CN102175381B - Pressure sensor and preparation method thereof based on composite plating of carbon nano tube and metallic copper - Google Patents
Pressure sensor and preparation method thereof based on composite plating of carbon nano tube and metallic copper Download PDFInfo
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- CN102175381B CN102175381B CN 201110058075 CN201110058075A CN102175381B CN 102175381 B CN102175381 B CN 102175381B CN 201110058075 CN201110058075 CN 201110058075 CN 201110058075 A CN201110058075 A CN 201110058075A CN 102175381 B CN102175381 B CN 102175381B
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Abstract
The invention provides a pressure sensor and a preparation method thereof based on composite plating of a carbon nano tube and a metallic copper, which belong to the technical field of pressure sensors. The pressure sensor comprises a cathode, an anode fixedly arranged at the top of the cathode, and a vacuum chamber arranged between the cathode and the anode; the anode is a monocrystalline silicon piece which is produced by a wet etching method and comprises a vacuum window and a pressure window, and the cathode comprises a sheet glass, a monocrystalline silicon piece, a chromium-copper layer, a carbon nano tube-copper composite layer and a carbon nano tube. The pressure sensor provided by the invention has the advantages of small volume and light weight, and can be used both at room temperature and in upper air or other environments.
Description
Technical field
What the present invention relates to is the device and method in a kind of pressure sensor technique field, specifically a kind of pressure transducer and preparation thereof based on carbon nano-tube and metallic copper composite plating.
Background technology
Pressure needs to measure real-time and accurately as an important parameter in the production work.Requirement to sensor comprises that measurement range is wide, is not subjected to the impact of environment.Utilize piezoresistive effect, piezoelectric effect all can produce pressure transducer, but compare with the sensor that the field lift-off technology is made, on volume, weight, environment for use, also have a certain distance.Pressure transducer based on the field lift-off technology is made has many merits, and the advantages such as its collective is long-pending little, lightweight, highly sensitive, bandwidth, corrosion-resistant, compact conformation meet the requirement in outdoor rugged surroundings work.
Find through the retrieval to prior art, Chinese patent application number 03114812.3 discloses a kind of " Nano-carbon based film field-emission pressure sensor ", this technology as field emission source, is obtained the size of ambient pressure with carbon nano-tube by the variation that detects strength of current.The PhD dissertation of Qian Kaiyou " research of carbon nanotube cathod field-emission pressure sensor " is to utilize the field emission principle of carbon nano-tube to make pressure transducer equally.Above two kinds of pressure transducers all be adopt chemical gaseous phase depositing process with carbon nano tube growth on silicon substrate.
But the temperature that the prior art needs is high, and the impurity in carbon nano-tube is many, affects field emission performance, and carbon nano-tube relies on the stickiness of catalyzer to be attached on the hearth electrode, and fastness can not be guaranteed.At present, adopt composite plating method that the pressure transducer that carbon nano-tube firmly is embedded in the metallic copper be yet there are no report at home and abroad.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of pressure transducer and preparation thereof based on carbon nano-tube and metallic copper composite plating is provided, have little, the lightweight advantage of volume, both can at room temperature use, can also in high-altitude or other environment, use.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of pressure transducer based on carbon nano-tube and metallic copper composite plating, comprising: negative electrode, be fixedly installed on the anode of cathode top, and the vacuum chamber between negative electrode and anode, wherein:
The monocrystalline silicon piece that comprise vacuum window and pressure window two windows of described anode for being made by wet etching, wherein: the structure of pressure window is the square window of 3-5mm, degree of depth 0.2mm, the structure of vacuum window is: 11 * 11 * 0.6mm.
Be respectively equipped with lead-in wire on described anode and the negative electrode, be used for connecting power supply and reometer.
Described negative electrode comprises: the glass sheet that from bottom to top sets gradually, monocrystalline silicon piece, chromium-copper layer and carbon nano tube-copper composite bed, carbon nano-tube, wherein: glass sheet and silicon chip adopt bonding technology bonding, and the thickness of chromium-copper layer is 500nm.
The present invention relates to the preparation method of above-mentioned pressure transducer, may further comprise the steps:
The first step, employing carbon nano-tube composite plating process prepare negative electrode, and concrete operations are:
1.1) get the twin polishing monocrystalline silicon piece of 6 * 6mm, thick 500 μ m, single face resist coating 2 μ m;
1.2) wicket of photoetching, as later lead-in wire coupling part;
1.3) double-faced sputter chromium and copper, the chromium of first sputter 100nm, the again copper of sputter 400nm;
1.4) two-sided again resist coating 3 μ m;
1.5) photoetching array window, each array diameter is 0.5mm, is arranged as 5 * 5;
1.6) place negative electrode and in the composite solution of carbon nano-tube and copper, electroplated 30 minutes;
1.7) composite bed of polish, polish flat carbon nano-tube and copper, erode a part of copper and expose carbon nano-tube;
1.8) remove photoresist with acetone soln.
Second step, employing wet etching prepare the sensor anode, and concrete operations are:
2.1) get 15 * 15mm, the two-sided oxidation growth SiO of thick 1000 μ m twin polishing monocrystalline silicon pieces
2, thickness 2.5 μ m;
2.2) two-sided resist coating 3 μ m;
2.3) photoetching vacuum window and pressure window;
2.4) corrosion SiO
2, for etching pressure window and vacuum window are prepared;
2.5) remove photoresist with acetone soln;
2.6) the wet etching pressure window, and a residue part;
2.7) wet etching vacuum window and the remaining part of pressure window;
2.8) erode SiO
2
2.9) two-sided resist coating 2 μ m;
2.10) the photoetching wicket, as later lead-in wire coupling part;
2.11) sputter chromium and copper, sputter chromium and copper, the chromium of first sputter 100nm, the again copper of sputter 400nm;
2.12) remove photoresist with acetone soln.
The 3rd step, employing vacuum bonding technology synthesis pressure sensor, concrete operations are:
3.1) first negative electrode and glass sheet are bonded together under vacuum environment;
3.2) again anode also is bonded on the glass sheet under vacuum environment.
Ultimate principle of the present invention is: the slenderness ratio of carbon nano-tube is large, and chemical stability and intensity are high, and these all are particularly suitable for field emission source.Carbon nano-tube is placed on the negative electrode, apply voltage between anode and cathode after, field emission characteristic will appear in carbon nano-tube.After the distance between anode and cathode changed, the electric current of two interpolars also can change, thereby obtained extraneous pressure by the variation of measuring strength of current.
The performance of pressure transducer of the present invention can be analyzed by the following method.
1) check of pressure transducer
For the relation of inspection pressure and strength of current, can stressed pressure pan with putting into behind the sensor insulating package, by the pressure in the tensimeter regulating tank, each pressure can corresponding electric current number, finally can obtain a pressure---current curve diagram.When using, by measuring the size that electric current also must cicada pressure.
2) elimination of temperature coupling
The variation of temperature can make anode film expand with heat and contract with cold.The experiment of temperature characterisitic is carried out in high-low temperature chamber, makes low temperature by liquid nitrogen, and heating rod is made high temperature.Temperature environment is controlled at-55 ℃～100 ℃, every 5 ℃ of record one strength of current.Can eliminate in actual applications the impact of temperature.
This invention has been used the field emission characteristic of carbon nano-tube and has been made pressure transducer, and the crushed element of sensor is analyzed through optimizing, and sensor bulk is little, and is lightweight, and precision is high, and measurement range is wide.
Description of drawings
Fig. 1 is structural representation of the present invention.
Fig. 2 is the production process charts of anode deformation film.
Fig. 3 is the production process charts of negative electrode.
Embodiment
Embodiment
The below elaborates to embodiments of the invention, and the present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
As shown in Figure 1, the present embodiment comprises: negative electrode 2, be fixedly installed on the anode 1 at negative electrode 2 tops, and the vacuum chamber 3 between negative electrode 2 and anode 1, wherein:
The monocrystalline silicon piece that comprise vacuum window 9 and pressure window 10 two windows of described anode 1 for being made by wet etching, wherein: the structure of pressure window is the square window of 3-5mm, degree of depth 0.2mm, the structure of vacuum window is: 11 * 11 * 0.6mm.
Described negative electrode 2 comprises: the glass sheet 4 that from bottom to top sets gradually, monocrystalline silicon piece 5, chromium-copper layer 6 and carbon nano tube-copper composite bed 7 and carbon nano-tube 8, wherein: glass sheet 4 adopts bonding technology bonding with monocrystalline silicon piece 5, and the thickness of chromium-copper layer 6 is 500nm.
Be respectively equipped with lead-in wire 11 and 12 on described anode 1 and the negative electrode 2, be used for connecting power supply and reometer.
This device prepares in the following manner:
The manufacturing process of negative electrode is:
A) get the twin polishing monocrystalline silicon piece of 6 * 6mm, thick 500 μ m, single face resist coating 2 μ m;
B) wicket of photoetching is as later lead-in wire coupling part;
C) double-faced sputter chromium and copper, the chromium of first sputter 100nm, the again copper of sputter 400nm;
D) two-sided again resist coating 3 μ m;
E) photoetching array window, each array diameter is 0.5mm, is arranged as 5 * 5;
F) placing negative electrode electroplated 30 minutes in the composite solution of carbon nano-tube and copper;
G) polish, the polish flat composite bed of carbon nano-tube and copper erodes a part of copper and exposes carbon nano-tube;
H) remove photoresist with acetone soln.
The manufacturing process of anode is:
A) get 15 * 15mm, the two-sided oxidation growth SiO of thick 1000 μ m twin polishing monocrystalline silicon pieces
2, thickness 2.5 μ m;
B) two-sided resist coating 3 μ m;
C) photoetching vacuum window and pressure window;
D) corrosion SiO
2, for etching pressure window and vacuum window are prepared;
E) remove photoresist with acetone soln;
F) wet etching pressure window, and a residue part;
G) the remaining part of wet etching vacuum window and pressure window;
H) erode SiO
2
I) two-sided resist coating 2 μ m;
G) photoetching wicket is as later lead-in wire coupling part;
K) sputter chromium and copper, the chromium of first sputter 100nm, the again copper of sputter 400nm;
L) remove photoresist with acetone soln.
With negative electrode first and glass sheet be bonded together, then anode is bonded together with glass sheet again, respectively with wire bonds at negative electrode and anode, namely finished the making of a pressure transducer.
When pressure window was of a size of 3 * 3mm, its range was 600kPa, sensitivity 0.18nA/Pa; When pressure window was of a size of 4 * 4mm, its range was 550kPa, sensitivity 0.2nA/Pa; When pressure window was of a size of 5 * 5mm, its range was 500kPa, sensitivity 0.23nA/Pa.
Claims (1)
1. method for preparing based on the pressure transducer of carbon nano-tube and metallic copper composite plating, described pressure transducer comprises: negative electrode, be fixedly installed on the anode of cathode top, and the carbon nano-tube in the vacuum chamber between negative electrode and anode and silicon chip, the monocrystalline silicon piece that comprise vacuum window and pressure window two windows of described anode for being made by wet etching; The method may further comprise the steps:
The first step, employing carbon nano-tube composite plating process prepare negative electrode;
Second step, employing wet etching prepare the sensor anode;
The 3rd step, employing vacuum bonding technology synthesis pressure sensor;
It is characterized in that, described first step concrete operations are:
1.1) get the twin polishing monocrystalline silicon piece of 6 * 6mm, thick 500 μ m, single face resist coating 2 μ m;
1.2) wicket of photoetching, as later lead-in wire coupling part;
1.3) double-faced sputter chromium and copper, the chromium of first sputter 100nm, the again copper of sputter 400nm;
1.4) two-sided again resist coating 3 μ m;
1.5) photoetching array window, each array diameter is 0.5mm, is arranged as 5 * 5;
1.6) place negative electrode and in the composite solution of carbon nano-tube and copper, electroplated 30 minutes;
1.7) composite bed of polish, polish flat carbon nano-tube and copper, erode a part of copper and expose carbon nano-tube;
1.8) remove photoresist with acetone soln;
Described second step concrete operations are:
2.1) get 15 * 15mm, the two-sided oxidation growth SiO of thick 1000 μ m twin polishing monocrystalline silicon pieces
2, thickness 2.5 μ m;
2.2) two-sided resist coating 3 μ m;
2.3) photoetching vacuum window and pressure window;
2.4) corrosion SiO
2, for etching pressure window and vacuum window are prepared;
2.5) remove photoresist with acetone soln;
2.6) the wet etching pressure window, and a residue part;
2.7) wet etching vacuum window and the remaining part of pressure window;
2.8) erode SiO
2
2.9) two-sided resist coating 2 μ m;
2.10) the photoetching wicket, as later lead-in wire coupling part;
2.11) sputter chromium and copper, the chromium of first sputter 100nm, the again copper of sputter 400nm;
2.12) remove photoresist with acetone soln.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110058075 CN102175381B (en) | 2011-03-10 | 2011-03-10 | Pressure sensor and preparation method thereof based on composite plating of carbon nano tube and metallic copper |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110058075 CN102175381B (en) | 2011-03-10 | 2011-03-10 | Pressure sensor and preparation method thereof based on composite plating of carbon nano tube and metallic copper |
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| CN102175381A CN102175381A (en) | 2011-09-07 |
| CN102175381B true CN102175381B (en) | 2013-02-27 |
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| CN 201110058075 Expired - Fee Related CN102175381B (en) | 2011-03-10 | 2011-03-10 | Pressure sensor and preparation method thereof based on composite plating of carbon nano tube and metallic copper |
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| CN106953001B (en) * | 2017-03-24 | 2019-01-22 | 中山大学 | A kind of pliable pressure sensor and preparation method thereof based on carbon nano-tube film and photoresist |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424565A (en) * | 2003-01-09 | 2003-06-18 | 上海交通大学 | Nano-carbon based film field-emission pressure sensor |
| CN1475807A (en) * | 2003-07-18 | 2004-02-18 | 清华大学 | Carbon nano pipe field emission micromachine acceleration instrument |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4556557B2 (en) * | 2004-08-25 | 2010-10-06 | パナソニック電工株式会社 | Method for producing carbon nanotube |
| KR100844513B1 (en) * | 2006-04-14 | 2008-07-08 | 한국표준과학연구원 | Pressure sensor using a Carbon Nanotube field emission |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424565A (en) * | 2003-01-09 | 2003-06-18 | 上海交通大学 | Nano-carbon based film field-emission pressure sensor |
| CN1475807A (en) * | 2003-07-18 | 2004-02-18 | 清华大学 | Carbon nano pipe field emission micromachine acceleration instrument |
Non-Patent Citations (4)
| Title |
|---|
| Jan Pekarek,et al..Electrodes Modified by Carbon Nanotubes for Pressure Measuring.《Electronics Technology》.2009, * |
| JP特开2006-62900A 2006.03.09 |
| 王裕超.金属基碳纳米管（碳纳米纤维）电接触复合电镀层的制备及表征.《中国优秀博硕士学位论文全文数据库（硕士） 工程科技Ⅰ辑》.2007,(第6期), * |
| 钱开友等.碳纳米管场发射压力传感器结构设计与测试.《微细加工技术》.2005,(第2期),69-72. * |
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Granted publication date: 20130227 Termination date: 20160310 |