CN106323525B - A kind of carbon nanotubes wall surface windage force snesor and preparation method thereof - Google Patents
A kind of carbon nanotubes wall surface windage force snesor and preparation method thereof Download PDFInfo
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- CN106323525B CN106323525B CN201610741449.2A CN201610741449A CN106323525B CN 106323525 B CN106323525 B CN 106323525B CN 201610741449 A CN201610741449 A CN 201610741449A CN 106323525 B CN106323525 B CN 106323525B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
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- G01M9/06—Measuring arrangements specially adapted for aerodynamic testing
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Abstract
The present invention relates to a kind of carbon nanotubes wall surface windage force snesors, core component includes sensor chip (6), wherein, sensor chip (6) composition specifically includes that organic glass substrate (1), one layer of Parylene C (2) in substrate, gold electrode (3) and the conducting wire (7) and carbon nanotubes (5) for connecting gold electrode.The sensor is for measuring macroturbulence boundary layer friction power, the present invention is formed according to above-mentioned component, focus primarily upon the sensor machining process, optimize manufacture craft to improve sensor space and temporal resolution, to improve its application, expand its application range, to be applied to the complicated turbulent boundary layer frictional force of measurement, measurement accuracy and index are above existing wall surface shear stress measurement product at present.
Description
Technical field
Aeronautical material technical field of the present invention specifically designs a kind of carbon nanotubes wall surface windage force snesor and its system
Preparation Method.
Background technique
China is as international big country, in Aeronautics and Astronautics or even national defense applications, the research and development of various high-speed aircrafts there is an urgent need to
Accurate and real-time measurement wall surface air friction.And wall friction force measuring method can be divided into direct or indirect two major classes.Directly
Type wall friction force snesor can by a microsprings (or other means) support rocker piece go balance wall friction power,
Equilibrant force, which can pass through spring deflection and convert, to be obtained.The deflection can be measured by electronics or optical instrument.It floats
Block has relatively high sensitivity and very high response frequency.The method of measurement wall friction power is divided into three kinds indirectly: (1) base
In calorifics principle, i.e., based on by calibration local wall frictional force and sensing element convective heat transfer relationship, such as hotting mask and
Wall surface hot line；(2) non-thermal method, such as Preston tube and Stanton tube, thin oil film interferometry, liquid crystal coatings method, micro-
Post jamb face friction force sensor and wall surface pulsation line etc.；(3) average velocity gradient extrapolation, the measurement of velocity gradient can be with
Use particle image velocimeter or hot line.
In turbulent boundary layer control (for the purpose of such as to reduce frictional resistance), it usually needs extract wall surface from flowing and rub
Wipe the real-time feedback information of power and its distribution.Turbulent boundary layer closed-loop control experimental study shows compared to other flow parameters,
Wall surface is used to flow to or open up the closed-loop control for being more advantageous to turbulent boundary layer for feedback signal to frictional force.Measure wall friction power
It can not only predict the flowing coherent structure of downstream near wall, and can directly assess closed-loop control effect.Therefore, realization pair
The accurate and real-time measurement of turbulent boundary layer wall friction power, and unstable turbulence boundary layer Complex Flows mechanism is deeply understood
And meet the needs of real-time control, become that current hydrodynamics discipline development is most challenging, direction of forefront.And this
The breakthrough of direction research work, key are to develop novel, the available wall friction with high-spatial and temporal resolution conscientiously
Force test system, the key for designing the system are to produce the sensing element for being satisfied with system operation.
In recent years, turbulent boundary layer is studied and controlled using microsensor have become a main trend.But it is domestic about
The research of the measurement method of turbulent boundary layer wall friction power is few, and the research and development of sensor are also less.
During gradually developing and improving, application range also becomes increasingly wall surface air friction measuring technique
Extensively.But in application existing measuring technique measurement high reynolds number turbulent flow wall friction power, various defects are exposed, such as
Preston tube and Stanton tube, thin oil film interferometry, liquid crystal layer method, average velocity gradient method etc. can only all measure wall surface
The average value of frictional force can not differentiate the pulsating quantity of wall surface frictional force in turbulent boundary layer.The dynamic response of Thermomembrane method is no more than
400Hz.Direct-type sensor processing and installation based on rocker piece is all extremely difficult.Largely surveyed using sensors with auxiliary electrode
In the case where amount, influence of the gap to flowing between rocker piece and wall surface also be can not ignore.Although micro-electro-mechanical sensors have
High-spatial and temporal resolution, but sensing element need by extremely complex technical process and very strict condition (such as temperature and
Time) under manufactured, thus limit it and be widely applied.
Summary of the invention
The technical problem to be solved in the present invention is that low, dynamic is rung for traditional wall surface friction force sensor spatial resolution
Answer the defects of frequency is low, processing and installations of traditional sensors are difficult, a kind of carbon nanotubes wall surface windage force snesor and
Preparation method.
The present invention is achieved through the following technical solutions: a kind of carbon nanotubes wall surface windage force snesor, core
Part includes sensor chip (6), wherein sensor chip (6) composition specifically includes that organic glass substrate (1), in substrate
One layer of Parylene C (2), gold electrode (3) is provided on Parylene C layer and connects the conducting wire of gold electrode
(7), the gold electrode (3) is two or more, and the carbon nanotubes (5) between gold electrode (3).
Further, it is provided with the photoresist layer of exposure on the gold electrode (3), is preferably provided with development on photoresist layer
Layer.
It is preferred that organic glass substrate 2mm is thick, 0.5 μ m-thick of Parylene C, the preferably gold electrode of 0.7 μ m-thick, and
Carbon nanotubes beam diameter is about 10-30nm, and length is 1-10 μm.It is each to belong to a kind of carbon nanotubes wall surface windage force snesor
The optimal size of component, and the performance that best performance is realized in advance.
In the present invention, sensor sensing element material is carbon nanotubes, is carbon nanotubes when specifically used.
A further object of the present invention is to provide a kind of preparation methods of carbon nanotubes wall surface windage force snesor: packet
Include following 8 steps:
(a) organic glass substrate (1) is rinsed with isopropanol, then its surface is cleaned with deionized water,
To achieve the purpose that remove surface impurity；
(b) organic glass substrate (1) is dried up, one layer of Parylene C (2) is placed on organic glass substrate (1)
Coating；Wherein, the Parylene C (2) is used to protect organic glass substrate (1) and reinforces gold electrode (3) and substrate
(1) bonding between；
(c) ion sputtering film coating method is used, one layer of gold electrode (3) is laid on Parylene C coating (2)；
(d) spin coating photoresist and the soft baking of use on gold electrode, is pre-processed；
(e) photoresist is exposed by mask plate using litho machine, then the spraying developer solution on photoresist (4),
Finally rinsed with deionized water；
(f) gold electrode (3) is etched with gold etchant, is then rinsed with deionized water, remove impurity；
(g) photoresist (4) of unfinished exposure acetone and deionized water are rinsed, obtains required pattern；
(h) by AC dielectric swimming (DEP) technology, manipulation arrangement carbon nanotubes (5) is connected into pairs gold electrode (3), most
Form sensor chip (6) afterwards；By thermal anneal process, wherein impure impurity is removed, the work of stability sensor resistance is played
With finally completing the arrangement of carbon nanotubes.
Further, the last access measurement that is connected with printed circuit board is passed through using preceding method carbon nanotube sensor chip
Circuit.After sensor chip (6) and circuit integration, sensor is tested, I-V (current-voltage) curve is obtained.
In sensor of the present invention, under room temperature state, the I-V curve of carbon nanotube sensor chip (6) is determined.
Carbon nanotube sensor chip (6) temperature-coefficient of electrical resistance is obtained by I-V curve, calculates carbon nanotube sensor chip (6) energy
Amount consumption.
The working principle of sensor of the present invention is as follows: due to spontaneous heating, the work temperature of nano-sensor chip (6)
It spends (T) and is higher than environment temperature (T0).The electrical resistance overheats ratio α of nano-sensor chip (6)RIs defined as:
αR=(R-R0)/R0 (a)
Wherein R0The resistance value that do not generate heat respectively with R with nano-sensor chip (6) under spontaneous heating.Pass through formula (a)
Nano-sensor chip (6) α that can be calculatedRWith the change curve of voltage V.Obtained measurement result can be multinomial with second order
Formula expression, i.e. I ≈ AV2+ BV, A and B are respectively the curve coefficients obtained after being fitted.The formula shows the sensing element electricity of spontaneous heating
Flow increase an order of magnitude faster than the increase of voltage V of I.Thus it obtains
αR≈[(AV+B)R0]-1-1 (b)
Formula (b) shows αRIt is inversely proportional with voltage V.αRSelection depend on two factors: 1. input currents cannot be too big, no
Then nano-sensor chip (6) structure can be destroyed.2. nano-sensor chip (6) self-heating temperature cannot be excessively high, otherwise can
Nature convection phenomena is generated around it, and interference is generated to flow field around.So αRIt must be limited within the scope of some, αRMost
Small value will depend on measurement result.
In sensor of the present invention, the temperature coefficient α of resistance be used to describe the resistance of nano-sensor chip (6) with
Temperature change and change characteristic, is defined as:
Thus the relationship of temperature and electrical resistance overheats ratio is obtained:
αR=α αTT0 (d)
In sensor of the present invention, carbon nanotubes sensing element (R-R0)/R0(%) is with T0The variation of (DEG C).
In sensor of the present invention, the sensitivity S of sensor is by sensing element output voltageIt is averaged with what is measured
Wall surface shear stress (frictional force)Quantitative relationship determine, it may be assumed that
With the increase of convective heat transfer near wall, parameter A value increases, and sensitivity is reinforced therewith.It is sensed by calibration
Device determinesWithQuantitative relationship, can get sensor in the case that it is different overheat ratio sensitivity Ss.
Compared with the prior art, the beneficial effects of the invention include:
Sensor of the present invention is for measuring macroturbulence boundary layer friction power.The sensor tracks turbulence pulsation
Ability depend on its dynamic response frequency i.e. time response feature.The sensor is made using single-wall carbon nanotubes (5)
For sensing element, under constant current (CC) operating mode, sensor can reach the response frequency of 177kHz.Wherein, carbon nanotubes passes
The output noise of sensor can be predicted by the standard deviation of sensor resistance.The sensor is restrained using functionalized nano carbon
As sensing element, typical output noise of the sensor under non-overheat setting is predicted between 0.1-0.2%, with external circuits
It compares, intrinsic noise accounts for the 90% of overall noise ratio.
The present invention is formed according to the sensor component, focuses primarily upon the sensor machining process, optimization production
Technique improves sensor space and temporal resolution, to improve its application, expands its application range, to be applied
In the turbulent boundary layer frictional force that measurement is complicated, measurement accuracy and index are above existing wall surface shear stress measurement at present
Product.
In sensor of the present invention, when using hot-wire measurement turbulent flow, constant temperature measurement circuit module is generally used for arteries and veins
Dynamic tachometric survey, and constant current is then used for fluctuating temperature measurement, application range further expansion.
Sensor of the present invention has high spatial and temporal resolution.In the micron-scale, dynamic response is spatial resolution
100kHz or more.Its sensing element energy consumption is extremely low, and in microwatt level, draw ratio is very big, 103The order of magnitude, and manufacture craft
Simply.
Detailed description of the invention
Fig. 1 is the production schematic diagram of sensing element, 1 (a) to 1 (h) preparation process for respectively representing each layer in figure.
Fig. 2 is sensor chip top view
Fig. 3 is Survey Software flow chart
Wherein, organic glass substrate (1), Parylene C layer (2), gold electrode (3), photoresist (4), carbon nanotubes
Beam (5), sensor chip (6), conducting wire (7), (8) solder joint, (9) weld tabs.
Specific embodiment
The present invention uses sensing element of the carbon nanotubes as novel wall surface air friction sensor, is made by optimization
Technique and working method improve sensor space and temporal resolution, increase the practical of sensor using system software
Property.
The specific embodiment of sensor of the invention manufacture craft and working method is discussed in detail with reference to the accompanying drawing, but
The present invention is not limited to this:
A kind of carbon nanotubes wall surface windage force snesor of embodiment 1 and preparation method thereof (shown in such as 1 (a) to 1 (h))
(a) firstly, with isopropanol to a 3mm thickness, side length is that the rectangular organic glass substrate (1) of 3cm is rinsed.So
Its surface is cleaned with deionized water afterwards.
(b) then, organic glass substrate (1) is dried up with pure nitrogen (N2).Use Labcoter (Specially
Coating SystemTM) Parylene C (2) of one layer of 0.5 μ m-thick is placed on organic glass substrate (1) for protecting
It protects organic glass substrate (1) and reinforces the bonding between gold electrode (3) and substrate (1).
(c) ion sputtering film coating method is used, gold target connects anode, has the organic glass of one layer of Parylene C (2)
Substrate (1) connects cathode, after passing to three to five kilovolts of high voltage direct currents, generates arc between gold target and organic glass substrate (1)
Light electric discharge.Argon gas under electric field action in the vacuum (-tight) housing of part is ionized, to be formed around cathode organic glass substrate (1)
The sub- dark space of one leafing.Argon ion is bombarded workpiece surface, makes organic glass substrate (1) surface layer particle by the attraction of cathode negative high voltage
It is banged to splash with foul and be dished out, the surface to be plated of organic glass substrate (1) is made to have obtained sufficient icon bombardment cleaning.Then, will
Gold target connects AC power source, and the fusing of gold target particle is evaporated and is ionized.Gold ion rushes under cathode attraction in company with argon ion together
To organic glass substrate (1), when the evaporated ions that throwing is plated on organic glass substrate (1) surface are more than to splash the quantity for losing ion
When, then it is gradually accumulated to form one layer of secure adhesion in the coating on organic glass substrate (1) surface, that is, completes in polychlorostyrene generation to diformazan
The gold electrode (3) of one layer of 0.7 μ m-thick is laid on benzene coating (2).
(d) rotten quarter is carried out to it using photoetching process.Firstly, being operated AZ5214-E photoresist (4) with two steps in golden electricity
Pole is laid on (3), and with revolving speed gluing 6 seconds of 500 turns per minute, second step was applied the first step with 3000 turns of revolving speed per minute
Glue 30 seconds.Later, on hot plate with 70 DEG C it is soft dry 1 minute.
It (e) is 9mW/ with uitraviolet intensity by mask plate using litho machine (Karl Suss MA6 Mask Aligner)
Cm2 is exposed it.Then (4) spraying developer solution on a photoresist, is finally rinsed with deionized water.
(f) gold electrode (3) is etched with golden etchant (KI:I2:H2O=4:1:80).
(g) unexposed photoresist (4) are rinsed with acetone and deionized water.
(h) carbon nanotubes (5) are ultrasonically treated to reduce its aggregation extent, the carbon nanotubes (5) of 5mg are molten
The solution of 0.01mg/ml is made in the alcohol of 500ml in solution.The sensor chip tentatively made before (6) is placed in vacuum
Under environment, its gold electrode (3) is operated with microprobe under the microscope.It is 16V with peak-to-peak value, frequency is the typical case of 1MHz
AC power source excites gold electrode (3).At the same time, the carbon nanotubes/alcoholic solution that will be about 10 μ L is injected into sensing
Between two gold electrodes (3) on device.With the evaporation of alcohol, left carbon nanotubes will pass through gold electrode to (3)
Gap, the gold electrode being connected into pairs (3).Finally, sensor chip (6) passes through 60 DEG C of thermal anneal process, solvent is evaporated, removes it
In impure impurity.It can play the role of stability sensor chip (6) resistance in this way.
A kind of carbon nanotubes wall surface windage force snesor described in embodiment 2 and preparation method thereof
On the basis of embodiment 1, another program includes: (a) using clean organic glass (PMMA) as substrate.It is rectangular
Organic glass substrate side length 3cm, thickness 3mm.
(b) in organic glass base top, the Parylene C of 0.5 μ m-thick of layer overlay, for protecting organic glass
Bonding between glass substrate and reinforcement gold electrode and substrate.
(c) by sputtering and rotten needle drawing case, gold electrode and the company of 0.7 μ m-thick are arranged on Parylene C coating
Connect the conducting wire of gold electrode.
(d) by AC dielectric swimming (DEP) technology, manipulation arrangement carbon nanotubes are connected into pairs gold electrode (paired electrode
Between gap be 2 μm), eventually form the sensing element of sensor chip.By thermal anneal process, can remove wherein impure
Impurity plays the role of stability sensor resistance.
3 performance test of embodiment
A kind of carbon nanotubes wall surface windage force snesor prepared using 1 the method for embodiment, using aforementioned side
Method carbon nanotube sensor chip is by the last access measuring circuit that is connected with printed circuit board, as shown in Figure 2.
The carbon nanotubes wall friction force test system technical indicator is as shown in table 1:
1 carbon nanotubes wall friction force test system technical indicator of table
As shown in figure 3, carbon nanotube sensor system software is divided into three parts: pre-treatment in the present embodiment, acquisition, after
Processing.Pre-treatment first measures sensor resistance, and according to gained resistance value and overheat ratio, it is (permanent to adjust measuring circuit
Circuit temperature and constant-current circuit are general) variable resistance R in electric bridge3Trim bridge circuit.Then electricity is determined by square-wave test
Response and response frequency of the sensor to pulse signal in bridge.Finally be set as needed output signal DC compensation and
Gain, reducing measurement error keeps the data measured more accurate.Collecting part is calibration sensor first.It is passed in the present embodiment
The calibration of sensor chip measures wind speed by Pitot tube, to obtain the wall shear stress at sensorIt senses at the same time
Element output voltage isChange wind speed to obtainWithCorresponding relationship, be fitted and obtain relationship
After the completion of calibration, setting sample frequency and acquisition data volume, system carry out data acquisition.Software last part is post-processing,
Preliminary analysis can be carried out to the data of acquisition.Analysis method include calculate the average value of data, root-mean-square value, spectrum analysis, from
Correlation analysis, VITA analysis etc..
Using the spatial distribution of carbon nanotubes sensing element array measurement boundary layer wall friction power, by analyzing shear stress
With flow field data, thus be able to further investigation wall friction power and boundary layer coherent structure interaction and relationship.
Test result are as follows: for the sensor under constant current (CC) operating mode, sensor can reach the response frequency of 177kHz
Rate, typical output noise of the prediction sensor under non-overheat setting is between 0.1-0.2%, compared with external circuits, inherently
Noise accounts for the 90% of overall noise ratio.In the micron-scale, dynamic response is 100kHz or more, sensing element energy consumption to spatial resolution
Extremely low, in microwatt level, draw ratio is very big, 103The order of magnitude.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (4)
1. a kind of carbon nanotubes wall surface windage force snesor, it is characterised in that: core component includes sensor chip (6),
Wherein, sensor chip (6) composition specifically includes that organic glass substrate (1), one layer of Parylene C in substrate
(2), it is provided with gold electrode (3) on Parylene C layer and connects the conducting wire (7) of gold electrode, the gold electrode (3) is two
More than a, it is provided with the photoresist layer of exposure on the gold electrode (3), developing layer is provided on photoresist layer, and be located at gold
Carbon nanotubes (5) between electrode (3)；
The preparation method of the sensor includes:
(a) organic glass substrate (1) is rinsed with isopropanol, then its surface is cleaned with deionized water；
(b) organic glass substrate (1) is dried up, one layer of Parylene C (2) is placed on organic glass substrate (1) and is applied
Layer；
(c) ion sputtering film coating method is used, one layer of gold electrode (3) is laid on Parylene C coating (2)；
(d) spin coating photoresist and soft baking is carried out on gold electrode；
(e) photoresist is exposed by mask plate using litho machine, then the spraying developer solution on photoresist (4), finally
It is rinsed with deionized water；
(f) gold electrode (3) is etched with gold etchant, is then rinsed with deionized water；
(g) photoresist (4) of unfinished exposure acetone and deionized water are rinsed；
(h) by AC dielectric swimming skills art, manipulation arrangement carbon nanotubes (5) is connected into pairs gold electrode (3), eventually forms sensing
Device chip (6)；By thermal anneal process, wherein impure impurity is removed.
2. a kind of carbon nanotubes wall surface windage force snesor according to claim 1, it is characterised in that: organic glass
Substrate 2mm is thick, and 0.5 μ m-thick of Parylene C, the gold electrode and carbon nanotubes beam diameter of 0.7 μ m-thick are about 10-
30nm, length are 1-10 μm.
3. a kind of carbon nanotubes wall surface windage force snesor described in claim 1-2 any claim is for measuring
The application of macroturbulence boundary layer friction power.
4. application according to claim 3, comprising: passed through using preceding method carbon nanotube sensor chip electric with printing
Road plate, which is connected, finally accesses measuring circuit, after sensor chip (6) and circuit integration, tests sensor, obtains I-V
(current-voltage) curve.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101344447A (en) * | 2007-07-13 | 2009-01-14 | 清华大学 | Micro-electromechanical pressure transducer |
| CN102313625A (en) * | 2011-05-27 | 2012-01-11 | 北京大学 | Pirani vacuum gauge of carbon nanotube and vacuum degree detection method thereof |
| CN102313818A (en) * | 2011-07-18 | 2012-01-11 | 清华大学 | Flexible pressure resistance flow field sensor based on single-wall carbon nanotube array and manufacturing method thereof |
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| JPH06254668A (en) * | 1993-03-08 | 1994-09-13 | Toyota Motor Corp | Method for regulating punching force of knock hammer and method for specifying defective portion |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101344447A (en) * | 2007-07-13 | 2009-01-14 | 清华大学 | Micro-electromechanical pressure transducer |
| CN102313625A (en) * | 2011-05-27 | 2012-01-11 | 北京大学 | Pirani vacuum gauge of carbon nanotube and vacuum degree detection method thereof |
| CN102313818A (en) * | 2011-07-18 | 2012-01-11 | 清华大学 | Flexible pressure resistance flow field sensor based on single-wall carbon nanotube array and manufacturing method thereof |
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