CN104880390A - Method for measuring performance parameters of micro-nano particles - Google Patents

Method for measuring performance parameters of micro-nano particles Download PDF

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CN104880390A
CN104880390A CN201510263349.9A CN201510263349A CN104880390A CN 104880390 A CN104880390 A CN 104880390A CN 201510263349 A CN201510263349 A CN 201510263349A CN 104880390 A CN104880390 A CN 104880390A
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CN104880390B (en
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李皓
白鹏飞
林烈鑫
井一涵
周国富
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South China Normal University
Shenzhen Guohua Optoelectronics Co Ltd
Academy of Shenzhen Guohua Optoelectronics
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Shenzhen Guohua Optoelectronics Co Ltd
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Abstract

The invention discloses a method for measuring performance parameters of micro-nano particles. The method comprises the following steps: constructing a system for measuring performance parameters of micro-nano particles, wherein the system comprises a detection ware, a constant temperature control regulator, an ultrasonic module, a soundproofing module, a signal analysis and process module; the specific value of the backscatter intensity of free micro-nano particles in solid-liquid continuous phase medium for ultrasonic waves to the incident intensity of the free micro-nano particles in solid-liquid continuous phase medium for ultrasonic waves, and other parameters like the sound pressure, the particle concentration, the particle size, the medium viscosity and the medium density are utilized for calculating to obtain the characteristic mechanical parameters. According to the method for measuring performance parameters of micro-nano particles, the elastic coefficient and the surface tension of micro-nano particles can be precisely measured under the same measuring system and the same measuring environment, so that accurate experimental data is provided for study on the relation between the elastic coefficient and the surface tension, the properties of materials can be more deeply mastered, the service life of the materials is prolonged, and the quality of the materials is improved.

Description

一种微纳米粒子性能参数的测量方法A method for measuring performance parameters of micro-nano particles

技术领域technical field

本发明涉及微纳米粒子的特征力学性能参数的测量,具体涉及一种微纳米粒子性能参数的测量方法。The invention relates to the measurement of characteristic mechanical performance parameters of micro-nano particles, in particular to a method for measuring the performance parameters of micro-nano particles.

背景技术Background technique

微纳米粒子的特征力学性能参数,特别是表面张力和弹性系数,与粒子的稳定性密切相关。通过研究和检测微纳米粒子的特征力学性能参数,能够更好地研究在什么条件下,微纳米粒子最稳定,使用寿命最长,还可以得到粒子在外界的作用下,最大的稳定临界点等重要信息,从而可以通过控制外界条件,使得粒子能够稳定的,长时间的使用。纳米材料是指材料粒子尺寸在纳米数量级(通常指1-100nm)的极细粒子组成的固体材料,通常划分为两个层次:纳米微粒和纳米固体。纳米材料自从被人们所认识,就与应用紧密联系在一起。纳米粒子的特殊效应导致了纳米材料的特殊性质,而这些特殊性质带来了纳米材料的广泛应用。目前,纳米材料已经在催化、环保、能源行业及新型工程、磁性和防护材料的制备等方面等到了一定的应用。纳米科技与电子学、医学、生物学、计算机科学和军事科学等的交叉渗透,产生了诸如纳米电子学,纳米医学等传统学科前冠以纳米前缀的新学科,为纳米材料展现更为广阔的应用前景,因此,通过研究微纳米粒子,对于微纳米材料的发展有着巨大的作用,同时也是符合国家的重点发展对象。The characteristic mechanical performance parameters of micro-nano particles, especially the surface tension and elastic coefficient, are closely related to the stability of the particles. By studying and testing the characteristic mechanical performance parameters of micro-nano particles, we can better study under what conditions micro-nano particles are the most stable and have the longest service life, and we can also obtain the maximum stable critical point of particles under the action of the outside world, etc. Important information, so that the particles can be used stably and for a long time by controlling the external conditions. Nanomaterials refer to solid materials composed of extremely fine particles with particle sizes on the order of nanometers (usually 1-100nm), and are usually divided into two levels: nanoparticles and nanosolids. Nanomaterials have been closely related to applications since they were recognized by people. The special effects of nanoparticles lead to the special properties of nanomaterials, and these special properties bring about the wide application of nanomaterials. At present, nanomaterials have been applied in catalysis, environmental protection, energy industry and new engineering, preparation of magnetic and protective materials, etc. The cross-infiltration of nanotechnology and electronics, medicine, biology, computer science and military science has produced new disciplines such as nanoelectronics, nanomedicine and other traditional disciplines prefixed with nano, showing a broader scope for nanomaterials. Application prospects, therefore, through the study of micro-nano particles, it has a huge effect on the development of micro-nano materials, and it is also in line with the country's key development targets.

现有粒子表面张力和弹性系数的常见测量方法:Common measurement methods for existing particle surface tension and elastic coefficient:

1、粒子表面张力检测方法:1. Particle surface tension detection method:

(1)接触角测量法,在洁净的毛细管中液体平衡时所满足的条件是ρghπγ2=2πrγLA cosθ,式中ρ是液体密度,h是液体在毛细管中上升高度,r是毛细管半径,γLA是待测液体表面张力系数,θ是液体和毛细管壁的接触角。可利用前面提供的实验仪器,通过对接触角、毛细管管径和液体在毛细管中上升高度的测量,来测定特定温度下液体的特征力学性能参数。(1) The contact angle measurement method, the condition satisfied when the liquid is balanced in a clean capillary is ρghπγ 2 = 2πrγ LA cosθ, where ρ is the density of the liquid, h is the rising height of the liquid in the capillary, r is the radius of the capillary, γ LA is the surface tension coefficient of the liquid to be measured, and θ is the contact angle between the liquid and the capillary wall. The characteristic mechanical property parameters of the liquid at a specific temperature can be determined by measuring the contact angle, capillary diameter, and rising height of the liquid in the capillary by using the experimental instruments provided above.

缺点:该检测方法是应用在固体-液交界面上的检测,而且是大分子的检测,对于微纳米级别的检测以及其他接触面的检测,无法进行。Disadvantages: This detection method is applied to the detection of solid-liquid interface, and it is the detection of macromolecules. It cannot be used for the detection of micro-nano level and other contact surfaces.

(2)滴重法(滴体积法),自-毛细管滴头滴下液体时,液滴的大小与液体的表面张力有关,即表面张力越大,滴下的液滴也越大,二者存在关系式:(2) Drop weight method (drop volume method), when the liquid is dripped from the capillary dripper, the size of the droplet is related to the surface tension of the liquid, that is, the greater the surface tension, the larger the dropped droplet, there is a relationship between the two Mode:

W=2πRγf     (1)W=2πRγf (1)

γ=W/(2πRf)   (2)γ=W/(2πRf) (2)

式中,W为液滴的重量;R为毛细管的滴头半径,其值的大小由测量仪器决定;f为校正系数。一般实验室中测定液滴体积更为方便,因此式(2)又可写为:In the formula, W is the weight of the liquid drop; R is the radius of the dripper of the capillary, and its value is determined by the measuring instrument; f is the correction factor. It is more convenient to measure the droplet volume in the general laboratory, so formula (2) can be written as:

γ=(Vρg/R)*(1/2πf)     (3)γ=(Vρg/R)*(1/2πf) (3)

式中,V为液滴体积;ρ为液体的密度;f为校正因子。对于特定的测量仪器和被测液体,R和ρ是固定的,在测量过程中,只要测出数滴液体的体积,就可计算出该液体的表面张力。In the formula, V is the volume of the droplet; ρ is the density of the liquid; f is the correction factor. For a specific measuring instrument and liquid to be measured, R and ρ are fixed. During the measurement process, as long as the volume of a few drops of liquid is measured, the surface tension of the liquid can be calculated.

缺点:a.至今只能算是一种经验方法;b.不能用来测定达到平衡较慢的表面张力,同时该法也不能达到完全的平衡;c.存在准确测定液体体积和很好地控制液滴滴落速度等问题;d.只适用于液体的情况下,同时对于液滴的粒径,无法满足微纳米级别的。Disadvantages: a. It can only be regarded as an empirical method so far; b. It cannot be used to measure the surface tension that reaches equilibrium slowly, and at the same time, this method cannot achieve complete equilibrium; c. There are accurate determination of liquid volume and good control of liquid Droplet speed and other issues; d. It is only applicable to liquid, and at the same time, the particle size of the droplet cannot meet the micro-nano level.

(3)毛细管上升法,将一支毛细管插入液体中,液体将沿毛细管上升,升到一定高度后,毛细管内外液体将达到平衡状态,液体就不再上升了。此时,液面对液体所施加的向上的拉力与液体总的向下的力相等,则γ=1/2ρ1gghr cosθ式中γ为表面张力;r为毛细管的半径;h为毛细管中液面上升的高度;ρ1为测量液体的密度;ρg为气体的密度(空气和蒸汽);g为当地的重力加速度;θ为液体与管壁的接触角。若毛细管管径很小,而且θ=0时,则上式可简化为γ=1/2ρghr。(3) Capillary ascending method, a capillary is inserted into the liquid, and the liquid will rise along the capillary. After rising to a certain height, the liquid inside and outside the capillary will reach an equilibrium state, and the liquid will no longer rise. At this time, the upward pulling force exerted by the liquid on the liquid is equal to the total downward force of the liquid, then γ=1/2ρ 1g ghr cosθ where γ is the surface tension; r is the radius of the capillary; h is The rising height of the liquid level in the capillary; ρ1 is the density of the measured liquid; ρg is the density of the gas (air and steam); g is the local acceleration of gravity; θ is the contact angle between the liquid and the tube wall. If the diameter of the capillary is very small and θ=0, the above formula can be simplified to γ=1/2ρghr.

缺点:a.不易选得内径均匀的毛细管和准确测定内径值;b.液体与管壁的接触角不易测量;c.溶液的纯度会对表面张力的测量造成不同程度的影响。d.需要较多液体才能获得水平基准面(一般认为直径在10cm以上液面才能看作平面),所以基准液面的确定可能产生误差;e.只适用于液体的检测,无法用于气体等的检测,而且达不到微纳米的级别。Disadvantages: a. It is not easy to select a capillary with uniform inner diameter and accurately measure the inner diameter; b. It is not easy to measure the contact angle between the liquid and the tube wall; c. The purity of the solution will affect the measurement of surface tension to varying degrees. d. More liquid is needed to obtain a horizontal reference surface (it is generally considered that a liquid surface with a diameter of more than 10cm can be regarded as a plane), so the determination of the reference liquid level may cause errors; e. It is only suitable for the detection of liquids and cannot be used for gases, etc. detection, and can not reach the micro-nano level.

目前,还有许多现代仪器方法,如最大气泡压力法差分最大气泡压力法、Wilhelmy盘法、滴外形法等。但是,上述的所有方法,均是对液体的表面张力的检测,无法实现微纳米级材料粒子表面张力的检测。而且,这种检测方法,只是局限在液气的条件下,无法测试其他环境下的特征力学性能参数。At present, there are many modern instrument methods, such as the maximum bubble pressure method, the differential maximum bubble pressure method, the Wilhelmy disk method, and the drop shape method. However, all the above-mentioned methods are for detecting the surface tension of the liquid, and cannot realize the detection of the surface tension of the micro-nano-scale material particles. Moreover, this detection method is only limited to liquid and gas conditions, and cannot test characteristic mechanical performance parameters in other environments.

2、粒子弹性系数检测方法:2. Particle elastic coefficient detection method:

原子力显微镜测试材料粒子的弹性系数,原子力显微镜称为AFM,即Atomic Force Microscope,在AFM的系统中,所要检测的力是原子与原子之间的范德华力,所以在本系统中是使用微小悬臂来检测原子之间力的变化量。微悬臂通常由一个一般100-500um长和大约500nm-5um厚的硅片或氮化硅片制成。微悬臂顶端有一个尖锐针尖,用来检测样品-针尖间的相互作用力,利用AFM获得的力谱曲线在生物医学中的应用:在探测一个细胞之后,根据所遇到的阻力,AFM就会赋予一个表明力度的数值,即为粒子的力谱,并通过粒子的变形情况,利用杨氏模量,就可以得到相应的弹性系数。The atomic force microscope tests the elastic coefficient of material particles. The atomic force microscope is called AFM, that is, Atomic Force Microscope. In the AFM system, the force to be detected is the van der Waals force between atoms, so in this system, a tiny cantilever is used. Detects the amount of change in force between atoms. Cantilevers are usually fabricated from a silicon or silicon nitride wafer typically 100-500um long and approximately 500nm-5um thick. There is a sharp needle tip at the top of the microcantilever, which is used to detect the interaction force between the sample and the needle tip. The application of the force spectrum curve obtained by AFM in biomedicine: after detecting a cell, according to the resistance encountered, AFM will Give a numerical value indicating strength, which is the force spectrum of the particle, and through the deformation of the particle, use Young's modulus to obtain the corresponding elastic coefficient.

缺点:AFM的缺点在于成像范围太小,速度慢,受探头的影响太大。该检测方法是在空气中检测,较为精确,但检测液体样品时,由于溶剂分子的存在,将会严重影响探头的检测,无法保证检测精度,同时也不能达到本项目的目的,更无法将两个检测量联系到一起。Disadvantages: The disadvantages of AFM are that the imaging range is too small, the speed is slow, and it is too much affected by the probe. This detection method is to detect in the air, which is relatively accurate, but when detecting liquid samples, due to the existence of solvent molecules, the detection of the probe will be seriously affected, and the detection accuracy cannot be guaranteed. At the same time, the purpose of this project cannot be achieved, let alone the two linked together.

目前,对于微纳米粒子,特别是液相体系中处于自由状态的微纳米粒子特征力学性能参数的检测方法,都无法提供可靠、准确、精密的检测结果,而且很多检测方法对于粒子的尺寸下限都无法达到微纳米级,受外部环境的限制比较严重,可应用范围小。At present, for the detection methods of micro-nano particles, especially the characteristic mechanical properties parameters of micro-nano particles in the free state in the liquid phase system, they cannot provide reliable, accurate and precise detection results, and many detection methods have no limit for the particle size lower limit. It cannot reach the micro-nano level, and is severely restricted by the external environment, and its applicable range is small.

发明内容Contents of the invention

为解决现有技术中存在的问题,本发明提供一种微纳米粒子性能参数的测量方法。In order to solve the problems existing in the prior art, the invention provides a method for measuring performance parameters of micro-nano particles.

本发明解决上述技术问题的技术方案如下:一种微纳米粒子性能参数的测量方法,包括如下步骤:The technical solution of the present invention to solve the above-mentioned technical problems is as follows: a method for measuring performance parameters of micro-nano particles, comprising the following steps:

步骤10:搭建一微纳米粒子性能参数的测量系统,该测量系统包括:Step 10: Build a measurement system for the performance parameters of micro-nano particles, which includes:

检测器皿,用于承载待检测的微纳米粒子;The detection vessel is used to carry the micro-nano particles to be detected;

恒温控制调节器:用于控制、调节检测器皿内的温度达到所需的温度值;Constant temperature control regulator: used to control and adjust the temperature in the detection vessel to reach the required temperature value;

超声模块,用于将超声波发射至微纳米粒子,接收由微纳米粒子反射和散射的超声波回波信号,并将超声波回波信号传输至信息分析处理模块;The ultrasonic module is used to transmit ultrasonic waves to the micro-nano particles, receive the ultrasonic echo signals reflected and scattered by the micro-nano particles, and transmit the ultrasonic echo signals to the information analysis and processing module;

消声模块,用于吸收检测器皿中多余的超声波信号;Noise elimination module for absorbing redundant ultrasonic signals in the detection vessel;

信号分析处理模块,用于对超声波回波信号进行处理得到微纳米粒子的背向散射强度,并基于特征公式求得微纳米粒子的表面张力和弹性系数;The signal analysis and processing module is used to process the ultrasonic echo signal to obtain the backscattering intensity of the micro-nano particles, and obtain the surface tension and elastic coefficient of the micro-nano particles based on the characteristic formula;

步骤20:制备微纳米粒子,并记录微纳米粒子个数、微纳米粒子的浓度;Step 20: Prepare micro-nano particles, and record the number of micro-nano particles and the concentration of micro-nano particles;

步骤30:向检测器皿内放置固液连续相介质,通过恒温控制器调节器皿内的温度达到所需温度,待温度稳定后,将所述微纳米粒子置于所述固液连续相介质中,并维持检测器皿内温度恒定;Step 30: Place the solid-liquid continuous phase medium in the detection vessel, adjust the temperature in the vessel to reach the required temperature through a thermostat controller, and place the micro-nano particles in the solid-liquid continuous phase medium after the temperature is stable, And maintain a constant temperature in the detection vessel;

步骤40:控制超声模块向微纳米粒子发送所需频率的超声波,记录施加的声压,实时观测并记录微纳米粒子的半径变化情况;Step 40: Control the ultrasonic module to send ultrasonic waves of the required frequency to the micro-nano particles, record the applied sound pressure, observe and record the change of the radius of the micro-nano particles in real time;

步骤50:超声模块接收由微纳米粒子反射和散射的超声波回波信号,并将超声波回波信号传输至信息分析处理模块;由信号分析处理模块对超声波回波信号进行处理得到微纳米粒子的背向散射强度;Step 50: The ultrasonic module receives the ultrasonic echo signals reflected and scattered by the micro-nano particles, and transmits the ultrasonic echo signals to the information analysis and processing module; the signal analysis and processing module processes the ultrasonic echo signals to obtain the background of the micro-nano particles to the scattering intensity;

步骤60:信号分析处理模块基于特征公式求得微纳米粒子的表面张力和弹性系数。Step 60: The signal analysis and processing module obtains the surface tension and elastic coefficient of the micro-nano particles based on the characteristic formula.

在上述技术方案的基础上,本发明还可以做如下改进。On the basis of the above technical solutions, the present invention can also be improved as follows.

进一步,所述步骤S60中基于特征公式求得微纳米粒子的表面张力和弹性系数,其具体为:Further, in the step S60, the surface tension and elastic coefficient of the micro-nano particles are obtained based on the characteristic formula, which is specifically:

弹性系数Ks由以下特征公式(1)和(2)计算出:The elastic coefficient K s is calculated by the following characteristic formulas (1) and (2):

II sthe s II == 11 99 ** NVΣSNVΣS -- -- -- (( 11 ))

ΣSΣS == 44 ππ 99 KK 44 RR 66 {{ (( KK SS -- KK KK )) 22 ++ 11 33 (( 33 (( ρρ SS -- ρρ LL )) 22 ρρ SS ++ ρρ LL )) 22 }} -- -- -- (( 22 ))

其中,Is为微纳米粒子背向散射强度,I为入射声波的强度,N为微纳米粒子的个数,V为微纳米粒子的体积,∑S为单个散射微纳米粒子的有效散射面积,ρS为微纳米粒子的密度,ρL为介质的密度,K为气体多变指数,R为随时间变化的微纳米粒子的半径;Wherein, I s is the backscattering intensity of micro-nanoparticles, I is the intensity of incident acoustic wave, N is the number of micro-nanoparticles, V is the volume of micro-nanoparticles, ΣS is the effective scattering area of a single scattering micro-nanoparticles, ρ S is the density of the micro-nano particles, ρ L is the density of the medium, K is the gas variability index, and R is the radius of the micro-nano particles changing with time;

表面张力σ由以下特征公式(3)、(4)、(5)给出:The surface tension σ is given by the following characteristic formulas (3), (4), (5):

RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( ∂∂ RR ∂∂ tt )) 22 == 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 22 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP 00 -- pp acac (( tt )) ]] -- -- -- (( 33 ))

(( 11 -- 22 ∂∂ RR ∂∂ tt cc )) RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( 11 -- 44 ∂∂ RR ∂∂ tt 33 cc )) (( ∂∂ RR ∂∂ tt )) 22 == (( 11 ++ RR cc dd dtdt )) 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 33 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP 00 -- PP acac (( tt )) ]] -- -- -- (( 44 ))

(( 11 -- ∂∂ RR ∂∂ tt cc )) RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( 11 -- 44 ∂∂ RR ∂∂ tt 33 cc )) (( ∂∂ RR ∂∂ tt )) 22 == (( 11 ++ ∂∂ RR ∂∂ tt cc ++ RR cc dd dtdt )) 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 33 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP 00 -- PP acac (( tt )) ]] -- -- -- (( 55 ))

其中,ρL为介质的密度,R为随时间变化的粒子的半径,R0为粒子的初始半径,PV为粒子的内部压力,ηL为介质的动力粘度,PO为流体静压力,Pac(t)为声压,c为介质中超声波的速度,PG0为粒子内部的压强。Among them, ρ L is the density of the medium, R is the radius of the particle changing with time, R 0 is the initial radius of the particle, PV is the internal pressure of the particle, η L is the dynamic viscosity of the medium, P O is the hydrostatic pressure, P ac (t) is the sound pressure, c is the velocity of the ultrasonic wave in the medium, and P G0 is the pressure inside the particle.

进一步,所述超声模块包括脉冲发生接收器、发送换能器、接收换能器、前置放大器;所述信号分析处理模块包括示波器和计算机;Further, the ultrasonic module includes a pulse generator receiver, a sending transducer, a receiving transducer, and a preamplifier; the signal analysis and processing module includes an oscilloscope and a computer;

所述脉冲发生接收器,其用于为所述发送换能器提供驱动电压,并将经前置放大器放大的超声波回波信号提供给所述示波器进行显示;The pulse generating receiver is used to provide a driving voltage for the transmitting transducer, and provide the ultrasonic echo signal amplified by the preamplifier to the oscilloscope for display;

所述发送换能器,其用于根据所述驱动电压输出相应频率的超声波至微纳米粒子;The sending transducer is used to output ultrasonic waves of a corresponding frequency to micro-nano particles according to the driving voltage;

所述接收换能器,其接收由微纳米粒子反射和散射的超声波回波信号,并将接收的超声波回波信号输出至前置放大器进行放大;The receiving transducer receives ultrasonic echo signals reflected and scattered by micro-nano particles, and outputs the received ultrasonic echo signals to a preamplifier for amplification;

所述计算机,其用于对示波器上显示的信号进行读取,根据超声波回波信号得到微纳米粒子的背向散射强度,并基于特征公式求得微纳米粒子的表面张力和弹性系数。The computer is used to read the signal displayed on the oscilloscope, obtain the backscattering intensity of the micro-nano particles according to the ultrasonic echo signal, and obtain the surface tension and elastic coefficient of the micro-nano particles based on the characteristic formula.

上述进一步技术方案的有益效果是:通过由脉冲发送接收器、发送/接收换能器、前置放大器组成的超声模块,可以发射和接受超声波,实现了接收和发射的一体化,减少了不必要的操作和设备的麻烦,同时可以根据测试的需要,随时的改变所用的超声频率,实现不同频率的超声波的检测,同时,可以检测出不同粒子的临界外部作用力的大小,确定粒子的临界值,在进行检测时,更不会对检测人员造成伤害。The beneficial effect of the above-mentioned further technical scheme is: through the ultrasonic module composed of the pulse transmitting receiver, the transmitting/receiving transducer and the preamplifier, the ultrasonic wave can be transmitted and received, the integration of receiving and transmitting has been realized, and unnecessary The operation and equipment are troublesome. At the same time, according to the needs of the test, the ultrasonic frequency used can be changed at any time to realize the detection of ultrasonic waves of different frequencies. At the same time, the critical external force of different particles can be detected and the critical value of the particle can be determined. , When testing, it will not cause harm to the testing personnel.

进一步,所述检测器皿为圆柱形水槽,所述发送换能器和接收换能器安装在所述圆柱形水槽的顶部;所述消声模块相对应的置于所述圆柱形水槽的底部,用于吸收所述圆柱形水槽中多余的超声波信号。Further, the detection vessel is a cylindrical water tank, and the sending transducer and the receiving transducer are installed on the top of the cylindrical water tank; the noise reduction module is correspondingly placed at the bottom of the cylindrical water tank, Used to absorb redundant ultrasonic signals in the cylindrical water tank.

上述进一步技术方案的有益效果是:将发送换能器、接收换能器与消声模块相对的设置在圆柱形水槽的顶部和底部,使消声模块能够很好的消除杂声、杂波,提高和确保检测的准确性。The beneficial effect of the above further technical solution is: the sending transducer, the receiving transducer and the noise reduction module are arranged on the top and bottom of the cylindrical water tank oppositely, so that the noise reduction module can eliminate noise and clutter well, Improve and ensure the accuracy of detection.

进一步,所述消声模块为消声瓦或消声棉等消声材料。Further, the sound-absorbing module is made of sound-absorbing materials such as sound-absorbing tiles or sound-absorbing cotton.

进一步,所述步骤S20其具体为:通过微流控制制备技术制备微纳米粒子,利用如超高速摄像机等实验设备,通过对微纳米粒子制备的记录,得出微纳米粒子个数、微纳米粒子的浓度参数。Further, the step S20 specifically includes: preparing micro-nano particles through micro-flow control preparation technology, using experimental equipment such as ultra-high-speed cameras, and recording the preparation of micro-nano particles to obtain the number of micro-nano particles, micro-nano particles concentration parameter.

上述进一步技术方案的有益效果是:通过微流控制备技术,达到了微纳米级别,同时确保了绝大部分微纳米粒子的统一尺寸,保证了测试粒子有很好的单一性,还有,利用微流控技术,还可以改变粒子的尺寸,制备出不同大小的粒子,用于检测不同大小的粒子的表面张力和弹性系数。The beneficial effect of the above further technical solution is: through the microfluidic preparation technology, the micro-nano level is achieved, and at the same time, the uniform size of most of the micro-nano particles is ensured, which ensures that the test particles have a good singleness. In addition, the use of Microfluidic technology can also change the size of particles to prepare particles of different sizes for testing the surface tension and elastic coefficient of particles of different sizes.

进一步,该测量方法还包括如下步骤:Further, the measurement method also includes the following steps:

步骤60:控制超声模块向待检测的微纳米粒子发送所需频率的超声波,通过调节超声波的声压,检测出微纳米粒子的临界点,记录此时的声压;调节超声波的频率,检测出在不同频率下,微纳米粒子处于临界点时的声压;Step 60: Control the ultrasonic module to send ultrasonic waves of the required frequency to the micro-nano particles to be detected, detect the critical point of the micro-nano particles by adjusting the sound pressure of the ultrasonic waves, and record the sound pressure at this time; adjust the frequency of the ultrasonic waves to detect At different frequencies, the sound pressure of micro-nano particles at the critical point;

步骤70:通过恒温控制器调节器皿内的温度,重复执行步骤60,确定最佳条件下的微纳米粒子的临界点。Step 70: Regulate the temperature in the vessel through a thermostat controller, repeat step 60, and determine the critical point of micro-nano particles under optimal conditions.

本发明的有益效果是:本发明所述方法可以实现在同一测试系统和测试环境下对微纳米粒子的弹性系数和表面张力进行精确检测,为研究弹性系数和表面张力的关系提供精确的实验数据,因而可以更加深入地了解材料的特性,提高材料的使用寿命、质量。本发明利用超声波进行检测,超声波向性好,穿透能力强,易于获得较集中的声能,可在气体、液体、固体、固熔体等介质中有效传播;可传递很强的能量,会产生反射、干涉、叠加和共振现象,在液体介质中传播时,可在界面上产生强烈的冲击和空化现象;因而,本发明所述方法不会受到检测介质和检测的对象的限制,使得本发明应用广泛。The beneficial effects of the present invention are: the method of the present invention can realize accurate detection of the elastic coefficient and surface tension of micro-nano particles under the same test system and test environment, and provide accurate experimental data for studying the relationship between elastic coefficient and surface tension , so we can have a deeper understanding of the characteristics of the material and improve the service life and quality of the material. The invention uses ultrasonic waves for detection, and the ultrasonic waves have good tropism, strong penetrating ability, easy to obtain relatively concentrated sound energy, and can effectively propagate in media such as gas, liquid, solid, solid solution, etc.; can transmit strong energy, and will Produce reflection, interference, superposition and resonance phenomenon, when propagating in liquid medium, can produce strong shock and cavitation phenomenon on the interface; Therefore, the method of the present invention will not be subject to the restriction of detection medium and detection object, make The invention has wide application.

另外,在本发明所述方法中,通过恒温水槽,提供一个稳定的测试环境,不会受到外界环境和条件的限制和影响,通过消声模块,将多余的超声波进行吸收,可以有效减少超声杂波等干扰,确保了测试的精确度;通过由脉冲发送接收器、发送/接收换能器、前置放大器组成的超声模块,可以发射和接受超声波,实现了接收和发射的一体化,减少了不必要的操作和设备的麻烦,同时可以根据测试的需要,随时的改变所用的超声频率,实现不同频率的超声波的检测,同时,可以检测出不同粒子的临界外部作用力的大小,确定粒子的临界值,在进行检测时,更不会对检测人员造成伤害。In addition, in the method of the present invention, a stable test environment is provided through a constant temperature water tank, which will not be restricted and affected by the external environment and conditions, and the redundant ultrasonic waves are absorbed through the noise reduction module, which can effectively reduce ultrasonic noise. Interference such as waves ensures the accuracy of the test; through the ultrasonic module composed of pulse sending receiver, sending/receiving transducer, and preamplifier, ultrasonic waves can be transmitted and received, realizing the integration of receiving and transmitting, reducing the Unnecessary operation and equipment troubles. At the same time, according to the needs of the test, the ultrasonic frequency used can be changed at any time to realize the detection of ultrasonic waves of different frequencies. At the same time, the critical external force of different particles can be detected to determine the particle size. The critical value will not cause harm to the testing personnel during testing.

另外,本发明所述方法还可以测得不同条件下的微纳米粒子临界点,可以通过确定最佳条件下的微纳米粒子的临界点直接控制粒子的破裂,特别是医学领域可以有广泛的应用,有利于微纳米材料的研究。In addition, the method of the present invention can also measure the critical point of micro-nano particles under different conditions, and can directly control the rupture of particles by determining the critical point of micro-nano particles under optimal conditions, especially in the field of medicine, which can be widely used , which is conducive to the research of micro-nano materials.

附图说明Description of drawings

图1为微纳米粒子性能参数的测量系统结构示意图。Figure 1 is a schematic structural diagram of a measurement system for performance parameters of micro-nano particles.

具体实施方式Detailed ways

以下结合附图对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。The principles and features of the present invention are described below in conjunction with the accompanying drawings, and the examples given are only used to explain the present invention, and are not intended to limit the scope of the present invention.

本发明一种微纳米粒子性能参数的测量方法,包括如下步骤:A method for measuring performance parameters of micro-nano particles of the present invention comprises the following steps:

步骤S10:搭建一微纳米粒子性能参数的测量系统,图1为微纳米粒子性能参数的测量系统结构示意图;如图1所示,该测量系统,包括:检测器皿1,用于承载待检测的微纳米粒子4;恒温控制调节器:用于调节检测器皿1内的温度;超声模块,用于将超声波发射至微纳米粒子4,接收由微纳米粒子4反射和散射的超声波回波信号,并将超声波回波信号传输至信息分析处理模块;消声模块3,用于吸收检测器皿1中多余的超声波信号;信号分析处理模块,用于对超声波回波信号进行处理得到微纳米粒子4的背向散射强度,并基于特征公式求得微纳米粒子4的表面张力和弹性系数。Step S10: Build a measurement system for the performance parameters of micro-nano particles. FIG. 1 is a schematic structural diagram of the measurement system for the performance parameters of micro-nano particles; as shown in FIG. Micro-nano particles 4; constant temperature control regulator: used to adjust the temperature in the detection vessel 1; ultrasonic module, used to transmit ultrasonic waves to the micro-nano particles 4, receive ultrasonic echo signals reflected and scattered by the micro-nano particles 4, and The ultrasonic echo signal is transmitted to the information analysis and processing module; the noise elimination module 3 is used to absorb the redundant ultrasonic signal in the detection vessel 1; the signal analysis and processing module is used to process the ultrasonic echo signal to obtain the background of the micro-nano particle 4 Scattering intensity, and based on the characteristic formula to obtain the surface tension and elastic coefficient of the micro-nano particle 4.

在本具体实施例中,超声模块包括脉冲发生接收器、发送换能器、接收换能器、前置放大器;信号分析处理模块包括示波器和计算机;脉冲发生接收器,其用于为发送换能器提供驱动电压,并将经前置放大器放大的超声波回波信号提供给所述示波器进行显示;发送换能器,其用于根据所述驱动电压输出相应频率的超声波至微纳米粒子4;接收换能器,其接收由微纳米粒子4反射和散射的超声波回波信号,并将接收的超声波回波信号输出至前置放大器进行放大;计算机,其用于对示波器上显示的信号进行读取,根据超声波回波信号得到微纳米粒子4的背向散射强度,基于特征公式求得微纳米粒子4的表面张力和弹性系数。在本具体实施例中,检测器皿1为圆柱形水槽,发送换能器和接收换能器安装在圆柱形水槽的前壁;消声模块3相对应的置于圆柱形水槽的底部,用于吸收圆柱形水槽中多余的超声波信号,能够很好的消除杂声、杂波的干扰,提高和确保检测的准确性。In this specific embodiment, the ultrasonic module includes a pulse generation receiver, a sending transducer, a receiving transducer, and a preamplifier; the signal analysis and processing module includes an oscilloscope and a computer; the pulse generation receiver is used for sending a transducer The device provides the driving voltage, and provides the ultrasonic echo signal amplified by the preamplifier to the oscilloscope for display; the sending transducer is used to output the ultrasonic wave of the corresponding frequency to the micro-nano particle 4 according to the driving voltage; the receiving The transducer, which receives the ultrasonic echo signal reflected and scattered by the micro-nano particle 4, and outputs the received ultrasonic echo signal to the preamplifier for amplification; the computer, which is used to read the signal displayed on the oscilloscope , the backscattering intensity of the micro-nanoparticle 4 is obtained according to the ultrasonic echo signal, and the surface tension and elastic coefficient of the micro-nanoparticle 4 are obtained based on the characteristic formula. In this specific embodiment, the detection vessel 1 is a cylindrical water tank, and the sending transducer and the receiving transducer are installed on the front wall of the cylindrical water tank; the noise reduction module 3 is correspondingly placed at the bottom of the cylindrical water tank for Absorbing redundant ultrasonic signals in the cylindrical water tank can well eliminate the interference of noise and clutter, and improve and ensure the accuracy of detection.

步骤20:制备微纳米粒子4,并记录微纳米粒子4个数、微纳米粒子4的浓度;步骤S20其具体为:通过微流控制制备技术制备微纳米粒子4,利用超高速摄像机,通过对微纳米粒子4制备的记录,得出微纳米粒子4个数、微纳米粒子4的浓度参数;采用微流控制备技术,达到微纳米级别,确保了绝大部分微纳米粒子4的统一尺寸,保证了测试粒子有很好的单一性,另外,利用微流控技术,还可以改变颗粒的尺寸,制备出不同大小的颗粒,用于检测不同大小的颗粒的表面张力和弹性系数。Step 20: Prepare micro-nano particles 4, and record the number of micro-nano particles 4 and the concentration of micro-nano particles 4; Step S20 is specifically: prepare micro-nano particles 4 by micro-fluidic control preparation technology, use ultra-high-speed cameras, pass through The records of the preparation of micro-nano particles 4 obtained the number of micro-nano particles 4 and the concentration parameters of micro-nano particles 4; the use of micro-fluidic preparation technology reached the micro-nano level, ensuring the uniform size of most of the micro-nano particles 4, It ensures that the test particles have a good singleness. In addition, using microfluidic technology, the size of the particles can also be changed to prepare particles of different sizes, which are used to detect the surface tension and elastic coefficient of particles of different sizes.

步骤30:向检测器皿1内放置固液连续相介质2,通过恒温控制器调节器皿内的温度达到所需温度,待温度稳定后,将所述微纳米粒子4置于所述固液连续相介质2中,并维持检测器皿1内温度恒定。通过恒温控制器,可以使得检测时刻保持在一个稳定的环境下,可以有效地避免外界环境对检测结果的影响,同时,可以通过调节恒温水槽的温度,实现在不同温度下的检测,能够确定在不同温度下,颗粒的不同状态,得到颗粒的具体情况,有利于综合的检测粒子,而不会收到外界环境和条件的影响,保证了测试的准确性;使用固液连续相介质2可将微纳米粒子在介质中的运动参数作为空间点和时间的连续函数,因而可以采用数学工具来求解其性能参数;另外超声波在固液连续介质中无明显衰减,对检测的效果和回波的强度影响小。Step 30: Place the solid-liquid continuous phase medium 2 in the detection vessel 1, adjust the temperature in the vessel to the required temperature through a thermostatic controller, and place the micro-nano particles 4 in the solid-liquid continuous phase after the temperature is stable medium 2, and maintain a constant temperature in the detection vessel 1. Through the constant temperature controller, the detection can be kept in a stable environment at all times, and the influence of the external environment on the detection results can be effectively avoided. At the same time, the detection at different temperatures can be realized by adjusting the temperature of the constant temperature water tank. At different temperatures and different states of the particles, the specific situation of the particles can be obtained, which is conducive to the comprehensive detection of particles without being affected by the external environment and conditions, ensuring the accuracy of the test; using the solid-liquid continuous phase medium 2 can The motion parameters of micro-nano particles in the medium are continuous functions of space points and time, so mathematical tools can be used to solve their performance parameters; in addition, ultrasonic waves have no obvious attenuation in solid-liquid continuum media, and have no effect on the detection effect and echo intensity. Small impact.

步骤40:控制超声模块向微纳米粒子4发送所需频率的超声波,记录施加的声压,实时观测并记录微纳米粒子4的半径变化情况;具体的,在本实施例中使用脉冲发生接收器、发送换能器、接收换能器、前置放大器作为超声模块,可以发送特定频率的超声波,并实现接收,确保了频率的单一性,检测的准确性,并且可以通过不同频率来进行检测,确定不同频率、声压条件下,颗粒的稳定和力学特性,而不会受到限制,可以得到更加精准的测试结果。Step 40: Control the ultrasonic module to send ultrasonic waves of the required frequency to the micro-nanoparticles 4, record the applied sound pressure, and observe and record the change of the radius of the micro-nanoparticles 4 in real time; specifically, in this embodiment, a pulse generator receiver is used , Transmitting transducers, receiving transducers, and preamplifiers are used as ultrasonic modules, which can send ultrasonic waves of a specific frequency and achieve reception, ensuring the singleness of frequency and the accuracy of detection, and can be detected by different frequencies. Determine the stability and mechanical properties of particles under different frequencies and sound pressure conditions without being limited, and more accurate test results can be obtained.

步骤50:超声模块接收由微纳米粒子4反射和散射的超声波回波信号,并将超声波回波信号传输至信息分析处理模块;由信号分析处理模块对超声波回波信号进行处理得到微纳米粒子4的背向散射强度;在本实施例中,信号分析处理模块包括示波器和计算机;示波器用于显示超声波回波信号,计算机用于对示波器上显示的信号进行读取,根据超声波回波信号得到微纳米粒子4的背向散射强度;Step 50: The ultrasonic module receives the ultrasonic echo signal reflected and scattered by the micro-nano particle 4, and transmits the ultrasonic echo signal to the information analysis and processing module; the signal analysis and processing module processes the ultrasonic echo signal to obtain the micro-nano particle 4 In the present embodiment, the signal analysis and processing module includes an oscilloscope and a computer; the oscilloscope is used to display the ultrasonic echo signal, and the computer is used to read the signal displayed on the oscilloscope, and obtain the microwave according to the ultrasonic echo signal. the backscattering intensity of the nanoparticles 4;

步骤60:信号分析处理模块基于特征公式求得微纳米粒子4的表面张力和弹性系数。所述步骤S60中基于特征公式求得微纳米粒子4的表面张力和弹性系数,其具体为:Step 60: The signal analysis and processing module obtains the surface tension and elastic coefficient of the micro-nano particles 4 based on the characteristic formula. In the step S60, the surface tension and elastic coefficient of the micro-nano particles 4 are obtained based on the characteristic formula, which is specifically:

弹性系数Ks由以下特征公式(1)和(2)计算出:The elastic coefficient K s is calculated by the following characteristic formulas (1) and (2):

II sthe s II == 11 99 ** NVΣSNVΣS -- -- -- (( 11 ))

ΣSΣS == 44 ππ 99 KK 44 RR 66 {{ (( KK SS -- KK KK )) 22 ++ 11 33 (( 33 (( ρρ SS -- ρρ LL )) 22 ρρ SS ++ ρρ LL )) 22 }} -- -- -- (( 22 ))

其中,Is为微纳米粒子背向散射强度,I为入射声波的强度,N为微纳米粒子的个数,V为微纳米粒子的体积,∑S为单个散射微纳米粒子的有效散射面积,ρS为微纳米粒子的密度,ρL为介质的密度,K为气体多变指数,R为随时间变化的微纳米粒子的半径;Wherein, I s is the backscattering intensity of micro-nanoparticles, I is the intensity of incident acoustic wave, N is the number of micro-nanoparticles, V is the volume of micro-nanoparticles, ΣS is the effective scattering area of a single scattering micro-nanoparticles, ρ S is the density of the micro-nano particles, ρ L is the density of the medium, K is the gas variability index, and R is the radius of the micro-nano particles changing with time;

表面张力σ由以下特征公式(3)、(4)、(5)给出:The surface tension σ is given by the following characteristic formulas (3), (4), (5):

RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( ∂∂ RR ∂∂ tt )) 22 == 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 22 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP 00 -- pp acac (( tt )) ]] -- -- -- (( 33 ))

(( 11 -- 22 ∂∂ RR ∂∂ tt cc )) RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( 11 -- 44 ∂∂ RR ∂∂ tt 33 cc )) (( ∂∂ RR ∂∂ tt )) 22 == (( 11 ++ RR cc dd dtdt )) 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 33 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP 00 -- PP acac (( tt )) ]]

(( 44 ))

(( 11 -- ∂∂ RR ∂∂ tt cc )) RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( 11 -- 44 ∂∂ RR ∂∂ tt 33 cc )) (( ∂∂ RR ∂∂ tt )) 22 == (( 11 ++ ∂∂ RR ∂∂ tt cc ++ RR cc dd dtdt )) 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 33 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP 00 -- PP acac (( tt )) ]] -- -- -- (( 55 ))

其中,ρL为介质的密度,R为随时间变化的粒子的半径,R0为粒子的初始半径,PV为粒子的内部压力,ηL为介质的动力粘度,PO为流体静压力,Pac(t)为声压,c为介质中超声波的速度,PG0为粒子内部的压强,又Among them, ρ L is the density of the medium, R is the radius of the particle changing with time, R 0 is the initial radius of the particle, PV is the internal pressure of the particle, η L is the dynamic viscosity of the medium, P O is the hydrostatic pressure, P ac (t) is the sound pressure, c is the velocity of the ultrasonic wave in the medium, P G0 is the pressure inside the particle, and

PP GG 00 == PP 00 -- PP VV ++ 22 σσ RR 00 -- -- -- (( 66 ))

上述特征方程(3)是Rayleigh-Plesset方程(即瑞利-金斯方程),Rayleigh-Plesset方程是Lord Rayleigh(瑞利)最早提出的,用于分析粒子的动态压力和表面张力等力学特性的特征方程;The above characteristic equation (3) is the Rayleigh-Plesset equation (i.e. the Rayleigh-Jins equation). The Rayleigh-Plesset equation was first proposed by Lord Rayleigh (Rayleigh), and is used to analyze the mechanical properties of particles such as dynamic pressure and surface tension. characteristic equation;

上述特征方程(4)是Herring方程(即赫林公式);特征方程(5)是Keller-Miksis方程(即凯勒-米克西斯方程);Herring方程和Keller-Miksis方程是Prosperetti(普罗斯佩雷蒂)最早提出,适用于求解在粒子振动个引起的半径衰减的情况下的表面张力值。Above-mentioned characteristic equation (4) is Herring equation (being Herring's formula); Characteristic equation (5) is Keller-Miksis equation (being Keller-Miksis equation); Herring equation and Keller-Miksis equation are Prosperetti (Prosperetti Peretti) first proposed that it is suitable for solving the surface tension value in the case of particle vibration caused by radius attenuation.

该测量方法还包括如下步骤:The measurement method also includes the steps of:

步骤60:控制超声模块向待检测的微纳米粒子4发送所需频率的超声波,通过调节超声波的声压,检测出微纳米粒子4的临界点,记录此时的声压;调节超声波的频率,检测出在不同频率下,微纳米粒子4处于临界点时的声压;在本实施例中,具体的,由超声模块的脉冲发送接收器提供驱动电压,经由发送换能器,转换成所需频率的超声波,将发送换能器垂直的对准要检测的微纳米粒子4,通过调节超声波的声压,检测出微纳米粒子4的临界点,将此时的声压记录下来,并将其进行相关计算;将发送换能器的频率进行调节,然后在不同的频率的情况下,调节超声波的声压,检测出微纳米粒子4在不同的超声波频率的条件下,不同的临界点,并将其进行记录;Step 60: Control the ultrasonic module to send ultrasonic waves of the required frequency to the micro-nanoparticles 4 to be detected, detect the critical point of the micro-nanoparticles 4 by adjusting the sound pressure of the ultrasonic waves, and record the sound pressure at this time; adjust the frequency of the ultrasonic waves, Detect the sound pressure when the micro-nano particle 4 is at the critical point at different frequencies; in this embodiment, specifically, the pulse transmitter receiver of the ultrasonic module provides the driving voltage, and converts it into the required voltage through the transmitter transducer. Frequency of ultrasonic waves, the sending transducer is vertically aligned with the micro-nano particles 4 to be detected, by adjusting the sound pressure of the ultrasonic waves, the critical point of the micro-nano particles 4 is detected, the sound pressure at this time is recorded, and its Carry out relevant calculations; adjust the frequency of the sending transducer, and then adjust the sound pressure of the ultrasonic wave at different frequencies to detect the different critical points of the micro-nanoparticles 4 under different ultrasonic frequencies, and record it;

步骤70:通过恒温控制器调节器皿内的温度,重复执行步骤60,确定最佳条件下的微纳米粒子4的临界点。Step 70: Adjust the temperature in the vessel through a thermostat controller, repeat step 60, and determine the critical point of micro-nanoparticles 4 under optimal conditions.

本发明所述方法利用固液连续相介质中自由微纳米粒子对超声波的背向散射强度与入射强度比值,以及声压、粒子浓度、粒子尺寸、介质粘度、介质密度等参数来计算得到粒子的特征力学参数;可以更好的了解微纳米粒子的特性,通过检测粒子的弹性系数和表面张力,以及不同参数的设置,能够更好地研究在什么条件下,粒子是最稳定,使用寿命最长,更可以通过确定最佳条件下的微纳米粒子的临界点直接控制粒子的破裂,特别是医学领域应用更加广泛,有利于微纳米材料的研究。The method of the present invention uses the ratio of the backscattering intensity of free micro-nano particles to ultrasonic waves in the solid-liquid continuous phase medium to the incident intensity, as well as parameters such as sound pressure, particle concentration, particle size, medium viscosity, and medium density to calculate the particle density. Characteristic mechanical parameters; can better understand the characteristics of micro-nano particles. By detecting the elastic coefficient and surface tension of the particles, as well as the settings of different parameters, it is possible to better study the conditions under which the particles are the most stable and have the longest service life. , and can directly control the breakage of particles by determining the critical point of micro-nano particles under the optimal conditions, especially in the medical field, which is more widely used, which is beneficial to the research of micro-nano materials.

以上所述实施步骤和方法仅仅表达了本发明的一种实施方式,描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。在不脱离本发明专利构思的前提下,所作的变形和改进应当都属于本发明专利的保护范围。The implementation steps and methods described above only express an implementation mode of the present invention, and the description is relatively specific and detailed, but it should not be construed as limiting the patent scope of the present invention. Under the premise of not departing from the concept of the patent of the present invention, the deformation and improvement made should all belong to the protection scope of the patent of the present invention.

Claims (7)

1.一种微纳米粒子性能参数的测量方法,其特征在于,包括如下步骤:1. A method for measuring performance parameters of micro-nanoparticles, characterized in that, comprising the steps: 步骤10:搭建一微纳米粒子性能参数的测量系统,该测量系统包括:Step 10: Build a measurement system for the performance parameters of micro-nano particles, which includes: 检测器皿,用于承载待检测的微纳米粒子;The detection vessel is used to carry the micro-nano particles to be detected; 恒温控制调节器:用于控制、调节检测器皿内的温度达到所需的温度值;Constant temperature control regulator: used to control and adjust the temperature in the detection vessel to reach the required temperature value; 超声模块,用于将超声波发射至微纳米粒子,接收由微纳米粒子反射和散射的超声波回波信号,并将超声波回波信号传输至信息分析处理模块;The ultrasonic module is used to transmit ultrasonic waves to the micro-nano particles, receive the ultrasonic echo signals reflected and scattered by the micro-nano particles, and transmit the ultrasonic echo signals to the information analysis and processing module; 消声模块,用于吸收检测器皿中多余的超声波信号;Noise elimination module for absorbing redundant ultrasonic signals in the detection vessel; 信号分析处理模块,用于对超声波回波信号进行处理得到微纳米粒子的背向散射强度,并基于特征公式求得微纳米粒子的表面张力和弹性系数;The signal analysis and processing module is used to process the ultrasonic echo signal to obtain the backscattering intensity of the micro-nano particles, and obtain the surface tension and elastic coefficient of the micro-nano particles based on the characteristic formula; 步骤20:制备微纳米粒子,并记录微纳米粒子个数、微纳米粒子的浓度;Step 20: Prepare micro-nano particles, and record the number of micro-nano particles and the concentration of micro-nano particles; 步骤30:向检测器皿内放置固液连续相介质,通过恒温控制器调节器皿内的温度达到所需温度,待温度稳定后,将所述微纳米粒子置于所述固液连续相介质中,并维持检测器皿内温度恒定;Step 30: Place the solid-liquid continuous phase medium in the detection vessel, adjust the temperature in the vessel to reach the required temperature through a thermostat controller, and place the micro-nano particles in the solid-liquid continuous phase medium after the temperature is stable, And maintain a constant temperature in the detection vessel; 步骤40:控制超声模块向微纳米粒子发送所需频率的超声波,记录施加的声压,实时观测并记录微纳米粒子的半径变化情况;Step 40: Control the ultrasonic module to send ultrasonic waves of the required frequency to the micro-nano particles, record the applied sound pressure, observe and record the change of the radius of the micro-nano particles in real time; 步骤50:超声模块接收由微纳米粒子反射和散射的超声波回波信号,并将超声波回波信号传输至信息分析处理模块;由信号分析处理模块对超声波回波信号进行处理得到微纳米粒子的背向散射强度;Step 50: The ultrasonic module receives the ultrasonic echo signals reflected and scattered by the micro-nano particles, and transmits the ultrasonic echo signals to the information analysis and processing module; the signal analysis and processing module processes the ultrasonic echo signals to obtain the background of the micro-nano particles to the scattering intensity; 步骤60:信号分析处理模块基于特征公式求得微纳米粒子的表面张力和弹性系数。Step 60: The signal analysis and processing module obtains the surface tension and elastic coefficient of the micro-nano particles based on the characteristic formula. 2.根据权利要求1所述一种微纳米粒子性能参数的测量方法,其特征在于:所述步骤S60中基于特征公式求得微纳米粒子的表面张力和弹性系数,其具体为:弹性系数Ks由以下特征公式(1)和(2)计算出:2. according to the measuring method of a kind of micro-nanoparticle performance parameter described in claim 1, it is characterized in that: in the described step S60, obtain surface tension and elastic coefficient of micro-nanoparticle based on characteristic formula, it is specifically: elastic coefficient K s is calculated from the following characteristic formulas (1) and (2): II sthe s II == 11 99 ** NVΣSNVΣS -- -- -- (( 11 )) ΣSΣS == 44 ππ 99 KK 44 RR 66 {{ KK SS -- KK KK 22 ++ 11 33 (( 33 (( ρρ SS -- ρρ LL )) 22 ρρ SS ++ ρρ LL )) 22 }} -- -- -- (( 22 )) 其中,Is为微纳米粒子背向散射强度,I为入射声波的强度,N为微纳米粒子的个数,V为微纳米粒子的体积,ΣS为单个散射微纳米粒子的有效散射面积,ρS为微纳米粒子的密度,ρL为介质的密度,K为气体多变指数,R为随时间变化的微纳米粒子的半径;Among them, I s is the backscattering intensity of micro-nanoparticles, I is the intensity of incident acoustic wave, N is the number of micro-nanoparticles, V is the volume of micro-nanoparticles, ΣS is the effective scattering area of a single scattering micro-nanoparticles, ρ S is the density of micro-nano particles, ρ L is the density of the medium, K is the gas variability index, and R is the radius of the micro-nano particles changing with time; 表面张力σ由以下特征公式(3)、(4)、(5)给出:The surface tension σ is given by the following characteristic formulas (3), (4), (5): RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( ∂∂ RR ∂∂ tt )) 22 == 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 22 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP Oo -- pp acac (( tt )) ]] -- -- -- (( 33 )) (( 11 -- 22 ∂∂ RR ∂∂ tt cc )) RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( 11 -- 44 ∂∂ RR ∂∂ tt 33 cc )) (( ∂∂ RR ∂∂ tt )) 22 == (( 11 ++ RR cc dd dtdt )) 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 33 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP Oo -- PP acac (( tt )) ]] -- -- -- (( 44 )) (( 11 -- ∂∂ RR ∂∂ tt cc )) RR ∂∂ 22 RR ∂∂ tt 22 ++ 33 22 (( 11 -- 44 ∂∂ RR ∂∂ tt 33 cc )) (( ∂∂ RR ∂∂ tt )) 22 == (( 11 ++ ∂∂ RR ∂∂ tt cc ++ RR cc dd dtdt )) 11 ρρ LL [[ PP GG 00 (( RR 00 RR )) 33 kk ++ PP VV -- 22 σσ RR -- 44 ηη LL ∂∂ RR ∂∂ tt RR -- PP Oo -- PP acac (( tt )) ]] -- -- -- (( 55 )) 其中,ρL为介质的密度,R为随时间变化的粒子的半径,R0为粒子的初始半径,PV为粒子的内部压力,ηL为介质的动力粘度,PO为流体静压力,Pac(t)为声压,c为介质中超声波的速度,PG0为粒子内部的压强。Among them, ρ L is the density of the medium, R is the radius of the particle changing with time, R 0 is the initial radius of the particle, PV is the internal pressure of the particle, η L is the dynamic viscosity of the medium, P O is the hydrostatic pressure, P ac (t) is the sound pressure, c is the velocity of the ultrasonic wave in the medium, and P G0 is the pressure inside the particle. 3.根据权利要求1或2所述一种微纳米粒子性能参数的测量方法,其特征在于:3. according to the measuring method of a kind of micronano particle performance parameter described in claim 1 or 2, it is characterized in that: 所述超声模块包括脉冲发生接收器、发送换能器、接收换能器、前置放大器;所述信号分析处理模块包括示波器和计算机;The ultrasonic module includes a pulse generator receiver, a sending transducer, a receiving transducer, and a preamplifier; the signal analysis and processing module includes an oscilloscope and a computer; 所述脉冲发生接收器,其用于为所述发送换能器提供驱动电压,并将经前置放大器放大的超声波回波信号提供给所述示波器进行显示;The pulse generating receiver is used to provide a driving voltage for the transmitting transducer, and provide the ultrasonic echo signal amplified by the preamplifier to the oscilloscope for display; 所述发送换能器,其用于根据所述驱动电压输出相应频率的超声波至微纳米粒子;The sending transducer is used to output ultrasonic waves of a corresponding frequency to micro-nano particles according to the driving voltage; 所述接收换能器,其接收由微纳米粒子反射和散射的超声波回波信号,并将接收的超声波回波信号输出至前置放大器进行放大;The receiving transducer receives ultrasonic echo signals reflected and scattered by micro-nano particles, and outputs the received ultrasonic echo signals to a preamplifier for amplification; 所述计算机,其用于对示波器上显示的信号进行读取,根据超声波回波信号得到微纳米粒子的背向散射强度,并基于特征公式求得微纳米粒子的表面张力和弹性系数。The computer is used to read the signal displayed on the oscilloscope, obtain the backscattering intensity of the micro-nano particles according to the ultrasonic echo signal, and obtain the surface tension and elastic coefficient of the micro-nano particles based on the characteristic formula. 4.根据权利要求3所述一种微纳米粒子性能参数的测量方法,其特征在于:所述检测器皿为圆柱形水槽,所述发送换能器和接收换能器安装在所述圆柱形水槽的顶部;所述消声模块相对应的置于所述圆柱形水槽的底部,用于吸收所述圆柱形水槽中多余的超声波信号。4. The measuring method of a kind of micro-nano particle performance parameter according to claim 3, is characterized in that: described detection vessel is cylindrical water tank, and described sending transducer and receiving transducer are installed in described cylindrical water tank the top of the tank; the sound-absorbing module is correspondingly placed at the bottom of the cylindrical water tank for absorbing redundant ultrasonic signals in the cylindrical water tank. 5.根据权利要求1或2所述一种微纳米粒子性能参数的测量方法,其特征在于:所述消声模块为消声瓦或消声棉。5. The method for measuring performance parameters of micro-nano particles according to claim 1 or 2, characterized in that: the noise-absorbing module is an anechoic tile or an anechoic cotton. 6.根据权利要求1或2所述一种微纳米粒子性能参数的测量方法,其特征在于,所述步骤S20其具体为:通过微流控制制备技术制备微纳米粒子,利用超高速摄像机,通过对微纳米粒子制备的记录,得出微纳米粒子个数、微纳米粒子的浓度参数。6. According to claim 1 or 2, a method for measuring performance parameters of micro-nano particles is characterized in that, said step S20 is specifically: preparing micro-nano particles through micro-fluidic control preparation technology, using an ultra-high-speed camera, by The number of micro-nano particles and the concentration parameters of micro-nano particles are obtained by recording the preparation of micro-nano particles. 7.根据权利要求1或2所述一种微纳米粒子性能参数的测量方法,其特征在于:该测量方法还包括如下步骤:7. according to claim 1 or 2 described a kind of measuring method of micro-nano particle performance parameter, it is characterized in that: this measuring method also comprises the following steps: 步骤60:控制超声模块向待检测的微纳米粒子发送所需频率的超声波,通过调节超声波的声压,检测出微纳米粒子的临界点,记录此时的声压;调节超声波的频率,检测出在不同频率下,微纳米粒子处于临界点时的声压;Step 60: Control the ultrasonic module to send ultrasonic waves of the required frequency to the micro-nano particles to be detected, detect the critical point of the micro-nano particles by adjusting the sound pressure of the ultrasonic waves, and record the sound pressure at this time; adjust the frequency of the ultrasonic waves to detect At different frequencies, the sound pressure of micro-nano particles at the critical point; 步骤70:通过恒温控制器调节器皿内的温度,重复执行步骤60,确定最佳条件下的微纳米粒子的临界点。Step 70: Regulate the temperature in the vessel through a thermostat controller, repeat step 60, and determine the critical point of micro-nano particles under optimal conditions.
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