CN100402995C - Tubular liquid and soft matter shear wave resonant absorption instrument - Google Patents
Tubular liquid and soft matter shear wave resonant absorption instrument Download PDFInfo
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- CN100402995C CN100402995C CNB011298537A CN01129853A CN100402995C CN 100402995 C CN100402995 C CN 100402995C CN B011298537 A CNB011298537 A CN B011298537A CN 01129853 A CN01129853 A CN 01129853A CN 100402995 C CN100402995 C CN 100402995C
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Abstract
The present invention relates to a measuring instrument, particularly to a shear wave resonance absorption spectrometer for measuring liquid and soft matter. The spectrometer is composed of a torsional suspension device and a computer detection device, wherein the torsional suspension device is composed of a vibration element, a fixed gripping head, a torsional vibration gripping head, an oscillating rod, a permanent magnet, an electromagnetic drive coil, a rotary pipe and a bracket; the computer detection device is composed of a collimation light source, a reflecting mirror, a differential photocell, an A/D converter, a Fourier transformer, computer interfaces, a constant stress or constant strain feedback generator, a stress signal generator, a D/A converter, a power amplifier and an electromagnetic drive coil. The shear wave resonance absorption spectrometer of the present invention can measure the shear wave resonance absorption spectrums of the liquid and the soft matter in a temperature range of-20 to 150 DEG C, a frequency range of 10<-5> to 10<3> Hz, a wave number range of 10<-4> to 10<3>.
Description
Technical field
The present invention relates to a kind of surveying instrument, particularly a kind of shear wave resonant absorption instrument of measuring liquid and soft material.
Background technology
In the condensed state matter category, between the cluster in soft material and the solution, between long key and the interaction range between multikey, the collective behavior of molecule and cluster, long-chain in the Polymer Solution, group in the life liquid (as the aqueous solution of protein, nucleic acid, sugar, fat etc.) two, three, level Four or other chemical solutions and the complex compound, its yardstick that relates to are in from being slightly less than extremely some microns magnitude of 1nm.And the resonance absorption of common electromagnetic wave (light wave and microwave) or scattering (visible spectrum, Raman, infrared, NMR, ESR etc.) frequency are all 10
6~10
13Between the Hz or more than, what they can detect is the transition of various vibrations between electron level and key (comprising rotation) energy level, but for the whole energy state and the architectural feature of nanometer and the above yardstick material of nanometer, their but are difficult to measure.
Summary of the invention
The object of the present invention is to provide a kind of can be 10
-5~10
3The Hz frequency range is measured shear wave resonant absorption instrument in liquid and the soft material, be used for measurement Research liquid and soft material shear wave resonance absorption wavenumber spectrum, shear wave resonance absorption frequency spectrum, resonance energy absorption temperature spectrum, the dynamic modulus (mould of complex modulus and real part) of measuring condensed state matter is with wave number, frequency and variation of temperature relation, the viscosity of measuring liquid is with wave number, frequency and variation of temperature relation, and liquid and the kinetic parameter of soft material in added electric field, magnetic field, stress field or alternating temperature process.
Shear wave resonant absorption instrument of the present invention is formed (Fig. 1-2) by hanging torsional pendulum device and COMPUTER DETECTION device.Hang torsional pendulum device by the starting of oscillation element, last fixed chuck, following fixed chuck, the twisting vibration chuck, fork, permanent magnet, the Electromagnetic Drive coil, tube, support is formed, wherein starting of oscillation element one end is fixed on the last fixed chuck clamping on the support, the other end is fixed on the twisting vibration chuck clamping of fork end, tube one end is fixed on down fixed chuck, the other end is the twisting vibration chuck clamping of fork lower end, one permanent magnet is installed to the fork symmetria bilateralis, there is an Electromagnetic Drive coil each end outside of corresponding permanent magnet, can contain in the tube into fluid to be measured or soft material.The COMPUTER DETECTION device is by collimated light source, catoptron, differential photocell, A/D converter, Fourier transformer, computer interface, constant stress or constant strain ultramagnifier, the stress signal generator, D/A converter, power amplifier, the Electromagnetic Drive coil is formed, wherein catoptron is installed on the fork, catoptron and collimated light source, differential photocell constitutes the strain signal source of COMPUTER DETECTION device, differential photocell one tunnel connects A/D converter successively, Fourier transformer, computer interface, another road connect the constant ultramagnifier of strain amplitude successively, the stress signal generator, D/A converter, power amplifier, the Electromagnetic Drive circle, the Fourier interchanger, computer interface (Fig. 3).
In hanging torsional pendulum device, a permanent magnet passes fork and makes and exposes symmetria bilateralis, and also available pair of permanent magnets substitutes a magnet that passes across fork, and starting of oscillation element and tube branch are in fork two ends up and down, also can be in fork upper end or lower end together; Starting of oscillation element and tube two ends are separately fixed at rotates on chuck and the fixed chuck, and the starting of oscillation element is solid filament or solid piece.Hang torsional pendulum device and can adopt the mode of just rocking (Fig. 1), hang torsional pendulum device and can also adopt the mode of rocking (Fig. 2).When mode is rocked in employing, the fixed chuck liftable, the starting of oscillation element is substituted by tube, tube is the starting of oscillation element simultaneously, the fork other end is connected to fixed pulley and counterweight counterweight by fine rule, and fixed pulley is fixed on the support, and the counterweight counterweight is connected on the fork by fixed pulley and fine rule.
Just hanging and hanging by the feet and hang in the torsional pendulum device, can in tube, contain and go into liquid or soft material, the twisting vibration of tube can be in pipe in liquid or the soft material generation wave front be the shear wave of surface level.Can also just hang torsional pendulum device below or above adorn a liquid-holding pipe, its upper end be fixed on one heart on the torsion bar, the lower end be fixed in one heart the below fixed chuck; When torsion bar was done twisting vibration, the liquid in the pipe produced the shear wave that wave front is a surface level thereupon.The tube of also available Sheng liquid substitutes (both be used for containing liquid, again as starting of oscillation) starting of oscillation element and measures (Fig. 2).Utilize the restoring force of tube itself to come starting of oscillation this moment.What record when not containing liquid or soft material is the resonance absorption of tube, and what record when containing liquid or soft material is total resonance absorption of tube and liquid (or soft material).Because the resonance absorption of tube its background except that absorbing spike itself is very low, so the resonance absorbing peak of liquid (or soft material) is easy to discern (see figure 4).
Shear wave resonant absorption instrument of the present invention be to utilize the forced vibration method to produce main shear wave in condensed state matter, and shear wave velocity can make 10 much smaller than the principle of the light velocity in applying solid and the liquid
-5~10
3The twisting vibration of the continuous frequency conversion of HZ frequency range produces wave number in liquid be 10
-3~10
3(solid is 10 to cm
-8~10cm
-1) shear wave, by measuring its resonance absorbing peak, can record and be in liquid and the solid material from being slightly less than the feature of 1nm to the source of resonant excitation of some microns magnitude range scale, comprise energy level, size and the quality that can record the source of resonant excitation, reciprocation energy and bonding force, in cluster and the life liquid or the phase transformation in the biological membrane, myriameter waves transverse phonon mould is softening in the solid, and alternating temperature and add (life, chemistry or physics) process kinetics feature under (electricity, magnetic, power) field condition.Lower Half, MNR spectrum, ESR that the continuous variation range of its wave number can cover the Raman spectrum compose up to microwave, thereby can be in Condensed Matter Physics. be widely used in the research of solution research, colloidal chemistry, organic chemistry, biological chemistry and life process.
In shear wave resonant absorption instrument of the present invention, when measured object is liquid, contain measured liquid or soft material in the tube.When applying an alternate electrical signal by the Electromagnetic Drive coil, permanent magnet is subjected to alterante stress, thereby forms shear wave by the twisting vibration of liquid-holding pipe in liquid or soft material.By computing machine by software (or hardware) but the sinusoidal wave electric signal of the continuous frequency conversion that produces after D/A conversion and power amplification, import drive coil 6 and drive in the liquid of tube and form shear wave.After the strain signal that is received by photoelectric cell amplified, a part fed back to the constant of the amplitude of answering forcer to make to keep strain or stress.Stress signal in another part and the coil 6 is imported computing machine simultaneously, can draw the Ф that differs that strain lags behind stress after Fourier's exchange.Whole process is carried out automatically and can show in real time tg Ф-k on screen by process of measurement by computing machine, modulus M-k curve (k is a wave number), also can be in real time or measurement finish after printing curve and data.
The mode that the present invention produces shear wave is to utilize the twisting vibration of tube to be created in the shear wave that vertical direction is propagated.In spectrometer of the present invention, only otherwise put into liquid, all can directly measure the resonance absorption feature of solid sample (being starting of oscillation element or tube itself).The equation of motion of its shear wave is:
M wherein
0Exp (i ω t) is an applied moment, and I is the moment of inertia of device, and θ is a torsion angle, the viscous moment that γ produces when being the tube twisting, M
1Be the countermoment of starting of oscillation element, M
2Dissipation moment for the starting of oscillation element.Wherein can be regarded as
γ=Aη (2)
Wherein A is an instrument constant, and η is to being fluid to be measured viscosity.The energy that dissipates in one week of device vibration (energy of vibration that is absorbed by liquid and starting of oscillation element) can just be expressed with the phase angle φ that strain lags behind stress.The result who solves is:
Tg φ (ω)
Coefficient=tg φ (ω)
Torsion wire+ tg φ (ω)
Liquid(3)
When the forced vibration frequency ω of device can compare with system resonance frequencies omega r, must carry out following correction to the apparatus measures value:
When measuring the resonance absorption of liquid, the background dissipation that should drain the fluid to be measured in liquid-holding pipe or the dish earlier and measure the starting of oscillation element
Value tg φ
L, in containing liquid device 9, contain fluid to be measured again or soft material is measured tg φ
L, its difference
tgφ=tgφ
L-tgφ
S (5)
Be the resonance absorption value of liquid.But tg φ in the ordinary course of things,
LMuch larger than tg φ
SSo the latter often can ignore, with surveyed tg φ
LAs tg φ
MeasureCan draw the variation relation of the energy of vibration dissipation tg φ of liquid by (4) formula again with frequency.
In addition, the pass of the wavelength X of shear wave and vibration frequency ω etc. is in the liquid:
λ=1/k=(2η/ρω)
1/2 (6)
Wherein η is the coefficient of viscosity of fluid to be measured, and ρ is the density of fluid to be measured, and k is the wave number of fluid to be measured.Can learn the variation relation of the resonance absorption value tg φ of liquid by (4) to (6) formula with the viscosities il of wave number k and liquid.
For cylindric soft material and gel, its shear wave wave number is:
k=f/(G/ρ)
12 (7)
G is tested soft material shear modulus herein, and ρ is the density of tested soft material, and f is a survey frequency.Because the shear modulus of soft material and gel approximately has only 10 of common solid
8/ one, so the shear wave wave number in soft material and the gel is only than the low about magnitude of liquid.Can measure the variation of the dissipation tg φ of liquid (or soft material) with frequency or wave number; Also but stationary installation is in a certain forced vibration frequency ω, change the temperature of liquid, the dissipation tg φ that can learn liquid (or soft material) concerns with variation of temperature, with the dissipation tg φ of phase transformation, relaxation and liquid-liquid in further research liquid or the soft material (or soft material) with the kinetic parameter in added electric field, magnetic field, stress field or alternating temperature process.
When the shear wave frequency is 10
-4~10
3During Hz, the wave number of water is 0.1~560cm
-1(being equivalent to electromagnetic millimeter to infrared band), k has changed more than 5000 times.Therefore (low-frequency limit of double grating Raman spectrum is 30cm to the continuous wave-number range that shear wave resonant spectrum covered in the liquid than Raman
-1) and the INFRARED SPECTRUM sum also wide.
When temperature raise, the viscosities il of liquid and the shear modulus G of soft material reduced; Therefore, can make wave number 10 by the viscosity of frequency and liquid and the shear modulus G of soft material with variation of temperature
-3~10
3Cm
-1Between change continuously, this has covered from Raman spectrum Lower Half, INFRARED SPECTRUM, NMR spectrum, ESR and has composed hyperacoustic even wave-number range, so this spectrometer may detect and is of a size of the nm~μ m or the bigger source of resonant excitation in the liquid.
Shear wave resonant absorption instrument of the present invention can be at-20~150 ℃, 10
-5~10
3Hz, 10
-3~10
3Cm
-1In the frequency range, measure the shear wave resonant spectrum of liquid and soft material in the wave-number range.Its phase angle difference resolution is better than 5*10
-5Radian.Shear wave resonant absorption instrument of the present invention can (can be at the resonant frequency ω of system in forced vibration
rBelow or more than carry out), work under the stress relaxation under the free damping, constant strain condition or the modes such as strain rheology under the constant stress condition.Because the present invention adopts cast, what produced is the shear wave that wave front is vertically propagated, can make liquid-holding pipe with the medical transfusion pipe, and fluid volume can be lacked to about 1ml or liquid measure still less, and the two ends of pipe can be in closed state, liquid is not volatile, thereby is convenient to the measurement as life liquid, biological reagent, medicament and relevant soft material.
The present invention is further detailed explanation below in conjunction with accompanying drawing
Fig. 1 is for hanging torsional pendulum device for just rocking the cast shear wave resonant absorption instrument structural representation of mode.
Fig. 2 is for hanging torsional pendulum device for rocking the cast shear wave resonant absorption instrument structural representation of mode.
Fig. 3 is that the COMPUTER DETECTION device of shear wave resonant absorption instrument connects block diagram.
Fig. 4 is for being that liquid line shear wave resonant absorption instrument when just rocking mode records water wave number spectrogram at room temperature with hanging torsional pendulum device.
Among Fig. 1, hang torsional pendulum device and adopt the mode of just rocking.Starting of oscillation element 1 one ends are fixed on last fixed chuck 2 clampings of support 14, the other end is fixed on twisting vibration chuck 4 clampings of fork 3 one ends, 3 liang of middle side parts of fork are equipped with pair of permanent magnets 7 symmetrically, corresponding to permanent magnet 7 two ends, there is an Electromagnetic Drive coil 6 outside, tube 8 one ends are fixed on down fixed chuck 15, and the other end is twisting vibration chuck 13 clampings of fork 3 lower ends.Catoptron 11 is installed on the fork 3, it and collimated light source 10, and the differential photocell 12 that receives vibration signal constitutes the strain signal source of COMPUTER DETECTION devices.Tube can be made with plastics, metal, pottery, glass, rubber, bamboo trunk or timber, requires material therefor not react with fluid to be measured, is enough to drive the liquid motion with the wellability of fluid to be measured.
In Fig. 2, tube 8 (hold concurrently and be starting of oscillation element a 1) end is fixed on down fixed chuck 15, the other end is twisting vibration chuck 13 clampings of fork 3 lower ends, and fork 3 another ends are connected with counterweight counterweight 5 with line by two fixed pulleys 9 that are fixed on the support, and other are identical with Fig. 1.Utilize the restoring force of tube itself to come starting of oscillation this moment.What record when not containing liquid or soft material is the resonance absorption of tube, and what record when containing liquid or soft material is total resonance absorption of tube and liquid (or soft material).Because the resonance absorption of tube its background except that absorbing spike itself is very low, so the resonance absorbing peak of liquid is easy to discern (see figure 4).
Consider the balance of upper and lower torsion, be the drag of solid starting of oscillation element and the balance of liquid viscosity resistance, the magnet that applies twisting resistance is placed the middle part of putting stalk, and starting of oscillation element and tube are in two ends up and down respectively, so vibrational system is easy to balance and has the better resisting interference ability.
Among Fig. 3, differential photocell 12 one tunnel connects A/D converter 23, Fourier transformer 16, computer interface 17 successively, and another road connects the constant ultramagnifier 18 of strain amplitude, stress signal generator 19, D/A converter 20. power amplifiers 21, Electromagnetic Drive circle 22, Fourier transformer 16, computer interface 17 successively.
When applying an alternate electrical signal by coil 6 during measurement, permanent magnet 7 is subjected to alterante stress, sets up one in the starting of oscillation element 1 with the twisting vibration of alternate electrical signal same frequency ω and form shear wave in containing liquid film thereby make.By computing machine by software (or hardware) but the sinusoidal wave electric signal of the continuous frequency conversion that produces is imported drive coil 22 after D/A conversion and power amplification.After the strain signal amplification by photoelectric cell 12 receptions, a part feeds back to answers forcer 19 to make the constant of maintenance strain or stress amplitude.Stress signal in another part and the coil reason is imported computing machine simultaneously, can draw the φ that differs that strain lags behind stress after the Bo Liye exchange.Whole process is carried out automatically and can show in real time tg φ-k on screen by process of measurement by computing machine, M-k curve (k is a wave number), also can be in real time or measurement finish after printing curve and data.
Fig. 4 has provided with hanging the liquid line shear wave resonant absorption instrument of torsional pendulum device when just rocking mode and has recorded the wave number spectrogram of water in room temperature.Wherein top curve (black circle) is tube and total resonance absorption curve of containing the water of going into; Lower curve (hollow square frame) be in the tube complete when anhydrous the resonance absorption background and the resonance absorbing peak of pipe matter (medical infusion lines) itself, but the wide diffusing resonance absorbing peak of water breakthrough is easy to identification.
Claims (4)
1. shear wave resonant absorption instrument, form by hanging torsional pendulum device and COMPUTER DETECTION device, it is characterized in that hanging torsional pendulum device by the starting of oscillation element, last fixed chuck, following fixed chuck, the twisting vibration chuck, fork, permanent magnet, the Electromagnetic Drive coil, tube, support is formed, wherein starting of oscillation element one end is fixed on the last fixed chuck clamping on the support, the other end is fixed on the twisting vibration chuck clamping of fork end, tube one end is fixed on down fixed chuck, the other end is the twisting vibration chuck clamping of fork lower end, one permanent magnet is installed to the fork symmetria bilateralis, there is an Electromagnetic Drive coil each end outside of corresponding permanent magnet, can contain in the tube into fluid to be measured or soft material.
2. a shear wave resonant absorption instrument as claimed in claim 1 is characterized in that starting of oscillation element and tube branch are in fork two ends up and down, also can be in fork upper end or lower end together.
3. a shear wave resonant absorption instrument as claimed in claim 1 or 2 is characterized in that the starting of oscillation element is solid filament or solid piece.
4. a shear wave resonant absorption instrument as claimed in claim 1 or 2 is characterized in that the starting of oscillation element can be substituted by tube.
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CN100402995C true CN100402995C (en) | 2008-07-16 |
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CN1314589A (en) * | 2000-03-17 | 2001-09-26 | 中山大学 | Shear wave resonant absorption spectrum instrument of liquid film |
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CN1314589A (en) * | 2000-03-17 | 2001-09-26 | 中山大学 | Shear wave resonant absorption spectrum instrument of liquid film |
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