CN102175381A - 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 PDF

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Publication number
CN102175381A
CN102175381A CN 201110058075 CN201110058075A CN102175381A CN 102175381 A CN102175381 A CN 102175381A CN 201110058075 CN201110058075 CN 201110058075 CN 201110058075 A CN201110058075 A CN 201110058075A CN 102175381 A CN102175381 A CN 102175381A
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Prior art keywords
carbon nano
tube
copper
window
pressure
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CN102175381B (en
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赵海涛
陈吉安
王全保
范振民
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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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

Pressure transducer and preparation thereof based on carbon nano-tube and metallic copper composite plating
Technical field
What the present invention relates to is a kind of device and method of pressure transducer technical field, specifically is 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 influence of environment.Utilize piezoresistive effect, piezoelectric effect all can produce pressure transducer, but compare, on volume, weight, environment for use, also have a certain distance with the sensor that the field lift-off technology is made.Pressure transducer based on the field lift-off technology is made has numerous advantages, and advantages such as its collective is long-pending little, in light weight, highly sensitive, bandwidth, corrosion-resistant, compact conformation meet the requirement in outdoor rugged surroundings work.
Find through retrieval prior art, Chinese patent application number 03114812.3 discloses a kind of " nano carbon-base 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.More than two kinds of pressure transducers all be adopt chemical gaseous phase depositing process with carbon nano tube growth on silicon substrate.
But the temperature height that the prior art needs, the impurity in carbon nano-tube is many, influences field emission performance, and carbon nano-tube relies on the stickiness of catalyzer attached on the hearth electrode, and fastness can not get guaranteeing.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, comprising based on carbon nano-tube and metallic copper composite plating: negative electrode, be fixedly set in the anode at negative electrode 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 making 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 to connect 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 copper of sputter 400nm again;
1.4) the two-sided 3 μ m of resist coating again;
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) a 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 copper of sputter 400nm again;
2.12) remove photoresist with acetone soln.
The 3rd step, employing vacuum bonding technology synthesis pressure sensor, concrete operations are:
3.1) earlier 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 big, chemical stability and intensity height, 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 all 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
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 Temperature Influence in actual applications.
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 in light weight, the precision height, and measurement range is wide.
Description of drawings
Fig. 1 is a 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
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, 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, present embodiment comprises: negative electrode 2, be fixedly set in 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 making 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 to connect 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 copper of sputter 400nm again;
D) the two-sided 3 μ m of resist coating again;
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 copper of sputter 400nm again;
L) remove photoresist with acetone soln.
With negative electrode earlier and glass sheet be bonded together, anode is bonded together with glass sheet more then, respectively with wire bonds at negative electrode and anode, promptly 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 (10)

1. pressure transducer based on carbon nano-tube and metallic copper composite plating comprises: negative electrode, be fixedly set in the anode at negative electrode top, and carbon nano-tube in the vacuum chamber between negative electrode and anode and silicon chip, it is characterized in that:
The monocrystalline silicon piece that comprise vacuum window and pressure window two windows of described anode for making by wet etching.
2. the pressure transducer based on carbon nano-tube and metallic copper composite plating according to claim 1 is characterized in that the structure of described pressure window is the square window of 3-5mm, degree of depth 0.2mm, and the structure of vacuum window is: 11 * 11 * 0.6mm.
3. the pressure transducer based on carbon nano-tube and metallic copper composite plating according to claim 1 is characterized in that, is respectively equipped with lead-in wire on described anode and the negative electrode.
4. the pressure transducer based on carbon nano-tube and metallic copper composite plating according to claim 1 is characterized in that 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.
5. the pressure transducer based on carbon nano-tube and metallic copper composite plating according to claim 4 is characterized in that, described glass sheet and silicon chip adopt bonding technology bonding.
6. the pressure transducer based on carbon nano-tube and metallic copper composite plating according to claim 5 is characterized in that the thickness of described chromium-copper layer is 500nm.
7. the preparation method according to the described pressure transducer of above-mentioned arbitrary claim is characterized in that, 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.
8. preparation method according to claim 7 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 copper of sputter 400nm again;
1.4) the two-sided 3 μ m of resist coating again;
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.
9. preparation method according to claim 7 is characterized in that, the 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) a 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 copper of sputter 400nm again;
2.12) remove photoresist with acetone soln.
10. preparation method according to claim 7 is characterized in that, described the 3rd step concrete operations are:
3.1) earlier 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.
CN 201110058075 2011-03-10 2011-03-10 Pressure sensor and preparation method thereof based on composite plating of carbon nano tube and metallic copper Expired - Fee Related CN102175381B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106953001A (en) * 2017-03-24 2017-07-14 中山大学 A kind of pliable pressure sensor based on carbon nano-tube film and photoresist and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
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
JP2006062900A (en) * 2004-08-25 2006-03-09 Matsushita Electric Works Ltd Method for producing carbon nanotube
US20090072836A1 (en) * 2006-04-14 2009-03-19 In Mook Choi Pressure sensor using field emission of carbon nano-tube

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
JP2006062900A (en) * 2004-08-25 2006-03-09 Matsushita Electric Works Ltd Method for producing carbon nanotube
US20090072836A1 (en) * 2006-04-14 2009-03-19 In Mook Choi Pressure sensor using field emission of carbon nano-tube

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
《Electronics Technology》 20091231 Jan Pekarek,et al. Electrodes Modified by Carbon Nanotubes for Pressure Measuring 1-10 , 2 *
《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 20070615 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 , 第6期 2 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106953001A (en) * 2017-03-24 2017-07-14 中山大学 A kind of pliable pressure sensor based on carbon nano-tube film and photoresist and preparation method thereof

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