CN1779466A - Testing electrode of single nanometer materials and production thereof - Google Patents
Testing electrode of single nanometer materials and production thereof Download PDFInfo
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- CN1779466A CN1779466A CN 200410091205 CN200410091205A CN1779466A CN 1779466 A CN1779466 A CN 1779466A CN 200410091205 CN200410091205 CN 200410091205 CN 200410091205 A CN200410091205 A CN 200410091205A CN 1779466 A CN1779466 A CN 1779466A
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Abstract
A test electrode of one-dimensional nanomaterial in single piece form consists of electrode line contacted by one-dimensional material and connection part for measuring lead wire. Its preparing method includes preparing metal electrode according to size and form of single piece and one dimensional nanomaterial, setting thickness of substrate to be 0.5-2mm and placing a insulation layer on substrate for distributing tested single piece and one dimensional nanomaterial on.
Description
Technical field
The present invention relates to a kind of single nanometer materials test electrode and preparation method thereof, particularly focused ion beam technology and electron beam lithography are applied to test electrode of single nanometer materials and preparation method thereof.
Background technology
The sign of monodimension nanometer material rerum natura is the focus that people study always, particularly the measurement of single nanometer materials intrinsic rerum natura.Wherein the design and fabrication of potential electrode is to realize this purpose basis and crucial.The method for making of existing monodimension nanometer material test electrode mainly contains two kinds.A kind of is directly to use focused ion beam technology to make electrode, as documents 1 " the electrically contacting of thick oxide layer nano wire (Making electricalcontacts to nanowires with a thick oxide coating); be stated from " Nanotechnology "; 2002; Vol.13; No.5:653-658 is disclosed ", this method utilization two-beam focused ion beam system, at first find the position of single nanometer materials with electron beam, with the ion beam location, make electrode with the method for ion beam assisted depositing platinum then again.The advantage of this method is: directly, operation is shorter.But shortcoming also clearly: at first be the contaminated area problem, because the platinum of this deposition techniques is the charcoal hydrogen compound effects generation by high energy Ga ion and Pt, so the Pt gold of deposition in very large range exists, (near the every Pt line very big contaminated area is arranged) as shown in Figure 1, its contaminated area generally surpasses 1 μ m, thereby causes the short circuit of electrode easily; Secondly monodimension nanometer material can form defective and Ga ion and inject, thereby influence its character after high energy Ga ion scan; In addition, these all will have influence on subsequent measurement to contain a large amount of C and Ga among the deposition Pt.Another kind method is to utilize electron-beam exposure system (or combine with the uv-exposure system) a large amount of electrode pattern of exposure on substrate earlier, utilize metal coating deposition techniques electrodes such as magnetron sputtering or evaporation, monodimension nanometer material is dispersed on the substrate that has nano-electrode then, a kind of method similar to this kind method is earlier monodimension nanometer material to be dispersed on the substrate, and then make a large amount of electrodes, as documents 2 " the carbon nano-tube four-probe measurement of low ohm contact (Contacting carbon nanotubes selectively with low-ohmiccontacts for four-probe electric measurements); be stated from " Applied Physics Letters " 1998; Vol.84, No.7:274-276 is disclosed ".The advantage of the method for this making test electrode is pollution and the destruction problem of having avoided in the FIB manufacturing process.But shortcoming also clearly, will do a large amount of electrodes on the one hand on a substrate, increased Production Time and cost of manufacture, and material and interelectrode contact resistance are higher, have influenced the measurement of electrical properties; On the other hand, because the nanotube stochastic distribution, success ratio is lower, and this method for making is difficult to make the test electrode that shape and size have the single nanometer materials of specific (special) requirements.Therefore, use the test electrode that above two kinds of methods make single one-dimensional material and all have very big defective.
Summary of the invention
The objective of the invention is to: solve existing utilization focused ion beam technology and make in the electrode process, the platinum of deposition is the charcoal hydrogen compound effects generation by high energy Ga ion and Pt, near the every Pt line very big contaminated area is arranged, cause electric pole short circuit easily, and high energy Ga ion injects and the problem of the monodimension nanometer material defective that causes; It is higher also will to overcome the material and the interelectrode contact resistance that exist in other making electrode method, influence the measurement of electrical properties, and because the nanotube stochastic distribution, it is lower that electrode is made into power, and being difficult to make shape and size has the defective of the single nanometer materials test electrode of specific (special) requirements, thereby a kind of test electrode that destroys the single nanometer materials little, that contact resistance is low that one-dimensional material is polluted is provided; This method has the high characteristics of electrode make efficiency, and can come the design electrode pattern according to the difformity and the size of single nanometer materials, is the method for making of the high single nanometer materials test electrode of a kind of dirigibility and reliability.
The present invention is achieved in that
The test electrode of single nanometer materials of the present invention comprises: thickness is the substrate of 0.5mm~2mm; One deck is an insulation course above the substrate; The single nanometer materials that on insulation course, is distributing and to measure; Size and shape according to single nanometer materials are made metal electrode, and metal electrode comprises and one-dimensional material electrodes in contact line part and the coupling part that is used for measuring lead wire.
According to the needs of measuring, metal electrode can also be made 2 or more electrode on insulation course, and the shape of metal electrode and size be referring to the design of electrode pattern.
Described backing material comprises: Si, quartz or any material with better surface smoothness.
Described substrate dimension generally should be greater than 5 * 5mm.
Described insulating layer material comprises: SiO
2, Si
3N
4, insulating material such as adamas, the thickness of insulation course is as the criterion to reach insulation effect, is generally 10 nanometer to 1000 nanometers.
Described metal electrode material comprises: bilayer or metal multilayer films such as Ti/Pt and Ti/Au, or single-layer metal films such as Pd, Al, Cu, with good conductivity, can form good ohmic with surveyed monodimension nanometer material and contact and be advisable, metal electrode thickness is about tens and arrives the hundreds of nanometer.
The design of electrode pattern of the present invention: according to the size that will measure single nanometer materials and shape, the design electrode pattern, electrode pattern generally comprise contact conductor part and with the direct electrodes in contact line of monodimension nanometer material part, the contact conductor part generally can be regular shapes such as square or circle, its size and spacing are conveniently decided with follow-up lead-in wire, electrode wires partly is generally elongated linear, and its live width and spacing are according to the concrete shape and the size design of monodimension nanometer material.Provide a kind of electrode figure (accompanying drawing 3) of linear nano pipe (line) always at this, figure 4 is the contact conductor part, and its size and space D 1 to each other, the size of D2 conveniently are as the criterion with follow-up work; L1, L2, L3, L4 are the four strip electrode lines that directly contact with one-dimensional material, and L1, L2, L3, L4 minimum feature can be accomplished 30nm, and spacing each other is 80nm, and the width D between the four strip electrode lines is equal to or less than the length of nanotube (line).
The present invention is used to make the method for single nanometer materials test electrode, may further comprise the steps:
1) cleaning of substrate: adopt acetone, alcohol, secondary deionized water three step ultrasonic cleaning, per step cleaned 3~5 minutes; Adopt conventional method to make insulation course thereon, this insulating layer material comprises: SiO
2, Si
3N
4, insulating material such as adamas, the thickness of insulation course is as the criterion to reach insulation effect, is generally 10 nanometer to 1000 nanometers;
2) calibration is with the making of mark: sample is put into focused ion beam system, at distance substrate four angular distances is 1mm~1.5mm scope place, utilize deposition or etching to make calibration mark (or only on a limit, make two marks get final product), deposition materials is selected Pt for use, can select for use the different ions line to deposit or etching according to label size, mark shape and dimension of picture are with easy observation and the calibration of enough details is arranged is principle; Because the high resolving power of focused ion beam system is compared with other label creating technology, guaranteed the precision of follow-up electron beam calibration.Thereby can realize the making of short single nanometer materials test electrode of length; Again scattered nano wire or the conventional method of nanometer tubing utilization are arranged on the above-mentioned substrate;
3) determining of sample coordinate system: with step 2) put into electron-beam exposure system with the sample of monodimension nanometer material pipe or line and calibration mark, the identification point of one jiao of calibration of sample mark is decided to be the sample initial point, it is first point of u axle, to be decided to be sample u axle second point with the identification point of going up another calibration mark on one side, thereby the u axle of sample is determined, the v axle is then vertical with the u axle, and the sample coordinate system is determined;
4) read single nanometer materials pipe or line coordinates: on substrate, find the nanotube (line) that needs, read
Get its unique point coordinate;
5) coating of electron sensitive resist: sample taken out from electron-beam exposure system put into the coating that photoresist spinner carries out electron sensitive resist, electron sensitive resist can adopt positive electronic bundle resists such as PMMA, ZEP520, can select different rotating speeds (1000-7000rpm) or multiple spin coating according to the thickness (50nm-5 μ m) of required electron sensitive resist.Apply the condition of back according to different electron sensitive resists, the temperature and time of baking before selecting, preceding baking can be carried out in hot plate or baking oven, so that the exposure characteristics of electron sensitive resist is fixed;
6) single nanometer materials electrode pattern design: according to shape that reads single nanometer materials and the required electrode pattern of size design;
7) exposure of single nanometer materials potential electrode figure: electron-beam exposure system is put in sample consistent orientation when observing, 3 random sample product u set by step, the v axle, it is in full accord making twice position fixing.According to the coordinate position and the designed electrode of the nanotube that reads (line), determine the exposure reference position.Exposure voltage can be regulated between 1KV-30KV according to the thickness of electron sensitive resist, and the optional value of diaphragm is 7.5,10,20,30,60,120 microns, can select suitable write (a 1-800 μ m) according to electrode size.Select the proper exposure metering according to the conditions of exposure of different electron sensitive resists.The back sample that will expose takes out from electron-beam exposure system, after development, photographic fixing, with N gas sample is dried up at last.Select different back baking temperature and times for use according to the type of different electron sensitive resists, back baking can be adopted hot plate or baking oven.
8) utilize metal coating equipment such as sputter or evaporation to finish the deposition of metal electrode, the plated metal layer thickness is generally 1/3~1/2 of electron sensitive resist thickness, is about tens to the hundreds of nanometer.The sample that has plated metal film is put into the container that acetone is housed, soak about about 10 minutes, and rock container frequently the metal film of unexposed area is come off with electron sensitive resist.The ultrasonic auxiliary metal film that makes unexposed area that can adopt also simultaneously that ultrasonic device carries out the short time with electron sensitive resist fast, come off completely for not carrying out ultrasonic sample, also can adopt the mode of needle injection to realize removing photoresist.
Also comprise the sample that has plated metal film is put into ultrasonic device, carry out ultrasonic PROCESS FOR TREATMENT simultaneously, the metal film that makes unexposed area with electron sensitive resist fast, come off completely for not carrying out ultrasonic sample, adopts the mode of needle injection to realize removing photoresist.
Also comprise step 10), the electrode after step 8) is removed photoresist is under 300-800 ℃ and Ar or N in temperature
2Under the gas shiled, annealing can obtain good Ohmic contact in 1-20 minute, thereby finally realized the making of single nanometer materials test electrode.
The invention has the advantages that:
Method of the present invention is used has the electron-beam exposure system that mobile accuracy is the laser interference sample stage of 2nm, the calibration mark that the utilization focused ion beam system is made, realize that through twice calibration single nanometer materials is in on-chip accurate location, because the high resolving power of focused ion beam system, compare with other label creating technology, guaranteed the precision of follow-up electron beam calibration.Thereby can realize the making of short single nanometer materials test electrode of length, the efficient, accurate of realization nano-electrode made.Can increase the dirigibility that test electrode is made according to the difformity and the required electrode pattern of size design of single nanometer materials simultaneously.Electrode with the preparation of the method for simple application focused ion beam deposition electrode is compared, the defect problem that has not had metallic pollution district and high energy Ga ion to inject and cause.This method is the method for quick, efficient, a pollution-free making single nanometer materials test electrode, have higher flexibility, can make difformity and electrodes sized as required, the precision height, contact performance is good, is fit to the making of various single nanometer materials test electrodes.
Description of drawings
The nano line electrode SEM figure that Fig. 1, prior art utilize FIB to make
Fig. 2, test electrode substrate structure synoptic diagram
Among Fig. 2: 1-backing material 2-insulation course 3-metal electrode layer
Fig. 3, linear pattern single nanometer materials electrode synoptic diagram of the present invention
Among Fig. 3: 4-contact conductor part
D1, D2-contact conductor place space D-four electrode wire spacing
L1, L2, L3, L4-electrode wires
The Ag nano line electrode SEM figure that Fig. 4, the present invention make
Specific embodiment:
Embodiment 1.
Present embodiment is made a single one dimension Ag nano line electrode, and describes structure of the present invention in detail by following concrete making step, and concrete making step is as follows: the backing material 1 of substrate is the Si sheet, and a Si is set thereon
3N
4Insulation course 2, its thickness are 200nm, as shown in Figure 2; Be dispersed with the Ag nano wire on it, two nano wire spacings are about 1mm; Electrode pattern such as Fig. 3, wherein contact conductor part 4 is of a size of 100 * 100 μ m squares, and contact conductor place space D 1 and D2 are 100 μ m, and electrode wires L1, L2, L3, L4 live width are 750nm, and four electrode wires space D are 6 μ m; The Ag nano line electrode SEM figure of made.
Concrete making step: choosing the Si substrate is backing material 1, and the Si that a thickness is 200nm is set thereon
3N
4Insulation course 2.This is provided with Si
3N
4The substrate of insulation course is put into focused ion beam system, at distance substrate four angular distances is arbitrary place within 1mm~1.5mm scope, utilize focused ion beam system to deposit T type Pt mark thereon, be of a size of 2 * 10 μ, height of deposition is about 200nm, ion beam current adopts 100pA, and sedimentation time is about 90 seconds.Method with scattered Ag nano wire utilization spin coating is sprinkling upon on the above-mentioned substrate again, this substrate is put into the electron-beam exposure system calibration again and read the coordinate figure (u1 at Ag nano wire two ends, v1) (u2, v2), can on a slice, seek many nano wires, but two nano wire spacings should be about 1mm, so that the carrying out smoothly of follow-up test work.Electrode pattern such as Fig. 3, wherein contact conductor part 4 is of a size of 100 * 100 μ m squares, and contact conductor place space D 1 and D2 are 100 μ m, electrode wires L1, L2, L3, L4 live width-be 750nm, four electrode wires space D are 6 μ m.Adopt the 495PMMA electron sensitive resist, the spin coating rotating speed is 4000rpm, the thick 200nm that is about of electron sensitive resist this moment, and 180 ℃ of hot plate bakings 1 minute are adopted in preceding baking.Exposure parameter: write a size 100 μ m, accelerating potential 10KV, diaphragm 30 μ m, working depth 5mm, exposure dose 150 μ C/cm
2Develop and adopted MIBK: IPA (1: 3) developing liquid developing 40 seconds, photographic fixing adopts IPA to clean 30 seconds, dries up with drying nitrogen again.100 ℃ of hot plate bakings 1 minute are adopted in the back baking.Metal electrode layer 3 adopts high vacuum magnetron sputtering apparatus sputtered with Ti/Au film (Ti bed thickness 10nm, Au bed thickness 70nm), sample behind the plated film was soaked in acetone soln about 10 minutes, can also be aided with ultrasonic cleaning, the Ti/Au layer of unexposed area is come along with the electron sensitive resist layer remove.And also to be included in temperature be that 300 degree and Ar airshed are under the 1000ml/min, and annealing time is 20 minutes, realizes that at last the Ag nano line electrode makes, and accompanying drawing 4 is the Ag nano line electrode line SEM of the place photo of this method making.
Embodiment 2.
Present embodiment is made one dimension T (or Y) type carbon nanotube electrode, and method for making is with embodiment 1, and its concrete steps are as follows: the substrate of substrate is Si, and insulation course is SiO
2, its thickness is 400nm.T (or Y) type carbon nano-tube is that direct growth obtains in substrate.Utilize focused ion beam system etching T phenotypic marker, be of a size of 2 * 10 μ, the etching height is about 200nm, and ion beam current adopts 200pA, and etching time is about 60 seconds.Read the coordinate of T (or Y) type carbon nano-tube node and three end points.Size design electrode pattern according to T (or Y) type pipe.Adopt the 950PMMA electron sensitive resist, the spin coating rotating speed is 3000rpm, the thick 260nm that is about of electron sensitive resist this moment, and 180 ℃ of hot plate bakings 1 minute are adopted in preceding baking.Exposure parameter: write a size 100 μ m, accelerating potential 10KV, diaphragm 30 μ m, working depth 5mm, exposure dose 200 μ C/cm
2Develop and adopted MIBK: IPA (1: 3) developing liquid developing 40 seconds, photographic fixing adopts IPA to clean 30 seconds, dries up with drying nitrogen again.100 ℃ of hot plate bakings 1 minute are adopted in the back baking.Metal electrode layer adopts high vacuum magnetron sputtering apparatus sputtered with Ti/Pt film (Ti bed thickness 10nm, Pt bed thickness 100nm), sample behind the plated film is soaked about 10 minutes in acetone soln, be aided with ultrasonic cleaning, the Ti/Pt layer of unexposed area is come along with the electron sensitive resist layer remove.Annealing temperature is 800 degree, N
2Airshed is 100ml/min, and annealing time is 2 minutes, realizes the making of T (or Y) type carbon nano-tube test electrode at last.
Embodiment 3
Present embodiment is made the making of a single boron nanowire electrode, and concrete steps are as follows: the substrate of substrate is Si, and insulation course is SiO
2, its thickness is 300nm.The method of scattered boron nanowire utilization spin coating is sprinkling upon on the substrate, utilizes focused ion beam system deposition T type Pt mark, be of a size of 4 * 10 μ, height of deposition is about 400nm, and ion beam current adopts 200pA, and sedimentation time is about 100 seconds.Read the boron nanowire two ends coordinate figure (u1, v1) (u2, v2), according to the size design electrode pattern of boron nanowire.Adopt the ZEP520 electron sensitive resist, the spin coating rotating speed is 3000rpm, the thick 240nm that is about of electron sensitive resist this moment, and 200 ℃ of hot plate bakings 2 minutes are adopted in preceding baking.Exposure parameter: write a size 200 μ m., accelerating potential 30KV, diaphragm 20 μ m, working depth 7mm, exposure dose 180 μ C/cm
2, to develop and adopted the Xylene developing liquid developing 40 seconds, photographic fixing adopts MIBK: IPA (1: 3) and IPA respectively to clean 30 seconds, dries up with drying nitrogen again.100 ℃ of hot plate bakings 2 minutes are adopted in the back baking.Metal electrode layer adopts high vacuum magnetron sputtering apparatus sputter Pd metal film (Pd bed thickness 100nm), in acetone soln, soak the sample behind the plated film about 10 minutes, adopt the needle injection mode, the Pd layer of unexposed area is come along with the electron sensitive resist layer remove.Annealing temperature is 500 degree, and the Ar airshed is 200ml/min, and annealing time is 10 minutes, realizes the making of boron nanowire electrode at last.
Claims (10)
1. the test electrode of a single nanometer materials comprises: thickness is the substrate of 0.5mm~2mm, and one deck is an insulation course above the substrate, the single nanometer materials that is distributing on insulation course and will measure; Size and shape according to single nanometer materials are made metal electrode, and metal electrode comprises and one-dimensional material electrodes in contact line part and the coupling part that is used for measuring lead wire.
2. by the test electrode of the described single nanometer materials of claim 1, it is characterized in that described backing material comprises: any material of silicon chip, quartz or surfacing, its substrate dimension is at least 5 * 5mm size.
3. by the test electrode of the described single nanometer materials of claim 1, it is characterized in that described insulating layer material comprises: SiO
2, Si
3N
4, the adamas insulating material, the thickness of insulation course is 10 nanometer to 1000 nanometers.
4. by the test electrode of the described single nanometer materials of claim 1, it is characterized in that described metal electrode layer material comprises: Ti/Pt and Ti/Au bilayer or metal multilayer film; Or Pd, Au, Cu single-layer metal film, metal layer thickness is 10nm~1000nm.
5. press the test electrode of the described single nanometer materials of claim 1, it is characterized in that, described electrode shape is the electrode figure of linear nano pipe or line always, the electrode figure of this linear pattern nanotube or line is the contact conductor place, and its size and space D 1 to each other, the size of D2 conveniently are as the criterion with follow-up work; The four strip electrode line L1, L2, L3, the L4 minimum feature that directly contact with single nanometer materials are 30nm, and spacing each other is 80nm, and the width D between the four strip electrode lines is equal to or less than the length of 1-dimention nano pipe or wire material.
6. method of making the described single nanometer materials test electrode of claim 1 may further comprise the steps:
1) cleaning of substrate: adopt the three step ultrasonic cleaning in order of acetone, alcohol, secondary deionized water, per step cleaned 3~5 minutes; Adopt conventional method to make insulation course thereon, this insulating layer material comprises: SiO
2, Si
3N
4, insulating material such as adamas, the thickness of insulation course is as the criterion to reach insulation effect;
2) calibration is with the making of mark: the substrate that step 1) is cleaned is put into focused ion beam system, at distance substrate four angular distances is 1mm~1.5mm scope place, the method of utilization deposition or etching is manufactured calibration and is used mark, selects for use the different ions line to deposit or etching according to label size; Again scattered nano wire or the conventional method of tubing utilization are arranged on the above-mentioned substrate;
3) determining of sample coordinate system: with step 2) substrate with one-dimensional nano line or tubing that obtains is put into electron-beam exposure system, the identification point of one jiao of calibration of sample mark is decided to be the sample initial point, first point for the u axle, to be decided to be sample u axle second point with the identification point of going up another calibration mark on one side, after the u axle of sample determined, the v axle was then vertical with the u axle;
4) read single nanometer materials pipe or line coordinates: on substrate, find the nanotube or the line that need test, read its unique point coordinate;
5) coating of electron sensitive resist: sample is taken out from electron-beam exposure system, put into the coating that photoresist spinner carries out conventional electrical bundle resist;
6) single nanometer materials electrode pattern design: come the design electrode pattern according to shape that reads single nanometer materials and size;
7) exposure of single nanometer materials potential electrode figure: will calibrate the sample that the back applies resist and put into the direct electronic beam one-writing system, set by step 3) random sample product coordinate system.Determine the exposure reference position, carry out rotine exposure, development, photographic fixing according to the conditions of exposure of different electron sensitive resists after, with N gas sample is dried up at last, and select different back baking temperature and times for use according to the type of different electron sensitive resists;
8) sample that step 7) is made is put into sputter or evaporated metal filming equipment, finishes the deposition of metal electrode layer, and the thickness of metal electrode layer is 1/3~1/2 of electron sensitive resist thickness; The sample that has plated metal electrode layer is put into the container that acetone is housed, soaked about 10 minutes, the metal film of unexposed area is come off with electron sensitive resist.
7. press the method for the described making single nanometer materials of claim 6 test electrode, it is characterized in that, also comprise the sample that has plated metal film is put into ultrasonic device, the ultrasonic processing technique that the metal film of unexposed area is come off with electron sensitive resist; Or, adopt the mode of needle injection to realize removing photoresist for not carrying out ultrasonic sample.
8. by the method for the described making single nanometer materials of claim 6 test electrode, it is characterized in that also comprise step 9), the electrode after step 8) is removed photoresist is under 300-800 ℃ and Ar or N in temperature
2Under the gas shiled, annealed 1-20 minute.
9. by the method for the described making single nanometer materials of claim 6 test electrode, it is characterized in that, in above-mentioned steps 2) in, electron sensitive resist comprises PMMA or ZEP520 positive electronic bundle resist; Thickness according to required electron sensitive resist is 50nm-5 μ m, and the selection rotating speed is 1000-7000rpm or repeats spin coating more than 2 times during coating.
10. press the method for the described making single nanometer materials of claim 6 test electrode, it is characterized in that, wherein exposure voltage is regulated between 1KV-30KV according to the thickness of electron sensitive resist, diaphragm choosing value is 7.5,10,20,30,60,120 microns, selects a suitable 1-800 μ m that writes according to electrode size.
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