CN101308108A - Preparation method of sensor embodying one-dimensional nano material sensitive element - Google Patents
Preparation method of sensor embodying one-dimensional nano material sensitive element Download PDFInfo
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- CN101308108A CN101308108A CNA2007100991678A CN200710099167A CN101308108A CN 101308108 A CN101308108 A CN 101308108A CN A2007100991678 A CNA2007100991678 A CN A2007100991678A CN 200710099167 A CN200710099167 A CN 200710099167A CN 101308108 A CN101308108 A CN 101308108A
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Abstract
The invention relates to a process for preparing a sensor containing a one-dimensional nano-material sensing element, which laps a one-dimensional nano-material on a metal electrode couple on a substrate and then utilizes the metal electro-deposition technique to press, cover and fix the one-dimensional nano-material, so as to realize the reliable contact between the one-dimensional nano-material and electrodes. The process comprises the following steps of: 1) adopting the semiconductor technique to form a gold, copper, platinum or nickel metal electrode couple on a silicon chip; 2) lapping the one-dimensional nano-material on the metal electrode couple on the surface of the silicon chip; 3) electrically depositing metallic layers on the surface of the silicon chip lapped with one-dimensional nano-material on the metal electrode couple until the lapped two ends of the one-dimensional nano-material are covered with the deposited metallic layers fully; and 4) taking out the silicon chip and cleaning and drying the silicon chip to complete the connection between the one-dimensional nano-material and the metal electrode couple. The process can rapidly and economically realize the reliable connection between the one-dimensional nano-material and the metal electrode, and has no damage to the one-dimensional nano-material itself, and the batch production can be adopted.
Description
Technical field
The present invention relates to make the process of sensor, particularly a kind of preparation method who includes the sensor of monodimension nanometer material (nanotube, nano wire, nano belt) sensitive element.
Background technology
Nano material has become one of sensing material of tool potentiality because of its high sensitivity and by receiving new physics, the chemical effect that effect brings.Nano material with as receiving the problem that combines of microstructure of senser element carrier, promptly micro-nano is in conjunction with problem, is that sensing characteristics, the structure of giving full play to nano material received one of key issue of senser element.
When using the monodimension nanometer material structure sensor, usually need nano material is connected on the metal electrode.When being overlapped in monodimension nanometer material on the electrode, the contact performance between nano material and the metal electrode is often not good utilizing the whole bag of tricks (as electrophoresis, microoperation, direct growth etc.), and contact resistance is bigger usually, and has Schottky characteristic.For avoiding this situation, the method that adopts at present usually focused ion beam induction and deposition (hereinafter to be referred as FIB) with the nano material of electrode contact position on cover layer of metal, to improve the contact performance (A.Vila of nano material and electrode, F.Hernandez-Ramirez, J.Rodriguez, et al.Fabrication of metallic contacts to nanometre-sizedmaterials using a focused ion beam (FIB) .Materials Science and Engineering C, 2006,26:1063-1066).But because the impact momentum of ion is big, the FIB method usually can be destroyed the surface structure of nano material, causes the variation of material property.FIB technology costs an arm and a leg simultaneously, and operation easier is big, speed is low, brings difficulty for the reliable connection of monodimension nanometer material on metal electrode.
Summary of the invention
The objective of the invention is to: the contact performance that overcomes existing in prior technology nano material and electrode is not good, and the defective that has Schottky characteristic, and overcome existing focused ion beam induction and deposition (FIB) method poor reliability, defect of high cost, thereby provide a kind of preparation method who includes the sensor of monodimension nanometer material sensitive element.
A kind of preparation method who comprises the sensor of monodimension nanometer material sensitive element of the present invention, it is right at first to make metal electrode on substrate; It is characterized in that, monodimension nanometer material is overlapped on on-chip metal electrode to after last, utilize metal electrodeposition technology electro-deposition layer of metal layer on electrode pair, this metal level cover fixedly monodimension nanometer material metal electrode on, realize reliably contact between monodimension nanometer material and electrode, formation comprises the sensor of monodimension nanometer material sensitive element.Method provided by the present invention will be with the surface of metal electrode electro-deposition layer of metal of the monodimension nanometer material with enough bond strengths, and the thickness of metal deposition layer is according to coated electrode fully last monodimension nanometer material being advisable.
In above-mentioned technical scheme, this method can comprise following concrete steps:
1) make electrode pair: the metal electrode of gold, copper, platinum or nickel that the employing semiconductor technology forms on silicon chip is right;
2) at the nonpolar monodimension nanometer material of overlap joint on the electrode pair: silicon chip metal electrode that step 1) makes on overlap monodimension nanometer material;
3) metal level of deposition covers: with above-mentioned steps 2) silicon chip that overlapped monodimension nanometer material puts into electroplating bath,, covered by the metal level that is deposited fully the surface depositing metal layers that powers at metal electrode until the two ends of monodimension nanometer material overlap joint;
4) silicon chip that will deposit metal level takes out, and cleaning, drying is finished monodimension nanometer material and right being connected of metal electrode, forms the sensor that comprises the monodimension nanometer material sensitive element.
In above-mentioned technical scheme, this method is in step 2) in also comprise:
When the monodimension nanometer material that is overlapped is the polarity monodimension nanometer material, after overlap joint is finished metal electrode on apply direct current or the rectangle square-wave voltage carries out electric adsorption treatment, make metal electrode between resistance value＜10
7～10
8Ω realizes Ohmic contact between metal electrode and the monodimension nanometer material.
In above-mentioned technical scheme, described dc voltage value is 1～10V.The peak-to-peak value of described rectangle square-wave voltage is 1～10V, and frequency is 0.1～2000kHz.Described rectangle square-wave voltage comprises symmetry or the asymmetric rectangle square-wave voltage that has biasing.
In above-mentioned technical scheme, the metal electrode in the described step 1) is to being the metallic film of gold, copper, platinum or nickel system.
In above-mentioned technical scheme, step 2) on electrode pair, overlaps monodimension nanometer material described in, adopt method, the method for dielectrophoresis or the method for CVD direct growth of conventional microoperation.
In above-mentioned technical scheme, the metal of described step 3) electro-deposition comprises copper, silver, gold, platinum or the palladium with satisfactory electrical conductivity.
The invention has the advantages that:
A kind of preparation provided by the invention comprises the method for the sensor of monodimension nanometer material sensitive element, by the metal electrodeposition method on monodimension nanometer material and electrode pair, adopt electro-deposition method deposition layer of metal layer, play cover, fixedly monodimension nanometer material is with structure sensor.Reliable connection the between rapid, the economic realization monodimension nanometer material of this method and the metal electrode, and in connection procedure to the no any damage of nano material itself, can complete maintenance himself performance.
Preparation provided by the invention comprises the method for the sensor of monodimension nanometer material sensitive element, also adopt polarity monodimension nanometer material and electrode pair overlapped after, carry out electric adsorption treatment, through realizing Ohmic contact between polarity monodimension nanometer material after the electric adsorption treatment and the metal electrode.Adsorption strength after the electricity adsorption treatment between polarity monodimension nanometer material and metal electrode, in the time of can bearing electrodeposition technology Semi-polarity monodimension nanometer material and enter electrolytic solution, solution surface tension is to the resistance of nano material, guarantees that nano material do not drift about, do not come off.
This method cost is low, and can produce in batches.
Description of drawings
The structural representation of polarity monodimension nanometer material and electrode when Fig. 1 is electric adsorption treatment.
Fig. 2 is the synoptic diagram that electro-deposition of the present invention covers monodimension nanometer material.
The drawing explanation
1, silicon chip 2, metal electrode to 3, the polarity monodimension nanometer material
4, SiO
2 Layer 5, signal generator 6, electroplating bath
7, anode 8, electrolytic solution 9, electrodeposit metals
Embodiment
In detail preparation method of the present invention is described below in conjunction with embodiment and accompanying drawing:
Polarity monodimension nanometer material provided by the invention may further comprise the steps in the process that metal electrode powers on and adsorbs:
1) make electrode pair: the present invention at first adopts semiconductor technology, and for example method of vacuum coating or sputtering method etc. are at the SiO of silicon chip 1
2Form the metal electrode of gold, copper, platinum or nickel film on the layer 4 to 2;
2) at overlap joint polarity monodimension nanometer material on the electrode pair: metal electrode that step 1) is made on, for example adopt the method for microoperation or the method for dielectrophoresis, the two ends of one dimension polar nano line (as zinc paste, gallium oxide etc.) are overlapped on metal electrode to last;
3) use signal generator 5, to the metal electrode two ends that overlapped the polarity monodimension nanometer material, pass to 1～10V direct current or rectangle square-wave voltage (P-to-P voltage 1～10V, frequency 0.1～2000kHz) 5～10 minute, the rectangle square-wave voltage that is applied can be the symmetry or the asymmetric rectangle square-wave voltages of various biasings;
4) measure the overlap joint resistance in circuit judge polarity monodimension nanometer material and metal electrode between bonding state, for monodimension nanometer material and metal electrode to combining qualified standby electrodeposit metals layer.
5) depositing metal layers covers: as shown in Figure 1, silicon chip 1 is put into electroplating bath 6, use platinized platinum anode 7, at the metal electrode of gold, copper, platinum or nickel film to 2 surface electrical deposited gold layers, 9 about 1 μ m, one dimension polar nano line 3 (as zinc paste, gallium oxide etc.) is covered by institute's deposited gold layer 9 fully, form the sensor that comprises one dimension polar nano line sensitive element.
Preparation technology is with embodiment 1 for the absorption of present embodiment electricity, and concrete difference is that monodimension nanometer material is a zinc oxide nano-belt.
1). as shown in Figure 2, the epontic gold electrode of silicon chip 1 to 2 on, adopt method (exchanging frequency 5MHz, voltage peak-to-peak value 10V) the overlap joint zinc oxide nano-belt 3 of dielectrophoresis;
2). in above-mentioned steps 1) overlap joint made on the silicon chip 1 of zinc oxide nano-belt 3, be 10V to gold electrode to applying peak-to-peak value on 2, frequency is the rectangle square-wave voltage of 400Hz, application time is 10 minutes;
3). measure gold electrode to the resistance between 2, resistance＜10
7Ω is qualified;
4). the metal level of deposition covers: as shown in Figure 1, silicon chip 1 is put into electroplating bath 6, uses platinized platinum anode 7, at gold electrode to 2 surface electrical deposited gold layers, 9 about 1 μ m, zinc oxide nano-belt 3 is covered by institute's deposited gold layer 9 fully, form the sensor that comprises the monodimension nanometer material sensitive element.
Present embodiment carries out the electrolytic solution 8 of deposited Au layer 9 and selects the sulphite plating bath, the sulphite electroplate liquid formulation:
Ammonium sulfite 150g/l
Gold 6g/l
Potassium citrate 80g/l
PH 8.5；
The technology of deposited Au layer 9 is as follows:
45 ℃ of temperature
Cathode-current density 0.5A/dm
2
Time 10min
5. silicon chip 1 is taken out, cleaning, drying is finished being connected of zinc oxide nano-belt 3 and gold electrode 2.
The sensor of present embodiment preparation adopts nonpolar monodimension nanometer material carbon nano-tube, and the preparation electrode pair is identical with embodiment 1 with the overlap joint monodimension nanometer material on silicon chip, and its difference is as follows:
1). adopt the method for CVD technology direct growth, utilize the air-flow guiding to make the catalyzer cross growth of carbon nano-tube, be implemented in silicon chip 1 epontic platinum electrode and on 2, overlapped carbon nano-tube 3 from silicon chip 1 edge;
2). reference diagram 1, with above-mentioned steps 1) overlap joint made the silicon chip 1 of carbon nano-tube 3 put into electroplating bath 6, use stainless steel anode 7, at platinum electrode to 2 surface electrical copper layer 9, covered by institute's copper layer 9 fully until carbon nano-tube 3, form the sensor that comprises the monodimension nanometer material sensitive element; Copper layer 9 thickness that wherein deposited are 500nm.
Present embodiment carries out the electrolytic solution 8 of electric deposited copper floor 9 and selects pyrophosphate plating solution, the pyrophosphate plating solution prescription:
Cupric pyrophosphate 60g/l
Potassium pyrophosphate 280g/l
Ammonium citrate 20g/l
PH 8.5；
The technology of electric deposited copper floor 9 is as follows:
30 ℃ of temperature
Cathode-current density 1A/dm
2
Time 5min;
3). silicon chip 1 is taken out, and cleaning, drying is finished being connected of carbon nano-tube 3 and platinum electrode 2.
Claims (9)
1, a kind of preparation method who comprises the sensor of monodimension nanometer material sensitive element, it is right at first to make metal electrode on substrate; It is characterized in that, with monodimension nanometer material be overlapped in the metal electrode that forms on the substrate on after, utilize metal electrodeposition technology electro-deposition layer of metal layer on electrode, this metal level cover fixedly monodimension nanometer material metal electrode on, form the sensor that comprises the monodimension nanometer material sensitive element.
2, the preparation method of sensor according to claim 1 is characterized in that, this method may further comprise the steps:
1) adopt the metal electrode of gold, copper, platinum or nickel that semiconductor technology forms on silicon chip right;
2) the metal electrode of silicon chip surface on overlap monodimension nanometer material;
3) with above-mentioned steps 2) the good monodimension nanometer material silicon chip of overlap joint that makes puts into electroplating bath, and to the depositing metal layers that powers on, the two ends that are overlapped on the electrode pair until monodimension nanometer material are covered by the metal level that is deposited fully at metal electrode;
4) silicon chip is taken out, cleaning, drying is finished monodimension nanometer material and right being connected of metal electrode, forms the sensor that comprises the monodimension nanometer material sensitive element.
3, the preparation method of sensor according to claim 2 is characterized in that, in step 2) in also comprise:
When the monodimension nanometer material that is overlapped is the polarity monodimension nanometer material, after overlap joint is finished metal electrode on apply direct current or the rectangle square-wave voltage carries out electric adsorption treatment, make metal electrode between resistance value＜10
7～10
8Ω realizes Ohmic contact between metal electrode and the monodimension nanometer material.
4, according to the preparation method of claim 1,2 or 3 described sensors, it is characterized in that the metallic film of the metal electrode in the described step 1) to making for gold, copper, platinum or nickel material.
According to the preparation method of claim 1,2 or 3 described sensors, it is characterized in that 5, the layer of metal of described step 3) electro-deposition comprises copper, silver, gold, platinum or the palladium with electric conductivity.
6, the preparation method of sensor according to claim 2 is characterized in that, described step 2) adopt microoperation method, dielectrophoresis method or CVD direct growth method metal electrode on overlap monodimension nanometer material.
7, the preparation method of sensor according to claim 3 is characterized in that, the described dc voltage value that applies is 1～10V.
8, the preparation method of sensor according to claim 3 is characterized in that, the described peak-to-peak value that applies the rectangle square-wave voltage is 1～10V, and frequency is 0.1～2000kHz.
9, the preparation method of sensor according to claim 3 is characterized in that, the described rectangle square-wave voltage that applies comprises symmetry or the asymmetric rectangle square-wave voltage that has biasing.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183201A (en) * | 2011-02-20 | 2011-09-14 | 汪小知 | Low-dimensional nano material-based sensor for measuring mechanical deformation |
| CN102222730A (en) * | 2011-06-27 | 2011-10-19 | 北京航空航天大学 | Method for preparing ultraviolet sensor with gallium oxide one-dimensional sub-micrometer structure |
| CN103114319A (en) * | 2011-11-17 | 2013-05-22 | 盛美半导体设备（上海）有限公司 | Method and device for realizing deep hole uniform metal interconnection on semiconductor silicon chip |
| CN104538293A (en) * | 2014-12-30 | 2015-04-22 | 清华大学 | Method for preparing gold nano array structure on target electrode of chip structure |
| CN105474494A (en) * | 2013-08-26 | 2016-04-06 | 三菱电机株式会社 | DC power generation system and protection method for DC power generation system |
| CN103114319B (en) * | 2011-11-17 | 2016-12-14 | 盛美半导体设备（上海）有限公司 | The method and apparatus of deep hole homogeneous metal interconnection on semi-conductor silicon chip |
| US9666426B2 (en) | 2011-06-24 | 2017-05-30 | Acm Research (Shanghai) Inc. | Methods and apparatus for uniformly metallization on substrates |
Family Cites Families (4)
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| JP3902883B2 (en) * | 1998-03-27 | 2007-04-11 | キヤノン株式会社 | Nanostructure and manufacturing method thereof |
| CN100437120C (en) * | 2004-11-17 | 2008-11-26 | 中国科学院物理研究所 | Testing electrode of single nanometer materials and production thereof |
| CN100443893C (en) * | 2005-12-29 | 2008-12-17 | 上海交通大学 | Manufacturing method of microgas sensor based on one-dimension manometer material |
| CN100428500C (en) * | 2006-01-13 | 2008-10-22 | 清华大学 | One-dimensional nanometer semiconductor structure based photoelectric sensor and its manufacturing method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102183201A (en) * | 2011-02-20 | 2011-09-14 | 汪小知 | Low-dimensional nano material-based sensor for measuring mechanical deformation |
| US9666426B2 (en) | 2011-06-24 | 2017-05-30 | Acm Research (Shanghai) Inc. | Methods and apparatus for uniformly metallization on substrates |
| CN102222730A (en) * | 2011-06-27 | 2011-10-19 | 北京航空航天大学 | Method for preparing ultraviolet sensor with gallium oxide one-dimensional sub-micrometer structure |
| CN103114319A (en) * | 2011-11-17 | 2013-05-22 | 盛美半导体设备（上海）有限公司 | Method and device for realizing deep hole uniform metal interconnection on semiconductor silicon chip |
| CN103114319B (en) * | 2011-11-17 | 2016-12-14 | 盛美半导体设备（上海）有限公司 | The method and apparatus of deep hole homogeneous metal interconnection on semi-conductor silicon chip |
| CN105474494A (en) * | 2013-08-26 | 2016-04-06 | 三菱电机株式会社 | DC power generation system and protection method for DC power generation system |
| CN105474494B (en) * | 2013-08-26 | 2017-10-03 | 三菱电机株式会社 | The guard method of DC power generation system and DC power generation system |
| CN104538293A (en) * | 2014-12-30 | 2015-04-22 | 清华大学 | Method for preparing gold nano array structure on target electrode of chip structure |
| CN104538293B (en) * | 2014-12-30 | 2017-05-24 | 清华大学 | Method for preparing gold nano array structure on target electrode of chip structure |
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