphere of 250 ℃ of air, can make Pt nanowires reach same bending effect.
in such scheme, described growth electrode contact piece or line are to realize by the deposition of material of FIB or electron beam-induced, specifically comprise: adjust the sample stage position, find the position of three-diemsnional electrode contact block or line growth under electron beam or ion beam, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, the drawing software that carries by system draws the electrode contact piece that will deposit or the figure of line in the position of want depositing electrode contact block or line, size and the thickness of figure are set, systems soft ware can be according to size and the position of drawn figure, after starting ion beam or electron beam scanning, controlling ion beam or electron beam scans it in the zone of drawn figure, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby form the deposition of pt atom at the scanning position place, carry out the growth of electrode contact piece or line.
(3) beneficial effect
Can find out from technique scheme, the present invention has following beneficial effect:
1. the high controllability of technique.
The present invention adopts FIB/required Pt nanowires of electron beam assistant depositing method growth, then by thermal annealing, controls the bending of nano wire, thereby prepares the electrode of 3-D nano, structure.In whole process, the growth of Pt nanowires comprises its length, growth position, and the condition that annealing is adopted, the position with respect to the precursor source during nano-pillar growth is all accurately controlled.Uncertain factor almost can be ignored, thereby can make highly controlled three-diemsnional electrode.The method is a kind of have highly repeatability, preparation method of the three-diemsnional electrode of uniformity and controllability.
2. the diversity of target nanostructured.
Adopting the present invention prepares the three-dimensional manometer electrode to the target nanostructured preparation process is exactly that annealing process does not exist destruction (can not change its structure to the target nanostructured to unique requirement of target nanostructured, material shape and material form, do not pollute this structure, do not change the character of this structure), the annealing conditions that adopts due to this method does not have uniqueness, so can pass through annealing conditions (annealing temperature, time, atmosphere) selection reaches the above-mentioned purpose of not destroying object construction.Therefore can make by the selection of annealing conditions selectively greatly improving of target nanostructured.
3. the high flexibility of technique.
The flexibility of technique shows following two aspects: position and the bending direction of (1) Pt nanowires can accurately be controlled, thereby can flexible design make the three-dimensional manometer electrode be distributed in as requested around the target nanostructured and with the privileged site of 3-D nano, structure, be combined; (2) selection of this technique annealing conditions has diversity, thereby the range of choice of target 3-D nano, structure is increased greatly.
4. the various dimensions feature of technique.
Because thereby prepared electrode is to make FIB/Pt nanowires bending and the target nanostructured of electron beam assistant depositing growth contact to form the three-diemsnional electrode of target nanostructured by thermal annealing.Prepared electrode has the three dimensionality characteristic, and the target nanostructured has the three dimensionality characteristic, so this technique has the various dimensions characteristic.
5. simple for process.
The technique of this technique is simple, only need adopting FIB/electron beam assistant depositing technology to deposit Pt nanowires on the nanostructured that plays the support sacrificial action around this nanostructured, then pass through thermal annealing process, do not need the participation of other techniques, simple for process with this.Can make the target nanostructured is not had destruction the selection of annealing process parameter, be conducive to the preparation of device and the raising of device performance.
Description of drawings
Fig. 1 is the method flow diagram that employing self-alignment forming provided by the invention prepares three-dimensional nano space electrode.
Fig. 2 is the schematic diagram of Pt nanowires of growing under electron beam or ion beam according to the embodiment of the present invention.Electron beam or ion beam be to the substrate scanning of fixing a point, and under the atmosphere of the precursor of platinum, by electron beam or ion beam induced, carries out growth perpendicular to (perhaps with substrate form an angle) substrate Pt nanowires.
Fig. 3 is according to the shape contrast picture of the embodiment of the present invention perpendicular to the annealed front and back of Pt nanowires of substrate.
Fig. 4 adopts the rear crooked characteristic of Pt nanowires annealing of FIB assistant depositing to study the electrology characteristic schematic diagram of orthotropic nano wire as space electrode according to the embodiment of the present invention; Wherein, (a) be near the Pt nanowires that adopts FIB assistant depositing technology/electron beam assistant depositing technology growth the nano wire of required measurement; (b) adopt the Pt nanowires of FIB assistant depositing technology/electron beam assistant depositing technology growth to buckle after annealing, with the research object nano wire that there is no bending after annealing, form and contact.
In figure, each Reference numeral is as follows:
1, substrate; 2, the Pt nanowires perpendicular to substrate of employing FIB assistant depositing technology/electron beam assistant depositing technology growth; 3, electron beam/ion beam chamber; 4, the precursor molecular source of platinum; 5, diastrophic Pt nanowires after annealing; 6, vertical nano-wire to be measured.
The specific embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
As shown in Figure 1, Fig. 1 is the method flow diagram that employing self-alignment forming provided by the invention prepares three-dimensional nano space electrode, and the method comprises the following steps:
Step 1: sample is fixed on substrate, and substrate is fixed on sample carrier, and the sample carrier that is fixed with sample and substrate is positioned on sample stage in FIB/SEM double-beam system vacuum chamber;
Step 2: adopt electron microscope to find particular nanostructure on sample, then adopt the Pt nanowires that FIB or electron beam assistant depositing technology are grown on sample and substrate forms an angle;
Step 3: adopt the thermal annealing mode to carry out the deformation operation to the Pt nanowires for preparing;
Step 4: growth electrode contact piece or line obtain three-dimensional nano space electrode.
Wherein, described in step 1, sample is fixed on substrate, substrate is fixed on sample carrier, comprising: if substrate face is insulating barrier, the back side is conductive layer, this substrate back conductive layer is contacted with sample carrier, and with conductive materials, substrate is fixed on sample carrier; If substrate face is conductive layer, the back side is insulating barrier, this substrate back insulating barrier is contacted with sample carrier, and with conductive materials, the substrate face conductive layer is connected with sample carrier after being fixed in sample on sample carrier again.
Adopt electron microscope described in step 2 after finding particular nanostructure on sample, also comprise: the position of selected Pt nanowires growth and the relative position in Pt nanowires and platinum precursor source, and the relative position in Pt nanowires and platinum precursor source is regulated.In the described step that the relative position in Pt nanowires and platinum precursor source is regulated, the control of this relative position realizes by specimen rotating holder.described employing FIB or electron beam assistant depositing technology comprise at growth on sample and the Pt nanowires that substrate forms an angle: adopt electron microscope after finding particular nanostructure on sample, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, start the point-scan mode of ion beam or electron beam in the position of selected Pt nanowires growth, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby form the deposition of pt atom at the scanning position place, and the metal organic molecule can continue to be adsorbed on substrate surface, and due to the invariant position of scanning element, so deposition can occur in identical position and the pt atom layer height of deposition constantly increases, the control of Pt nanowires height is to control by the time that control point is scanned, the diameter of Pt nanowires is that the adjustment of focusing is controlled by the choosing of line, because height of deposition is incident direction along ion beam or electron beam, the orientation of the nano-pillar that therefore deposits is determined by the incident direction of ion beam or electron beam, by the incline direction of adjusting sample stage, ion beam or electron beam are incided on sample stage with certain angle, thereby can control the Pt nanowires that growth and substrate form an angle.The length of described Pt nanowires is controlled by sedimentation time, and the diameter of Pt nanowires is determined by the line of the focus level in when growth and electron beam/ion beam used; The Pt nanowires diameter that adopts less than 3 microns and draw ratio greater than 1: 1, by annealing to regulate and control to make its deformation crooked.
Adopting the thermal annealing mode to carry out the deformation operation to the Pt nanowires for preparing described in step 3 comprises: the sample that will be prepared with Pt nanowires is positioned in the annealing furnace body of wall, selective annealing temperature, annealing time, and annealing atmosphere anneals, and makes Pt nanowires crooked; Wherein the angle of Pt nanowires bending is relevant with annealing time, annealing temperature and annealing atmosphere, realizes the angle of nano-pillar bending by the control to these three parameters.Described in these three parameters of annealing time, annealing temperature and annealing atmosphere are controlled to realize the process of nano-pillar angle of bend, adopt the combination of various temperature, time, atmosphere to realize identical bending effect.The combination of described employing various temperature, time, atmosphere realizes that identical bending effect comprises: annealing is 1 minute under the atmosphere of 900 ℃ of nitrogen, perhaps anneals 4 hours under the atmosphere of 250 ℃ of air, can make Pt nanowires reach same bending effect.
wherein, described growth electrode contact piece or line are to realize by the deposition of material of FIB or electron beam-induced, specifically comprise: adjust the sample stage position, find the position of three-diemsnional electrode contact block or line growth under electron beam or ion beam, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, the drawing software that carries by system draws the electrode contact piece that will deposit or the figure of line in the position of want depositing electrode contact block or line, size and the thickness of figure are set, systems soft ware can be according to size and the position of drawn figure, after starting ion beam or electron beam scanning, controlling ion beam or electron beam scans it in the zone of drawn figure, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby form the deposition of pt atom at the scanning position place, carry out the growth of electrode contact piece or line.
The method flow diagram for preparing three-dimensional nano space electrode based on employing self-alignment forming provided by the invention shown in Figure 1, Fig. 2 to Fig. 4 shows according to the embodiment of the present invention and adopts self-alignment forming to prepare the process chart of three-dimensional nano space electrode, this embodiment controls to make the three-dimensional nano space electrode of vertical nano-wire based on the three-dimensional deformation of Pt nanowires after annealing of FIB Material growth or the growth of electron beam assistant depositing, comprise the following steps:
(1) sample is placed with fixing:
There is the substrate of vertical nano wire to be measured substrate back to be fixed on the sample carrier with horizontal surface with the conduction carbon ribbon with long, the sample that will be fixed on sample carrier is put on the sample stage of two-beam SEM/FIB cavity, and system ion gun used becomes 52 ° of angles with electron gun.
(2) perpendicular to the growth of the Pt nanowires of substrate:
As shown in Figure 2, Fig. 2 is the schematic diagram of Pt nanowires of growing under electron beam or ion beam according to the embodiment of the present invention.Vacuumize, after vacuum reaches requirement, 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), sample stage is tilted 52 °, make ion beam make electron beam vertical incidence substrate perpendicular to substrate incident or the sample stage that do not tilt.The metallorganic gaseous molecular source import system of heating platinum, be incorporated into conduit substrate surface and open valve.Start ion beam or electron-beam point scan pattern, it is the ion current of 1pA that ion beam is adopted line, sets sweep time (length by needed Pt nanowires determines), at the Pt nanowires of Grown perpendicular to substrate surface.
(3) based on the deformation operation of annealing to Pt nanowires
Step comprises: sample is put in the quick anneal oven body of wall, and the selective annealing temperature, time, and annealing atmosphere, anneal.The angle of Pt nanowires bending is relevant with annealing time, temperature and annealing atmosphere, realizes the bending of nano-pillar by the control of these three parameters.The combination of various temperature, time, atmosphere can realize identical function.As adopting the annealing of high-temperature short time to make its bending to a certain degree, also can adopt low temperature to make for a long time it reach identical effect.Can make Pt nanowires crooked in one minute as annealing under the atmosphere at 900 ℃ of nitrogen, annealing can reach same bending effect in 4 hours under the atmosphere of 250 ℃ of air.Fig. 3 is according to the shape contrast picture of the embodiment of the present invention perpendicular to the annealed front and back of Pt nanowires of substrate.
(4) growth of electrode contact piece or line:
Electrode contact piece or line growth are to realize by the deposition of material of FIB/electron beam-induced.step comprises adjusts the sample stage position, find the position of three-diemsnional electrode contact block or line growth under electron beam or ion beam, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, the drawing software that carries by system draws the electrode contact piece that will deposit or the figure of line in the position of want depositing electrode contact block or line, size and the thickness of figure are set, systems soft ware can be according to size and the position of drawn figure, after starting ion beam or electron beam scanning, controlling ion beam or electron beam scans it in the zone of drawn figure, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby form the deposition of pt atom at the scanning position place.Thereby reach the growth of electrode contact piece or line.Also can adopt other process to prepare metal connecting line or electrode contact piece in needed position.Choosing of material to electrode contact piece or line should be followed such principle: can experience the annealing of uniform temperature and keep electric conductivity and pattern substantially constant, such temperature is 200C ° at least.
(5) obtain finished product, i.e. three-dimensional nano space electrode.
Fig. 4 adopts the rear crooked characteristic of Pt nanowires annealing of FIB assistant depositing to study the electrology characteristic schematic diagram of orthotropic nano wire as space electrode according to the embodiment of the present invention; Wherein, (a) be near the Pt nanowires that adopts FIB assistant depositing technology/electron beam assistant depositing technology growth the nano wire of required measurement; (b) adopt the Pt nanowires of FIB assistant depositing technology/electron beam assistant depositing technology growth to buckle after annealing, with the research object nano wire that there is no bending after annealing, form and contact.
Step 3 in the embodiment of the present invention) in, annealing temperature can have different combinations to form identical bending from choosing of annealing time and atmosphere.For example under the nitrogen of certain flow, the annealing temperature that the low annealing temperature of long annealing time and short annealing time are high can form identical bending.The combination of various temperature, time, atmosphere can realize identical function.As adopting the annealing of high-temperature short time to make its bending to a certain degree, also can adopt low temperature to make for a long time it reach identical effect.Can make Pt nanowires crooked in one minute as annealing under the atmosphere at 900 ℃ of nitrogen, annealing can reach same bending effect in 4 hours under the atmosphere of 250 ℃ of air.
In embodiments of the present invention, Pt nanowires with stick-up of larger depth-width ratio is to carry out three-dimensional deformation in the present invention to handle control, the major function unit for preparing three-dimension device and space electrode, but the present invention is not limited to employing electron beam/ion beam assisted depositing Pt nanowires of growing, also can adopt the nano-pillar of other kinds of additive method growth, as long as this nano-pillar can be towards the crooked specific angle of specific direction after thermal anneal process.
In embodiments of the present invention, the electric conductivity of the substrate that adopts in step 1 is various, can be good conductor, can be also semiconductor or insulator.The crystal structure of substrate is not limit, and can be monocrystalline, polycrystalline, perhaps amorphous.In step 2, the method for growth Pt nanowires can be the electron beam assistant depositing, can be also ion beam assisted depositing.In step 2, Pt nanowires and angle substrate are diversified, and Pt nanowires can be grown perpendicular to substrate, also can with the angled growth of substrate.The control of angle depends on the angle of electron beam/ion beam and substrate.In step 2, the length of Pt nanowires is opened control by sedimentation time, and the diameter of Pt nanowires is determined by the line of the focus level in when growth and electron beam/ion beam used.The Pt nanowires diameter that adopts less than 3 microns and draw ratio greater than 1: 1, can be by annealing to regulate and control to make its deformation crooked.The processing method of the thermal annealing that adopts in step 3 is varied, can adopt quick anneal oven to carry out, and also can carry out in other instruments, as long as this instrument can provide certain temperature and certain atmosphere.The annealing conditions that adopts in step 3 can be multiple combination, i.e. the combination of various temperature, time, atmosphere can realize identical function.As adopting the annealing of high-temperature short time to make its bending to a certain degree, also can adopt low temperature to make for a long time it reach identical effect.Annealing region in step 3 is very extensive, and making for Pt nanowires that the annealing temperature of its deformation is minimum can be less than 200C °.In step 4, the growing method of electrode contact piece and line is varied, can be to adopt electron beam/ion beam assisted depositing growth, also can adopt the additive method growth.
In addition, before in the present embodiment, step 4 also can be placed on step 2 and 3.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a method that adopts self-alignment forming to prepare three-dimensional nano space electrode, is characterized in that, comprising:
Sample is fixed on substrate, and substrate is fixed on sample carrier, and the sample carrier that is fixed with sample and substrate is positioned on sample stage in FIB/SEM double-beam system vacuum chamber;
Adopt electron microscope to find particular nanostructure on sample, then adopt the Pt nanowires that FIB or electron beam assistant depositing technology are grown on sample and substrate forms an angle;
Adopt the thermal annealing mode to carry out the deformation operation to the Pt nanowires for preparing; And
Growth electrode contact piece or line, obtain three-dimensional nano space electrode.
2. employing self-alignment forming according to claim 1 prepares the method for three-dimensional nano space electrode, it is characterized in that, described sample is fixed on substrate, and substrate is fixed on sample carrier, comprising:
If substrate face is insulating barrier, the back side is conductive layer, this substrate back conductive layer is contacted with sample carrier, and with conductive materials, substrate is fixed on sample carrier; If substrate face is conductive layer, the back side is insulating barrier, this substrate back insulating barrier is contacted with sample carrier, and with conductive materials, the substrate face conductive layer is connected with sample carrier after being fixed in sample on sample carrier again.
3. employing self-alignment forming according to claim 1 prepares the method for three-dimensional nano space electrode, it is characterized in that, described employing electron microscope after finding particular nanostructure on sample, also comprises:
The position of selected Pt nanowires growth and the relative position in Pt nanowires and platinum precursor source, and the relative position in Pt nanowires and platinum precursor source is regulated.
4. employing self-alignment forming according to claim 3 prepares the method for three-dimensional nano space electrode, it is characterized in that, in the described step that the relative position in Pt nanowires and platinum precursor source is regulated, the control of this relative position realizes by specimen rotating holder.
5. employing self-alignment forming according to claim 3 prepares the method for three-dimensional nano space electrode, it is characterized in that, the Pt nanowires that described employing FIB or electron beam assistant depositing technology are grown on sample and substrate forms an angle comprises:
Adopt electron microscope after finding particular nanostructure on sample, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, start the point-scan mode of ion beam or electron beam in the position of selected Pt nanowires growth, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby forms the deposition of pt atom at the scanning position place; And the metal organic molecule can continue to be adsorbed on substrate surface, and due to the invariant position of scanning element, so deposition can occur in identical position and the pt atom layer height of deposition constantly increases; The control of Pt nanowires height is to control by the time that control point is scanned; The diameter of Pt nanowires is that the adjustment of focusing is controlled by the choosing of line; Because height of deposition is incident direction along ion beam or electron beam, the orientation of the nano-pillar that therefore deposits is determined by the incident direction of ion beam or electron beam, by the incline direction of adjusting sample stage, ion beam or electron beam are incided on sample stage with certain angle, thereby can control the Pt nanowires that growth and substrate form an angle.
6. employing self-alignment forming according to claim 5 prepares the method for three-dimensional nano space electrode, it is characterized in that, the length of described Pt nanowires is controlled by sedimentation time, and the diameter of Pt nanowires is determined by the line of the focus level in when growth and electron beam/ion beam used; The Pt nanowires diameter that adopts less than 3 microns and draw ratio greater than 1: 1, by annealing to regulate and control to make its deformation crooked.
7. employing self-alignment forming according to claim 1 prepares the method for three-dimensional nano space electrode, it is characterized in that, described employing thermal annealing mode is carried out the deformation operation to the Pt nanowires for preparing and comprised:
The sample that is prepared with Pt nanowires is positioned in the annealing furnace body of wall, selective annealing temperature, annealing time, and annealing atmosphere anneals, and makes Pt nanowires crooked; Wherein the angle of Pt nanowires bending is relevant with annealing time, annealing temperature and annealing atmosphere, realizes the angle of nano-pillar bending by the control to these three parameters.
8. employing self-alignment forming according to claim 7 prepares the method for three-dimensional nano space electrode, it is characterized in that, described in these three parameters of annealing time, annealing temperature and annealing atmosphere are controlled to realize the process of nano-pillar angle of bend, adopt the combination of various temperature, time, atmosphere to realize identical bending effect.
9. employing self-alignment forming according to claim 8 prepares the method for three-dimensional nano space electrode, it is characterized in that, the combination of described employing various temperature, time, atmosphere realizes that identical bending effect comprises:
Annealing is 1 minute under the atmosphere of 900 ℃ of nitrogen, perhaps anneals 4 hours under the atmosphere of 250 ℃ of air, can make Pt nanowires reach same bending effect.
10. employing self-alignment forming according to claim 1 prepares the method for three-dimensional nano space electrode, it is characterized in that, described growth electrode contact piece or line are to realize by the deposition of material of FIB or electron beam-induced, specifically comprise:
adjust the sample stage position, find the position of three-diemsnional electrode contact block or line growth under electron beam or ion beam, introduce metallorganic gaseous molecular source by the gas assistant depositing system that the FIB/SEM double-beam system carries, the drawing software that carries by system draws the electrode contact piece that will deposit or the figure of line in the position of want depositing electrode contact block or line, size and the thickness of figure are set, systems soft ware can be according to size and the position of drawn figure, after starting ion beam or electron beam scanning, controlling ion beam or electron beam scans it in the zone of drawn figure, under the effect of ion beam or electron beam, the metal organic molecule that is adsorbed on substrate surface resolves into metallic atom and associated gas, metallic atom is deposited on the scanning position place, associated gas is taken away by vacuum system, thereby form the deposition of pt atom at the scanning position place, carry out the growth of electrode contact piece or line.
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| CN103196728B (en) * | 2013-04-09 | 2015-12-02 | 上海华力微电子有限公司 | FIB technology is used to prepare the method for SEM or TEM sample protective seam |
| CN104528635B (en) * | 2014-12-17 | 2016-08-31 | 东南大学 | A kind of method preparing ultra-fine vertical orientated nano wire |
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