CN109884119A - A kind of hydrophilic quartz resonance dew point recognition methods - Google Patents
A kind of hydrophilic quartz resonance dew point recognition methods Download PDFInfo
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- CN109884119A CN109884119A CN201910145129.4A CN201910145129A CN109884119A CN 109884119 A CN109884119 A CN 109884119A CN 201910145129 A CN201910145129 A CN 201910145129A CN 109884119 A CN109884119 A CN 109884119A
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- dew
- dew point
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- molybdenum disulfide
- montmorillonite
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Abstract
The present invention discloses a kind of hydrophilic quartz resonance dew point recognition methods, and this method has three big steps: step 1: preparation has the dew point transducer core dew cell of two-dimensional material nano thin-film；Step 2: double chill surface dew point transducer devices with active temperature control function are assembled；Step 3: Fourier's the Fitting Calculation is first carried out to the frequency signal of sensor device output, second order derivation then is carried out to fitting result, by finding the extreme value inflection point of second dervative, the inflection point moment temperature on corresponding dew cell surface is dew-point temperature.This method is available accurate and unique characteristic quantity is used to identify dew point, and can exclude influence of the warm frequency characteristic to measurement accuracy.
Description
Technical field
The present invention relates to intelligence manufacture, precision instrument and instrument fields, micro- more particularly to a kind of hydrophilic quartz crystal
The preparation method of balance sensing element and data extraction method to the characteristic value that can reflect the water-vapo(u)r saturation moment.
Background technique
The regulation of air humidity in industrial aspect such as air compressor machine industry, petroleum industry, lithium battery industry and electric power
The frequency that the fields such as industry use is more.The measurement of dew-point temperature is considered as the highest humidity measuring method of current precision, state
The transmission of quantity value of humidity is realized by dew point on border.
There are three ways to dew point testing: Cold Mirrors method, metal oxide method and the resonance method.
Cold Mirrors method can obtain higher precision in very wide measurement range, but its characteristics of relying on optical measurement is easily
By the dust and impurities pollution in air, to reduce the accuracy of measurement.Instrument internal optical system complexity leads to its cost
Also more expensive, most costs are in the cleaning and protection of sensor.
Metal oxide sensor can realize low dew point testing in industrial circle application.But metal oxide stability
Difference can generate measurement drift under the application scenarios of environment complexity.Measurement result need to be returned to genuine and be demarcated once drifting about, maintenance
Cost is sufficiently expensive.Once impaired, dew point sensor function will be unable to restore its sensing element.
The resonance method is mainly that the quality frequency characteristic combination active temperature control of resonating device is utilized to manufacture moisture condensation, passes through frequency
It deviates to identify that dew point, common resonating device have quartz crystal microbalance, this method has very strong sensitivity and measurement essence
Degree.But during refrigeration cool-down, since quartz crystal itself has warm frequency characteristic, temperature can generate one to frequency
Fixed influence, if not doing temperature-compensating if can bring very big measurement error.
Summary of the invention
1, purpose: the object of the present invention is to provide a kind of novel high-precision hydrophilic quartz resonance dew point recognition methods,
Centre includes the preparation method of Sensor core sensing element, subsequent dew point identification extraction algorithm and its application.This method can
To exclude influence of the warm frequency characteristic to dew point measurement precision.
2, technical solution:
On the one hand the application discloses the dew point transducer system that New Two Dimensional material is loaded in a kind of quartz crystal microbalance
Preparation Method, including by the preparation of two-dimensional material solution, two-dimensional material dispersion liquid jet atomization forms the aeroge of Nano grade,
Quartz crystal microbalance electrode surface forms a Nano grade thickness orderly two are stacked under electric field and pressure-air
Material film is tieed up, so that the dew point transducer core dew cell with two-dimensional material nano thin-film is obtained, finally by core
Frequency signal acquired in heart unit test carries out special data processing, can accurately extract use by special algorithm
To identify the characteristic quantity of dew point.
A kind of hydrophilic quartz resonance dew point recognition methods of the present invention, the process of this method is as shown in Figure 1, specific steps
It is as follows:
Step 1: the dew point transducer core dew cell of two-dimensional material nano thin-film is had according to the process preparation of Fig. 2.
Wherein, two-dimensional material can be used molybdenum disulfide either montmorillonite as main material.Molybdenum disulfide dispersion liquid can be by using fourth
The mode of base lithium chemical stripping commercialization molybdenum disulfide powder obtains dense suspension about 10g/ml, and then water-soluble using the ethyl alcohol of 3:1
It is spare that liquid is diluted to about 2mg/ml.Montmorillonite dispersions can be by being dispersed with stirring by overnight after blocky montmorillonite clay ball milling.Afterwards
It is spare that about 2mg/ml montmorillonite dispersions are diluted in the ethanol water of 3:1.It takes and prepares spare dispersion liquid by additional
High voltage and the form of air pressure, by its even application in quartz crystal microbalance electrode surface.Preferably, the electricity of high voltage electric field
Pressure is 0-20kV.Preferably, the intensity of air pressure is 20-100PSI.Preferably, molybdenum disulfide is 1T phase, for 1-5 layers or so receive
Rice lamellar structure.Preferably, nano coating of the invention with a thickness of 50~200nm.60 DEG C of vacuum drying are placed in after spraying
5 hours in case, make it dry.
Step 2: double chill surface dew point transducer devices with active temperature control function are assembled.See Fig. 3, including thermal conductive silicon
Film 10, semiconductor cooler 11, radiator 12, copper post 13, PT100 temperature sensor 14, gas chamber 15, electric silica gel gasket 17
And the dew point transducer core dew cell (QCM) 16 of two-dimensional material nano thin-film is had prepared by step 1.When measurement,
QCM dew cell is driven by impedance analyzer, is tested gas by gas chamber, under the cooling of semiconductor cooler, steam will
Dew cell surface is constantly attracted to until reaching saturation, generates hydrogenesis on the surface QCM.It is continuous in this course
The frequency values of dew cell surface temperature and QCM output are recorded, provide initial data for follow-up data processing.
Step 3: data processing is carried out to the frequency signal of sensor device output.That includes algorithm process gradually
Process: Fourier's fitting and second order derivation.Its method is that original frequency data are carried out Fourier's fitting, then to fitting
Curve afterwards carries out second order derivation transformation, and QCM surface temperature corresponding to the extreme value inflection point of curve is after second order derivation transformation
For dew-point temperature.The method is available accurate and unique characteristic quantity is used to identify dew point, without the concern for warm frequency characteristic
Influence.
It should be noted that two-dimensional material (such as montmorillonite) dispersion by super water-absorbent of the invention is injected in stone
The nano thin-film formed on English crystal microbalance electrode surface is the sensibility in order to improve sensor to hydrone.Montmorillonite is
It is very strong to the adsorption capacity of water compared with the material that molybdenum disulfide more absorbs water.Its unique two-dimensional structure will have vertically after absorbing water
The swelling in direction, interlamellar spacing between layers will become larger, and the density of material will become smaller.Its dilation and water suction
Maximum load power will affect the accuracy and stability of sensor.The sensor for having loaded two-dimensional material will be in the environment of low humidity
Under, more accurately judge dew point value.Load of the invention has the dew point transducer core dew cell of two-dimensional material more conventional
Sensor core dew cell have better water absorbing properties.And water suction saturation after material itself expansion, frequency
Rate variation by can obviously reflect the inflection point of physical change after data processing, identified for dew point and measurement provide it is more reliable
With accurate means.
Detailed description of the invention
Fig. 1 is the operating process of the method for the present invention.
Fig. 2 is the preparation process of the dew point transducer core dew cell with two-dimensional material nano thin-film of the invention.
Fig. 3 is dew point transducer schematic device of the invention.
Fig. 4 is the test result data of the method for the present invention.
Specific embodiment
Below by specific embodiment, invention is further described in detail.Following embodiment only to the present invention carry out into
One step explanation, should not be construed as limiting the invention.
Embodiment:
As shown in Fig. 2, this example includes the preparation facilities 1 of dew cell, the variation 2 of dew cell and two-dimentional material in test
The structure 3 of material.Wherein the surface variation of QCM includes following two steps: 1. by air and electrical spraying device 1 by two-dimensional material 3
Covering load 4 forms the dew cell 6 for having two-dimensional material film on dew cell bare die 5；2. test dew point, wet sensitive
Element surface is cooled in surface sweating 7, and the quality increase of the sensor surface for the generation that condenses will affect sensor oscillation frequency, leads to
The data processing form using Fourier transformation and second order derivation is crossed, judges the moment that condenses.
The dew cell painting equipment of this example is mainly made of electrical spraying device.The present apparatus includes atomization system, movement
Platform, high voltage power supply and control system；Atomization system includes syringe boost motor and spray head, and boost motor is mainly used for storing to be sprayed
Two-dimensional material (molybdenum disulfide 8, montmorillonite 9), and two-dimensional material is supplied to spray head, spray head is used to spray nano material,
Atomization.This example specifically uses the syringe of 10mL, and the speed released by programming Control syringe, and make spray head goes out liquid speed degree
0.1-50μL/min；This example specifically makes the 2.5 μ L/min of liquid speed degree out of spray head.
The two-dimensional material that this example uses is the molybdenum disulfide powder and montmorillonite ore of business procurement.Molybdenum disulfide powder
It is spare to 2mg/ml in ethanol water by being diluted in 3:1 after being removed in glove box with butyl lithium.Montmorillonite ore exists
After ball milling, 150W power ultrasound overnight into the water, after with 3:1 ethanol water to be diluted to 2mg/ml spare.
The anode of the high voltage power supply of this example is electrically connected with the nozzle of spray head, and the ground wire of high voltage power supply is connect with mobile platform；
Make to form a strong high voltage electric field between spray head and mobile platform.High voltage power supply is adjustable as DC power supply or alternating current
Source, output voltage 0-20kV.This example is specifically, do extra electric field using the stable voltage of DC power supply 5.6kV.
It, equally can be by nano particle in air using the mode that pressure-air is assisted in a kind of improvement project of this example
Middle atomization is covered on sensor surface in turn, forms fine and close nano coating.And so on move, same similar setting is herein not
Make specific limit.
In capital and interest in Back end data processing, the form of Fourier's fitting Combination second order derivation has been used.At this data
Purpose is managed in order to be the function containing " inflection point " form of more convenient identification by the unconspicuous frequency change transitions of variation tendency
Figure.And so on, same similar data processing algorithm is not specifically limited herein.
Test example:
The load that this example is prepared for a 50nm thickness according to above method respectively have molybdenum disulfide dew cell and one
50nm thickness loads the dew cell for having montmorillonite, and it is tested together with the dew cell of unsupported nano material, and
It is compared with standard dew point hygrometer MICHELL S4000.The ambient dew point range of test is between 3 DEG C of DP-15 DEG C of DP.
Sensor measurement with montmorillonite as shown in figure 4, under three different dew points (3 DEG C of DP, 9 DEG C of DP and 15
DEG C DP) have the tendency that similar monotonic decreasing.Have by (Fig. 4 (g) (h) (i)) after data processing and more significantly " turns
Point ".This inflection point is corresponding with dew point (dotted line) that standard dew point hygrometer measures.It calculates by statistics, is measured using the method for the present invention
Dew point and standard dew point instrument error be less than ± 0.3 DEG C of DP, meet industrial circle to high-accuracy dew point meter it is exhausted mostly
The number market demand.
The above content is specific embodiment is combined, further detailed description of the invention, and it cannot be said that this hair
Bright specific implementation is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, it is not taking off
Under the premise of from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to protection of the invention
Range.
Claims (1)
1. a kind of hydrophilic quartz resonance dew point recognition methods, it is characterised in that: specific step is as follows for this method:
Step 1: using molybdenum disulfide either montmorillonite as two-dimensional material, and molybdenum disulfide dispersion liquid is by with butyl lithiumation
The mode for learning the commercial molybdenum disulfide powder of removing obtains dense suspension about 10g/ml, and then is diluted using the ethanol water of 3:1
It is spare to about 2mg/ml；Montmorillonite dispersions by being dispersed with stirring overnight after blocky montmorillonite clay ball milling, after in the second of 3:1
It is spare that about 2mg/ml montmorillonite dispersions are diluted in alcohol solution；Take prepare spare dispersion liquid by applying high voltage and
The form of air pressure, by its even application in quartz crystal microbalance electrode surface；The voltage of high voltage electric field is 0-20kV, air pressure
Intensity is 20-100PSI, and molybdenum disulfide is 1T phase, is 1-5 layers or so of nano-lamellar structure, nano coating with a thickness of 50~
200nm；It is placed in 60 DEG C of vacuum ovens 5 hours, makes it dry after spraying；
Step 2: double chill surface dew point transducer devices with active temperature control function are assembled；Including heat-conducting silica gel sheet, semiconductor
Two are had prepared by refrigerator, radiator, copper post, PT100 temperature sensor, gas chamber, electric silica gel gasket and step 1
Tie up the dew point transducer core dew cell QCM of material nano film；When measurement, dew cell is driven by impedance analyzer,
Tested gas is by gas chamber, and under the cooling of semiconductor cooler, steam constantly will be attracted to dew cell surface until reaching
To saturation, hydrogenesis is generated on dew cell surface, continuously to record dew cell surface temperature and defeated in this course
Frequency values out；
Step 3: Fourier's fitting is first carried out to the frequency signal of sensor device output, second order then is carried out to matched curve
Derivation, dew cell surface temperature corresponding to the extreme value inflection point moment of curve is dew-point temperature after second order derivation transformation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024762A (en) * | 2019-12-05 | 2020-04-17 | 北京航空航天大学 | High-temperature flue gas dew point identification method |
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| CN106770460A (en) * | 2016-12-20 | 2017-05-31 | 北京航空航天大学 | A kind of dew point sensor device based on double refrigeration sensitive faces |
| CN106885826A (en) * | 2017-03-31 | 2017-06-23 | 北京航空航天大学 | A kind of Automatic Checkout ＆ Control System for quartz resonance dew point transducer |
| CN108982277A (en) * | 2018-06-20 | 2018-12-11 | 华中科技大学 | A kind of preparation method and product of quartz crystal microbalance humidity sensor |
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2019
- 2019-02-27 CN CN201910145129.4A patent/CN109884119A/en active Pending
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| CN102520019A (en) * | 2011-12-12 | 2012-06-27 | 北京航空航天大学 | Resonant dew point measurement method |
| CN105203423A (en) * | 2015-10-29 | 2015-12-30 | 青岛大学 | QCM (quartz crystal microbalance) humidity sensor adopting cerium doped zinc oxide nano-fiber and preparation method of QCM humidity sensor |
| CN106770460A (en) * | 2016-12-20 | 2017-05-31 | 北京航空航天大学 | A kind of dew point sensor device based on double refrigeration sensitive faces |
| CN106885826A (en) * | 2017-03-31 | 2017-06-23 | 北京航空航天大学 | A kind of Automatic Checkout ＆ Control System for quartz resonance dew point transducer |
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| CN111024762A (en) * | 2019-12-05 | 2020-04-17 | 北京航空航天大学 | High-temperature flue gas dew point identification method |
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Application publication date: 20190614 |