TWI648530B - Rheometer - Google Patents
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- TWI648530B TWI648530B TW106122926A TW106122926A TWI648530B TW I648530 B TWI648530 B TW I648530B TW 106122926 A TW106122926 A TW 106122926A TW 106122926 A TW106122926 A TW 106122926A TW I648530 B TWI648530 B TW I648530B
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Abstract
本發明提供一種流變儀,其係利用棒狀物與磁場之間的交互作用,造成棒狀物的振動,藉由雷射位移系統判斷棒狀物振動造成鏡子的位移量,並利用振輻電壓及相位差計算出待測流體的流變性質,包含儲存模數及消散模數。再者,流變儀可進行線上量測。 The invention provides a rheometer which utilizes the interaction between a rod and a magnetic field to cause vibration of the rod, and the laser displacement system determines the displacement of the mirror caused by the vibration of the rod, and utilizes the vibration The voltage and phase difference calculate the rheological properties of the fluid to be tested, including the storage modulus and the dissipation modulus. Furthermore, the rheometer can be used for on-line measurements.
Description
本發明是關於一種流變儀,特別是關於一種線上流變儀。 This invention relates to a rheometer, and more particularly to an in-line rheometer.
材料的流變行為係包含液體的黏性行為及固體的彈性行為。一般而言,完全彈性體係在受到外力時,可瞬間達到平衡的形變,且在外力除去後,完全彈性體會將外力對其做功所儲存的能量釋放;而完全黏性體係在受到外力後,形變隨時間變化呈線性關係,且在外力除去後,黏性體會將其所儲存的動能以熱的形式消散,此過程為不可逆。然而,當材料的形變性質與時間相關,則此材料的流變行為係介於完全彈性體與完全黏性體之間,即此材料同時具有彈性行為與黏性行為的黏彈性材料(viscoelastic materials),且其可逆性會隨著外力作用的時間增長而降低。 The rheological behavior of a material involves the viscous behavior of the liquid and the elastic behavior of the solid. In general, a fully elastic system can instantaneously reach a balanced deformation when subjected to an external force, and after the external force is removed, the complete elastic body will release the energy stored by the external force for its work; and the fully viscous system is deformed after being subjected to an external force. It changes linearly with time, and after the external force is removed, the viscous body will dissipate its stored kinetic energy in the form of heat, which is irreversible. However, when the deformation property of the material is related to time, the rheological behavior of the material is between the fully elastic body and the complete viscous body, that is, the viscoelastic material in which the material has both elastic behavior and viscous behavior. And its reversibility will decrease as the time of external force increases.
流變儀(rheometer)是用來量測材料之流變行為的儀器,主要是用以量測流體材料。流變儀係對待測材料施加外力,並測量其行為(包含不可逆的流動變形與可逆的彈性變形)。黏度係流體的基本流變性質之一,其係流體分子間摩擦力的度量值。若分子間的摩擦力大,則流體不易流 動,因此,黏度可視為流體抵抗流動的程度。黏度係定義為流體承受剪應力時,剪應力與剪應變梯度的比值。 A rheometer is an instrument used to measure the rheological behavior of a material, primarily to measure fluid material. The rheometer applies an external force to the material to be tested and measures its behavior (including irreversible flow deformation and reversible elastic deformation). One of the basic rheological properties of a viscosity fluid, which is a measure of the friction between fluid molecules. If the friction between the molecules is large, the fluid does not flow easily. Movement, therefore, viscosity can be considered as the extent to which the fluid resists flow. Viscosity is defined as the ratio of shear stress to shear strain gradient when a fluid is subjected to shear stress.
對牛頓流體(Newtonian fluid)而言,黏度不隨剪切率的改變而改變,而對非牛頓流體而言,黏度為剪切率的函數。因此,若為牛頓流體,黏度(η)與應力(τ)的關係式如下式(I):
若為非牛頓流體,則黏度需變更為時間的函數[η(t)]或稱為複合黏度(complex viscosity,η*),則黏度與應力的關係式如下式(II),其中式(II)中包含儲存模數(storage modulus,G’)及消散模數(loss modulus,G”),如下式(III)及式(IV):
G'(ω)=ωη"(ω) (III) G ' (ω)=ω η "( ω ) (III)
G"(ω)=ωη'(ω) (IV) G"(ω)=ω η' ( ω ) (IV)
因此,黏度(η)及黏彈模數(G)皆為頻率的函數,且可以下式(V)及式(VI)表示:
習知流變儀包含錐板式、平行板式、旋轉式及毛細管式。毛細管式流變儀係目前應用最廣泛的流變儀之一,可用來量測材料在巨觀下的流變特性。旋轉式流變儀則是藉由旋轉產生剪切力,將待測材料置於相對轉動的夾具下 進行剪切流動的量測。然而,上述習知流變儀並無法做為線上儀器,提供線上即時流變資訊。雖然目前亦有可提供線上即時量測資訊的線上儀器,但通常僅為線上黏度儀(viscometer),僅能提供待測材料的黏滯係數,而無法進一步量測待測材料的儲存模數與消散模數。 Conventional rheometers include cone and plate, parallel plate, rotary and capillary. Capillary rheometers are one of the most widely used rheometers available today to measure the rheological properties of materials under superviews. The rotary rheometer generates shear force by rotation, and places the material to be tested under a relatively rotating fixture. The measurement of the shear flow is performed. However, the above-mentioned conventional rheometer cannot be used as an online instrument to provide online real-time rheological information. Although there are currently online instruments that provide online real-time measurement information, they are usually only a line viscometer. They only provide the viscosity coefficient of the material to be tested, and cannot further measure the storage modulus of the material to be tested. Dissipate the modulus.
有鑑於此,亟須提供一種可以提供儲存模數與消散模數之資訊的線上儀器,以提供完整且即時的線上流變資訊。 In view of this, there is no need to provide an online instrument that provides information on the storage modulus and dissipation modulus to provide complete and instantaneous online rheological information.
本發明之一態樣是提供一種流變儀,其係藉由棒狀物係在磁場的作用下產生運動,並利用電射位移系統感測棒狀物的運動。因此,可藉由棒狀物與待測流體流固耦合作用,量測流體的流變性質。 One aspect of the present invention is to provide a rheometer that generates motion by a rod under the action of a magnetic field and senses the motion of the rod using an electro-radiation displacement system. Therefore, the rheological properties of the fluid can be measured by fluid-solid coupling of the rod to the fluid to be tested.
根據本發明之一態樣,提供一種流變儀,其係包含底座、設置在底座上的容器、設置於容器內的棒狀物、固定在棒狀之上的磁鐵、設置在棒狀物之上的鏡子、複數組線圏以及雷射位移系統。線圏係以磁鐵為中心,並環繞棒狀物。容器具有容置待測流體的空間。雷射位移系統係用以判斷鏡子的位移量,其係包含雷射源及位置感測器。雷射源係用以發射光線至鏡子,以使鏡子將光線反射回雷射位移系統。位置感測器係用以感應被反射的光線,以判斷鏡子的位移量。 According to an aspect of the invention, there is provided a rheometer comprising a base, a container disposed on the base, a rod disposed in the container, a magnet fixed on the rod, and disposed on the rod Mirrors, complex arrays, and laser displacement systems. The wire is centered on the magnet and surrounds the rod. The container has a space for accommodating the fluid to be tested. The laser displacement system is used to determine the displacement of the mirror, which includes a laser source and a position sensor. The laser source is used to emit light to the mirror so that the mirror reflects the light back to the laser displacement system. The position sensor is used to sense the reflected light to determine the amount of displacement of the mirror.
根據本發明之一實施例,上述流變儀更包含線 圏支架及線圏底座。線圏支架係用以固定線圏,而線圏底座係圍繞底座,並用以支撐線圏支架。 According to an embodiment of the invention, the rheometer further comprises a line 圏 bracket and cable 圏 base. The cymbal bracket is used to fix the cymbal, and the cymbal base surrounds the base and is used to support the cymbal bracket.
根據本發明之一實施例,上述容器包含流入管以及流出管。流入管係設於容器的底表面,並用以使流體流入容器。流出管係包含連通底表面的中空管,並用以使流體自容器中排出。 According to an embodiment of the invention, the container comprises an inflow tube and an outflow tube. The inflow tube is provided on the bottom surface of the container and serves to allow fluid to flow into the container. The outflow tube system includes a hollow tube that communicates with the bottom surface and is used to allow fluid to drain from the container.
根據本發明之一實施例,上述流變儀更包含訊號產生器,其係用以輸入電流至線圏。 According to an embodiment of the invention, the rheometer further includes a signal generator for inputting current to the coil.
根據本發明之一實施例,上述雷射位移系統係用以根據鏡子的位移量來量測棒狀物的振動變形量。 According to an embodiment of the invention, the laser displacement system is configured to measure the amount of vibration deformation of the rod according to the displacement amount of the mirror.
根據本發明之一實施例,上述棒狀物的振動模式包含扭轉、彎曲及其組合。 According to an embodiment of the invention, the vibration mode of the rod comprises twisting, bending and combinations thereof.
根據本發明之一實施例,上述棒狀物包含複數個橢圓孔洞,且橢圓孔洞之長軸及短軸的比值為0.1至10。 According to an embodiment of the invention, the rod comprises a plurality of elliptical holes, and the ratio of the major axis to the minor axis of the elliptical hole is 0.1 to 10.
根據本發明之一實施例,上述流變儀更包含電腦裝置,其中電腦裝置係電性連接至雷射位移系統以及訊號產生器。電腦裝置係根據鏡子的位移量來檢測流體的黏彈模數,其中黏彈模數係藉由下式(1)計算:|G *| LPVS =(α×V core -β×V liquid )×f n (1) According to an embodiment of the invention, the rheometer further includes a computer device, wherein the computer device is electrically connected to the laser displacement system and the signal generator. The computer device detects the viscoelastic modulus of the fluid according to the displacement of the mirror, wherein the viscoelastic modulus is calculated by the following formula (1): | G * | LPVS = ( α × V core - β × V liquid ) × f n (1)
在式(1)中,| G * |LPVS代表黏彈模數,f代表頻率,α、β及n為校正參數,Vcore及Vliquid分別代表該容器中僅有棒狀物及包含棒狀物及流體時的振幅電壓,其係由以下式(2)及式(3)計算:V core =V core-In /V core-Out (2) In the formula (1), | G * | LPVS represents the viscoelastic modulus, f represents the frequency, α, β and n are the correction parameters, and V core and V liquid respectively represent the rods and the rods in the container. The amplitude voltage of the object and the fluid is calculated by the following equations (2) and (3): V core = V core - In / V core-Out (2)
V liquid =V liquid-In /V liquid-Out (3) V liquid = V liquid-In / V liquid-Out (3)
在式(2)中,Vcore-In代表僅有棒狀物時輸入的振幅電壓,且Vcore-Out代表輸出的振幅電壓;在式(3)中,Vliquid-In代表包含棒狀物及流體時輸入的振幅電壓,且Vliquid-Out代表輸出的振幅電壓。 In the formula (2), V core-In represents the amplitude voltage input when only the rod is present, and V core-Out represents the amplitude voltage of the output; in the formula (3), V liquid-In represents the inclusion of the rod And the amplitude voltage input when the fluid is in, and V liquid-Out represents the amplitude voltage of the output.
根據本發明之一實施例,上述電腦裝置更係用以檢測流體的損耗正切值,其係由以下式(4)計算:tan δ LPVS =γ×|tan δ liquid -tan δ core |/f N (4) According to an embodiment of the invention, the computer device is further configured to detect a loss tangent value of the fluid, which is calculated by the following formula (4): tan δ LPVS = γ × | tan δ liquid - tan δ core | / f N (4)
在式(4)中,δLPVS代表損耗正切值,f代表頻率,γ及N為校正參數,δcore及δliquid分別代表容器中僅有棒狀物及包含流體時的相位差,其係由以下式(5)及式(6)計算:tan δ core =|tan[(θ core-Out -θ core-In )π/180]| (5) In equation (4), δ LPVS represents the loss tangent, f represents the frequency, γ and N are the correction parameters, and δ core and δ liquid represent the phase difference of only the rod and the fluid in the container, respectively. Calculated by the following equations (5) and (6): tan δ core =|tan[( θ core-Out - θ core-In ) π /180]| (5)
tan δ liquid =|tan[(θ liquid-Out -θ liquid-In )π/180]| (6) Tan δ liquid =|tan[( θ liquid-Out - θ liquid-In ) π /180]| (6)
在式(5)中,θcore-In代表僅有該棒狀物時輸入的相位角,且θcore-Out代表輸出的相位角;在式(6)中,θliquid-In代表包含該流體時輸入的相位角,且θliquid-Out代表輸出的相位角。 In the formula (5), θ core-In represents the phase angle input only when the rod is present, and θ core-Out represents the phase angle of the output; in the formula (6), θ liquid-In represents the fluid contained therein. The phase angle entered, and θ liquid-Out represents the phase angle of the output.
根據本發明之一實施例,上述電腦裝置更係用以檢測流體的儲存模數及消散模數,其中儲存模數及消散模數係藉由下式(7)及式(8)計算:
G" LPVS =G' LPVS ×tan δ LPVS (8) G " LPVS = G' LPVS ×tan δ LPVS (8)
在式(7)及式(8)中,G’LPVS代表儲存模數,G”LPVS代表消散模數。 In equations (7) and (8), G' LPVS represents the storage modulus, and G" LPVS represents the dissipation modulus.
應用本發明之流變儀,可進行線上量測,其係藉由棒狀物與磁場之間的交互作用力產生振動,而量測出待 測流體的流變性質,包含黏彈模數、儲存模數及消散模數與頻率之間的關係。 By using the rheometer of the present invention, on-line measurement can be performed, which is generated by the interaction force between the rod and the magnetic field, and the measurement is performed. The rheological properties of the fluid, including the viscoelastic modulus, the storage modulus, and the relationship between the dissipation modulus and the frequency.
100‧‧‧流變儀 100‧‧‧ rheometer
110/210‧‧‧主體部分 110/210‧‧‧ body part
120‧‧‧底座 120‧‧‧Base
130/230‧‧‧容器 130/230‧‧‧ Container
132‧‧‧流入管 132‧‧‧Inflow pipe
134‧‧‧流出管 134‧‧‧ Outflow tube
136‧‧‧空間 136‧‧‧ space
138/238‧‧‧底表面 138/238‧‧‧ bottom surface
140/240‧‧‧棒狀物 140/240‧‧‧ rods
150/250‧‧‧磁鐵 150/250‧‧‧ magnet
160‧‧‧鏡子 160‧‧‧Mirror
170/270‧‧‧線圈 170/270‧‧‧ coil
172‧‧‧線圈支架 172‧‧‧ coil bracket
174‧‧‧線圈底座 174‧‧‧Coil base
180‧‧‧雷射位移系統 180‧‧‧Laser Displacement System
182‧‧‧雷射源 182‧‧‧Laser source
184‧‧‧位置感測器 184‧‧‧ position sensor
290‧‧‧固定部 290‧‧‧ fixed department
h/h1/h2‧‧‧高度 h/h 1 /h 2 ‧‧‧height
為讓本發明之上述和其他目的、特徵、優點與實施例能更明顯易懂,所附圖式之詳細說明如下:[圖1]係繪示根據本發明一實施例之流變儀的側視視圖;[圖2A]至[圖2D]係繪示根據本發明之一些實施例的流變儀之主體部分的部分剖面視圖;[圖3A]係繪示根據本發明實施例一、實施例二及比較例一的黏彈模數與頻率的關係圖;[圖3B]係繪示根據本發明實施例一、實施例二及比較例一的儲存模數與頻率的關係圖;[圖3C]係繪示根據本發明實施例一、實施例二及比較例一的消散模數與頻率的關係圖;[圖4A]係繪示根據本發明實施例三、實施例四及比較例二的黏彈模數與頻率的關係圖;[圖4B]係繪示根據本發明實施例三、實施例四及比較例二的儲存模數與頻率的關係圖;以及[圖4C]係繪示根據本發明實施例三、實施例四及比較例二的消散模數與頻率的關係圖。 The above and other objects, features, advantages and embodiments of the present invention will become more <RTIgt; <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; [Fig. 2A] to [Fig. 2D] are partial cross-sectional views showing a main portion of a rheometer according to some embodiments of the present invention; [Fig. 3A] is a view showing an embodiment according to an embodiment of the present invention. 2 and the relationship between the modulus of the viscoelastic modulus and the frequency of the first example; [Fig. 3B] is a diagram showing the relationship between the storage modulus and the frequency according to the first embodiment, the second embodiment and the first comparative example of the present invention; [Fig. 3C] FIG. 4A is a diagram showing the relationship between the dissipation modulus and the frequency according to the first embodiment, the second embodiment, and the first embodiment of the present invention; [FIG. 4A] FIG. 4A is a diagram showing the third embodiment, the fourth embodiment, and the second embodiment of the present invention. FIG. 4B is a diagram showing the relationship between the storage modulus and the frequency according to Embodiment 3, Embodiment 4 and Comparative Example 2 of the present invention; and [FIG. 4C] is based on the relationship between the storage modulus and the frequency according to Embodiment 3 of the present invention; The relationship between the dissipative modulus and the frequency of the third embodiment and the second embodiment of the present invention.
承上所述,本發明提供一種流變儀,其係藉由棒狀物與磁場之間的交互作用力產生振動,而量測出待測流體的流變性質,包含儲存模數及消散模數與頻率之間的關係。 In view of the above, the present invention provides a rheometer that generates vibration by an interaction force between a rod and a magnetic field, and measures the rheological properties of the fluid to be tested, including the storage modulus and the dissipation mode. The relationship between numbers and frequencies.
請參閱圖1,其係繪示根據本發明一實施例之流變儀100的側視視圖。流變儀100包含主體部分110及雷射位移系統180。主體部分110係包含底座120、容器130、設置在容器130內的棒狀物140、固定在棒狀物140之上的磁鐵150、設置在棒狀物140之上的鏡子160及複數組線圏170。在一實施例中,磁鐵150及鏡子160係分別設置在棒狀物140的二側面。雷射位移系統180係包含雷射源182及位置感測器184。在一實施例中,容器130係設置在底座120上,且容器130具有用以容置待測流體的空間136。 Please refer to FIG. 1, which is a side elevational view of a rheometer 100 in accordance with an embodiment of the present invention. The rheometer 100 includes a body portion 110 and a laser displacement system 180. The body portion 110 includes a base 120, a container 130, a rod 140 disposed within the container 130, a magnet 150 secured to the rod 140, a mirror 160 disposed over the rod 140, and a plurality of arrays of turns 170. In one embodiment, the magnet 150 and the mirror 160 are disposed on opposite sides of the rod 140, respectively. The laser displacement system 180 includes a laser source 182 and a position sensor 184. In one embodiment, the container 130 is disposed on the base 120 and the container 130 has a space 136 for receiving a fluid to be tested.
在一實施例中,容器130可選擇性地包含流入管132及流出管134,其中流入管132係設於容器130的底表面138,以使待測流體流入容器130,而流出管134係用以使待測流體自容器中排出。在一具體例中,流出管134為具有高度h的中空管,其係連通底表面138,以排出待測流體。流出管134的高度h可根據待測流體的體積做調整,當待測流體的體積高度超過高度h,則過多的待測流體將自流出管134排出,藉以控制量測時待測流體的體積。 In one embodiment, the container 130 can optionally include an inflow tube 132 and an outflow tube 134, wherein the inflow tube 132 is disposed on the bottom surface 138 of the container 130 to allow the fluid to be tested to flow into the container 130, and the outflow tube 134 is used. In order to discharge the fluid to be tested from the container. In one embodiment, the outflow tube 134 is a hollow tube having a height h that communicates with the bottom surface 138 to expel the fluid to be tested. The height h of the outflow pipe 134 can be adjusted according to the volume of the fluid to be tested. When the volume height of the fluid to be tested exceeds the height h, excess fluid to be tested will be discharged from the outflow pipe 134, thereby controlling the volume of the fluid to be measured during the measurement. .
在一實施例中,線圏170係以磁鐵150為中心,環繞棒狀物140。在一實施例中,流變儀100可選擇性地包含訊號產生器(圖未繪示),其係用以輸入電流至線圏170, 以使線圏170產生均勻磁場,並與棒狀物140上的磁鐵150產生交互作用,進而驅動棒狀物140,使棒狀物140發生振動。在一實施例中,棒狀物140的振動模式包含扭轉、彎曲及其組合。在一具體例中,線圏170為2組亥姆霍茲線圏(Helmholtz coil),其中可為一組垂直線圏與一組水平線圏。在一實施例中,流變儀100可選擇性地包含線圏支架172及線圏底座174,其中線圏支架172可用以固定線圏170,而線圏底座174可設置為圍繞底座120,並用以支撐線圏支架172。 In one embodiment, the turn 170 is centered around the magnet 150 and surrounds the wand 140. In one embodiment, the rheometer 100 can optionally include a signal generator (not shown) for inputting current to the coil 170. The coil 170 is caused to generate a uniform magnetic field and interacts with the magnet 150 on the rod 140 to drive the rod 140 to vibrate the rod 140. In an embodiment, the vibration mode of the rod 140 includes twisting, bending, and combinations thereof. In one embodiment, the turns 170 are two sets of Helmholtz coils, which may be a set of vertical turns and a set of horizontal turns. In an embodiment, the rheometer 100 can optionally include a coil bracket 172 and a coil base 174, wherein the coil bracket 172 can be used to fix the coil 170, and the coil base 174 can be disposed to surround the base 120, and To support the wire 圏 bracket 172.
在一實施例中,雷射位移系統180係用以判斷鏡子160的位移量,其係利用雷射源182發出雷射光至鏡子160,而鏡子160會將光線反射回雷射位移系統180,再藉由位置感測器184感應反射之光線,以判斷鏡子160的位移量。在一實施例中,鏡子160的位移量係根據上述棒狀物140之振動所產生,因此,雷射位移系統180係根據鏡子160的位移量來量測棒狀物140之振動所產生的振動變形量。在一具體例中,雷射源182發出的雷射光為波長632奈米的雷射光。 In one embodiment, the laser displacement system 180 is used to determine the amount of displacement of the mirror 160, which utilizes a laser source 182 to emit laser light to the mirror 160, and the mirror 160 reflects the light back to the laser displacement system 180. The reflected light is sensed by the position sensor 184 to determine the amount of displacement of the mirror 160. In one embodiment, the amount of displacement of the mirror 160 is generated according to the vibration of the rod 140 described above. Therefore, the laser displacement system 180 measures the vibration generated by the vibration of the rod 140 according to the displacement amount of the mirror 160. The amount of deformation. In one embodiment, the laser light emitted by the laser source 182 is laser light having a wavelength of 632 nm.
流變儀100係可用以在不同溫度與頻率下,量測非牛頓流體或膠體懸浮液的流變性質。在一實施例中,流變儀100量測的頻率範圍為10-6Hz至106Hz。在另一實施例中,流變儀100可量測的溫度範圍為0℃至300℃。 The rheometer 100 can be used to measure the rheological properties of a non-Newtonian fluid or a colloidal suspension at different temperatures and frequencies. In one embodiment, the rheometer 100 measures a frequency ranging from 10 -6 Hz to 10 6 Hz. In another embodiment, the rheometer 100 can measure a temperature ranging from 0 °C to 300 °C.
流變儀100係藉由棒狀物140的振動,而使待測流體與棒狀物140產生流固耦合的交互作用,進而量測待測 流體的流變性質(包含儲存模數與消散模數)。因此,棒狀物140的設計會對流固耦合的交互作用產生影響。舉例而言,當棒狀物140與待測流體的接觸面積增加時,可增加流固耦合的交互作用,進而提升待測流體之流變性質的量測精確度。在一實施例中,棒狀物140包含複數個橢圓孔洞,其中橢圓孔洞之長軸及短軸的比值為0.1至10。控制橢圓孔洞之長軸及短軸的比值除了可使棒狀物140與待測流體的接觸面積增加,進而增加量測的靈敏度之外,亦可藉此降低棒狀物140的彈性勁度,以增加量測低頻率訊號的準確度。在一實施例中,橢圓孔洞的體積百分比可為0%至99%,較佳為40%至70%。藉由調整橢圓孔洞的體積百分比亦可增加棒狀物140與待測流體的接觸面積。在一實施例中,棒狀物140之斷面的直徑為約0.1mm至約3mm,棒狀物140之長度為約3mm至約30mm。在另一實施例中,棒狀物140之表面粗糙度為約10μm至約500μm,其係藉由改變棒狀物140對待測流體的擾動狀況,以優化檢測待測流體之流變性質的精確度。 The rheometer 100 is a fluid-solid coupling interaction between the fluid to be tested and the rod 140 by the vibration of the rod 140, and then the measurement is to be tested. The rheological properties of the fluid (including the storage modulus and the dissipation modulus). Therefore, the design of the rod 140 can have an effect on the interaction of fluid-solid coupling. For example, when the contact area of the rod 140 with the fluid to be tested is increased, the interaction of fluid-solid coupling can be increased, thereby improving the measurement accuracy of the rheological properties of the fluid to be tested. In one embodiment, the rod 140 includes a plurality of elliptical holes, wherein the ratio of the major axis to the minor axis of the elliptical hole is 0.1 to 10. Controlling the ratio of the major axis to the minor axis of the elliptical hole can increase the contact stiffness of the rod 140 and the fluid to be tested, thereby increasing the sensitivity of the measurement, thereby reducing the elastic stiffness of the rod 140. Increase the accuracy of low frequency signals by increasing the amount. In an embodiment, the volume percentage of the elliptical holes may be from 0% to 99%, preferably from 40% to 70%. The contact area of the rod 140 with the fluid to be tested can also be increased by adjusting the volume percentage of the elliptical hole. In one embodiment, the cross-section of the rod 140 has a diameter of from about 0.1 mm to about 3 mm and the length of the rod 140 is from about 3 mm to about 30 mm. In another embodiment, the surface roughness of the rod 140 is from about 10 [mu]m to about 500 [mu]m by altering the disturbance of the fluid to be measured by the rod 140 to optimize the accuracy of detecting the rheological properties of the fluid to be tested. degree.
在一實施例中,棒狀物140在待測流體中的比例為10%至100%,即待測流體在空間136中的高度與棒狀物140之高度的比例,此比例係根據待測流體的黏度不同而調整。一般而言,量測黏度較高的流體時,使棒狀物140在待測流體中的比例較低;反之,量測黏度較低的流體時,須使棒狀物140與較多待測流體接觸,則棒狀物140在待測流體中的比例較高。在一實施例中,棒狀物140之材料可為矽 凝膠、矽膠、橡膠、高分子[例如:聚甲基丙烯酸甲酯(polymethyl methacrylate,PMMA)或聚乙烯醇(poly vinyl alcohol,PVA)]、金屬、合金或陶瓷。 In an embodiment, the ratio of the rod 140 in the fluid to be tested is 10% to 100%, that is, the ratio of the height of the fluid to be tested in the space 136 to the height of the rod 140, which is determined according to the test. The viscosity of the fluid is adjusted differently. In general, when measuring a fluid with a higher viscosity, the proportion of the rod 140 in the fluid to be tested is lower; conversely, when measuring a fluid having a lower viscosity, the rod 140 is required to be tested more. When the fluid is in contact, the proportion of the rod 140 in the fluid to be tested is high. In an embodiment, the material of the rod 140 may be 矽 Gel, silicone, rubber, polymer [for example: polymethyl methacrylate (PMMA) or polyvinyl alcohol (PVA)], metal, alloy or ceramic.
流變儀100可根據量測需求,改變主體部分110的配置,其中包含開放式、封閉式、封閉管路式及可拋棄式。請參閱圖2A至圖2D,其係繪示根據本發明之一些實施例的流變儀之主體部分210的部分剖面視圖。圖2A係繪示開放式流變儀之主體部分210的配置示意圖,其中棒狀物240之高度h1係超過容器230之高度h2,且線圏270保持以磁鐵250為中心,環繞棒狀物240,因此線圏270係在容器230之上方。開放式流變儀較佳係用於線上量測沒有壓力的流體,例如在開放式渠道裡的流體。 The rheometer 100 can change the configuration of the body portion 110 according to the measurement requirements, including open type, closed type, closed line type and disposable type. 2A-2D, which are partial cross-sectional views of a body portion 210 of a rheometer in accordance with some embodiments of the present invention. 2A is a schematic view showing the configuration of the main body portion 210 of the open rheometer, wherein the height h 1 of the rod 240 exceeds the height h 2 of the container 230, and the coil 270 remains centered on the magnet 250, and surrounds the rod. The object 240 is such that the turns 270 are above the container 230. Open rheometers are preferably used to measure fluids without pressure, such as fluids in open channels.
圖2B係繪示封閉式流變儀之主體部分210的配置示意圖,其中棒狀物240之高度h1係低於容器230之高度h2,且線圏270保持以磁鐵250為中心,環繞棒狀物240,因此線圏270不高於容器230之高度h2。封閉式流變儀較佳係用於線上量測有壓力的流體,例如在封閉式管內流動的流體。須注意的是,由於封閉式流變儀之高度h1低於高度h2,因此,封閉式流變儀所量測的流體必須為透明或半透明,以使雷射可至少部分穿透流體,進而被鏡子(圖2B未繪示)反射。 2B is a schematic view showing the configuration of the main body portion 210 of the closed rheometer, wherein the height h 1 of the rod 240 is lower than the height h 2 of the container 230, and the coil 270 remains centered on the magnet 250, and surrounds the rod. The shape 240 is such that the turns 270 are not higher than the height h 2 of the container 230. A closed rheometer is preferably used to measure a pressurized fluid on-line, such as a fluid flowing within a closed tube. It should be noted that since the height h 1 of the closed rheometer is lower than the height h 2 , the fluid measured by the closed rheometer must be transparent or translucent so that the laser can at least partially penetrate the fluid. And then reflected by the mirror (not shown in Figure 2B).
圖2C係繪示封閉管路式流變儀之主體部分210的配置示意圖,其中棒狀物240不與容器230之底表面238接觸,而係利用容器230之頂表面固定。棒狀物240係凸出 於容器230,故磁鐵250亦在容器230上方,且線圏270同樣在容器230上方。封閉管路式流變儀與封閉式流變儀類似,皆係用於線上量測有壓力的流體,其差異在於封閉管路式流變儀之磁鐵250係在容器230上方,則鏡子亦在容器230上方,因此,封閉管路式流變儀可用以量測非透明的流體。 2C is a schematic view showing the configuration of the main body portion 210 of the closed-line rheometer, wherein the rod 240 is not in contact with the bottom surface 238 of the container 230, but is fixed by the top surface of the container 230. Rod 240 is protruding In the container 230, the magnet 250 is also above the container 230, and the coil 270 is also above the container 230. A closed-line rheometer is similar to a closed rheometer in that it is used to measure a pressurized fluid on-line. The difference is that the magnet 250 of the closed-line rheometer is attached to the vessel 230, and the mirror is also Above the container 230, a closed line rheometer can therefore be used to measure non-transparent fluid.
圖2D係繪示可拋棄式流變儀之主體部分210的配置示意圖,其中棒狀物240及磁鐵250係與上方的固定部290連接,且棒狀物240及磁鐵250同樣係凸出於容器230,而線圏270在容器230上方。可拋棄式流變儀之棒狀物240為可拋棄式的,主要係用以量測會對棒狀物240造成污染的流體,例如具有污染性的流體或會在量測過程中發生化學反應而固化的流體。 2D is a schematic view showing the configuration of the main body portion 210 of the disposable rheometer, wherein the rod 240 and the magnet 250 are connected to the upper fixing portion 290, and the rod 240 and the magnet 250 are also protruded from the container. 230, while the coil 270 is above the container 230. The disposable rheometer rod 240 is disposable, primarily for measuring fluids that can contaminate the rod 240, such as contaminating fluids or chemical reactions that may occur during the measurement process. And the solidified fluid.
在一實施例中,流變儀100可選擇性地包含電腦裝置(圖未繪示),電腦裝置係電性連接雷射位移系統180及訊號產生器(圖未繪示),並根據鏡子160的位移量來檢測待測流體的振幅電壓(amplitude voltage)及相位差(phase lags),進而獲得待測流體的黏彈模數(viscoelastic modulus)、儲存模數及消散模數。應用本發明之流變儀100,須分別進行僅有棒狀物140(即容器中未添加待測流體)時及容器130內含待測流體(即容器中同時含有棒狀物140及待測流體)時的量測。 In one embodiment, the rheometer 100 can optionally include a computer device (not shown), and the computer device is electrically connected to the laser displacement system 180 and the signal generator (not shown), and according to the mirror 160 The displacement amount is used to detect the amplitude voltage and the phase lags of the fluid to be tested, thereby obtaining the viscoelastic modulus, the storage modulus, and the dissipation modulus of the fluid to be tested. The rheometer 100 of the present invention is required to perform only the rod 140 (ie, the fluid to be tested is not added in the container) and the container 130 contains the fluid to be tested (ie, the rod 140 is contained in the container and is to be tested) Measurement when fluid).
首先,流變儀100係藉由分別計算僅有棒狀物140及包含待測流體時的振幅電壓,其係分別以Vcore及Vliquid表示,進而利用下式(1)計算出待測流體的黏彈模 數。在一實施例中,流變儀100量測的黏彈模數範圍為0.1N/m2(Pa)至107N/m2。 First, the rheometer 100 calculates the amplitude voltages when only the rods 140 and the fluid to be tested are respectively calculated by V core and V liquid , and then calculates the fluid to be tested by using the following formula (1). The viscoelastic modulus. In one embodiment, the viscoelastic modulus measured by the rheometer 100 ranges from 0.1 N/m 2 (Pa) to 10 7 N/m 2 .
|G *| LPVS =(α×V core -β×V liquid )×f n (1) | G * | LPVS = ( α × V core - β × V liquid ) × f n (1)
在式(1)中,| G * |LPVS代表黏彈模數,f代表頻率,α、β及n為校正參數。在一實施例中,α及β皆為0.1,而n為2。然而,根據不同待測流體或不同振動模式,校正參數會有所差異,故本發明不限制校正參數值α、β及n。 In the formula (1), | G * | LPVS represents the viscoelastic modulus, f represents the frequency, and α, β, and n are correction parameters. In one embodiment, both α and β are 0.1 and n is 2. However, the correction parameters may vary depending on the fluid to be tested or the different vibration modes, so the present invention does not limit the correction parameter values α, β, and n.
其中,Vcore及Vliquid係分別利用式(2)及式(3)計算:V core =V core-In /V core-Out (2) Among them, V core and V liquid are calculated by equations (2) and (3), respectively: V core = V core-In / V core-Out (2)
V liquid =V liquid-In /V liquid-Out (3) V liquid = V liquid-In / V liquid-Out (3)
在式(2)中,Vcore-In代表僅有棒狀物時輸入的振幅電壓,且Vcore-Out代表輸出的振幅電壓。在式(3)中,Vliquid-In代表包含棒狀物及流體時輸入的振幅電壓,且Vliquid-Out代表輸出的振幅電壓。Vcore-In及Vliquid-In係從輸入的電壓訊號得知,而Vcore-Out及Vliquid-Out則是藉由雷射位移系統提供之棒狀物的振動變形量所獲得。 In the formula (2), V core-In represents the amplitude voltage input when only the rod is present, and V core-Out represents the amplitude voltage of the output. In the formula (3), V liquid-In represents an amplitude voltage input when a rod and a fluid are contained, and V liquid-Out represents an amplitude voltage of the output. V core-In and V liquid-In are known from the input voltage signal, while V core-Out and V liquid-Out are obtained by the vibration deformation amount of the rod provided by the laser displacement system.
再者,流變儀100藉由分別計算僅有棒狀物140及包含待測流體時的相位差,其係分別以δcore及δliquid表示,進而利用δcore及δliquid的正切值及下式(4)計算出待測流體的損耗正切值(loss tangent)。δcore及δliquid係分別利用式(5)及式(6)計算:tan δ LPVS =γ×|tan δ liquid -tan δ core |/f N (4) Furthermore, the rheometer 100 calculates the phase difference when only the rod 140 and the fluid to be tested are respectively calculated, which are represented by δ core and δ liquid , respectively, and further utilizes the tangent values of δ core and δ liquid and Equation (4) calculates the loss tangent of the fluid to be tested. The δ core and δ liquid systems are calculated using equations (5) and (6), respectively: tan δ LPVS = γ × | tan δ liquid -tan δ core | / f N (4)
在式(4)中,δLPVS代表待測流體的損耗正切值,f代表頻率,γ及N為校正參數。在一實施例中,γ為10000,而N為1。然而,根據不同待測流體或不同振動模式,校正參 數會有所差異,故本發明不限制校正參數值γ及N。 In equation (4), δ LPVS represents the loss tangent of the fluid to be tested, f represents the frequency, and γ and N are the correction parameters. In one embodiment, γ is 10,000 and N is 1. However, the correction parameters may vary depending on the fluid to be tested or the different vibration modes, so the present invention does not limit the correction parameter values γ and N.
tan δ core =|tan[(θ core-Out -θ core-In )π/180]| (5) Tan δ core =|tan[( θ core-Out - θ core-In ) π /180]| (5)
tan δ liquid =|tan[(θ liquid-Out -θ liquid-In )π/180]| (6) Tan δ liquid =|tan[( θ liquid-Out - θ liquid-In ) π /180]| (6)
在式(5)中,θcore-In代表僅有棒狀物時輸入的相位角,且θcore-Out代表輸出的相位角。在式(6)中,θliquid-In代表包含該流體時輸入的相位角,且θliquid-Out代表輸出的相位角。θcore-In及θliquid-In是來自於輸入電流後,來自線圏170的電磁訊號與訊號產生器提供的訊號之間的相位角差,而θcore-Out及θliquid-Out是在輸入電流後,棒狀物140的振動產生的訊號與訊號產生器提供的訊號之間的相位角差。 In the formula (5), θ core-In represents the phase angle input when only the rod is present, and θ core-Out represents the phase angle of the output. In the formula (6), θ liquid-In represents the phase angle input when the fluid is contained, and θ liquid-Out represents the phase angle of the output. θ core-In and θ liquid-In are the phase angle difference between the electromagnetic signal from the coil 170 and the signal provided by the signal generator after the input current, and θ core-Out and θ liquid-Out are at the input. After the current, the phase difference between the signal generated by the vibration of the rod 140 and the signal provided by the signal generator.
黏彈模數係來自於儲存模數(storage modulus,G’)及消散模數(loss modulus,G”),且黏彈模數亦和待測流體的黏滯係數相關,其係具有上述之式(VI)的關係:
再者,相位差與儲存模數及消散模數具有下式(VII)的關係式:
因此,藉由上述獲得之黏彈模數及相位差,儲存模數及消散模數可分別利用下式(7)及式(8)求得:
G" LPVS =G' LPVS ×tan δ LPVS (8)。 G " LPVS = G' LPVS × tan δ LPVS (8).
如上所述,本發明之流變儀100係藉由流固耦合及磁場的交互作用,利用振幅電壓及相位差,計算出待測流體的黏彈模數、儲存模數及消散模數,進而求得待測流體 的黏滯係數。再者,流變儀100係適合與其他儀器結合,以線上偵測待測流體的流變性質。 As described above, the rheometer 100 of the present invention calculates the viscoelastic modulus, the storage modulus, and the dissipation modulus of the fluid to be tested by using the interaction of the fluid-solid coupling and the magnetic field, and using the amplitude voltage and the phase difference. Find the fluid to be tested Viscosity coefficient. Furthermore, the rheometer 100 is suitable for combination with other instruments to detect the rheological properties of the fluid to be tested on-line.
以下利用數個實施例以說明本發明之應用,然其並非用以限定本發明,本發明技術領域中具有通常知識者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾。 The following examples are used to illustrate the application of the present invention, and are not intended to limit the present invention. Those skilled in the art can make various changes without departing from the spirit and scope of the present invention. Retouching.
實施例一、實施例二及比較例一係分別利用本發明提供之流變儀100以及目前市面上販售的流變儀(Thermo Haake,德國),測量5wt%的聚乙烯醇水溶液的黏彈模數,其中流變儀100分別利用彎曲(實施例一)及扭轉(實施例二)的二種振動模式。請參閱圖3A至圖3C,圖3A係繪示根據本發明實施例一、實施例二及比較例一之黏彈模數與頻率的關係圖;圖3B係繪示根據本發明實施例一、實施例二及比較例一之儲存模數與頻率的關係圖;而圖3C係繪示根據本發明實施例一、實施例二及比較例一之消散模數與頻率的關係圖。 The first embodiment, the second embodiment and the comparative example 1 respectively measure the viscoelasticity of a 5 wt% aqueous solution of polyvinyl alcohol by using the rheometer 100 provided by the present invention and a rheometer (Thermo Haake, Germany) currently on the market. The modulus, wherein the rheometer 100 utilizes two modes of vibration, namely bending (Example 1) and twisting (Example 2). Referring to FIG. 3A to FIG. 3C, FIG. 3A is a diagram showing the relationship between the modulus of the viscoelastic modulus and the frequency according to the first embodiment, the second embodiment and the first comparative example, and FIG. 3B is a diagram showing the relationship between the modulus of the viscoelastic modulus and the frequency according to the first embodiment of the present invention; FIG. 3C is a diagram showing the relationship between the dissipation modulus and the frequency according to the first embodiment, the second embodiment, and the first embodiment of the present invention. FIG.
如圖3A至圖3C所示,實施例一及實施例二所測得之聚乙烯醇的黏彈模數、儲存模數及消散模數相近,表示流變儀100的二種振動模式均適用於測量聚乙烯醇的流變性質。再者,圖3A顯示實施例一及實施例二所測得之聚乙烯醇的黏彈模數皆與比較例一測得之黏彈模數相近。如圖3B及圖3C所示,實施例一及實施例二與比較例一所測得之 聚乙烯醇的儲存模數及消散模數亦相近,尤其在100Hz至102Hz的頻率區域。據此,流變儀100在量測聚乙烯醇的黏彈模數、儲存模數及消散模數時皆具有足夠的準確度。 As shown in FIG. 3A to FIG. 3C , the viscoelastic modulus, the storage modulus and the dissipation modulus of the polyvinyl alcohol measured in the first embodiment and the second embodiment are similar, indicating that the two vibration modes of the rheometer 100 are applicable. For measuring the rheological properties of polyvinyl alcohol. Furthermore, FIG. 3A shows that the viscoelastic modulus of the polyvinyl alcohol measured in the first embodiment and the second embodiment is similar to the viscoelastic modulus measured in the first comparative example. As shown in FIG. 3B and FIG. 3C, the storage modulus and the dissipation modulus of the polyvinyl alcohol measured in the first embodiment and the second embodiment are similar to those in the first embodiment, especially in the frequency region of 10 0 Hz to 10 2 Hz. . Accordingly, the rheometer 100 has sufficient accuracy in measuring the viscoelastic modulus, the storage modulus, and the dissipation modulus of the polyvinyl alcohol.
與上述聚乙烯醇水溶液進行相同的量測,差異是測量流體為二氧化鋯漿液(ZrO2 slurry)。請參閱圖4A至圖4C,圖4A係繪示根據本發明實施例三、實施例四及比較例二的黏彈模數與頻率的關係圖;圖4B係繪示根據本發明實施例三、實施例四及比較例二的儲存模數與頻率的關係圖;圖4C係繪示根據本發明實施例三、實施例四及比較例二的消散模數與頻率的關係圖。 The same measurement was carried out as the above aqueous solution of polyvinyl alcohol, the difference being that the measuring fluid was a zirconium dioxide slurry (ZrO 2 slurry). 4A to FIG. 4C, FIG. 4A is a diagram showing the relationship between the modulus of the viscoelastic modulus and the frequency according to the third embodiment, the fourth embodiment and the second comparative example of the present invention; FIG. 4B is a diagram showing the relationship between the modulus of the viscoelastic modulus and the frequency according to the third embodiment of the present invention; FIG. 4C is a diagram showing the relationship between the dissipation modulus and the frequency according to Embodiment 3, Embodiment 4, and Comparative Example 2 of the present invention. FIG.
如圖4A所示,實施例三及實施例四所測得之二氧化鋯的黏彈模數之變化趨勢及數值均相近,且在100Hz至102Hz的頻率區段,實施例三及實施例四與比較例二測得之黏彈模數也幾乎相同。如圖4B所示,實施例三、實施例四及比較例一所量測之二氧化鋯的儲存模數曲線幾乎完全重疊。圖4C顯示,實施例三及實施例四測得之二氧化鋯的消散模數行為相近。相較於比較例二,消散模數行為似乎略有差異,但在101Hz至102Hz的頻率範圍內,消散模數的數值仍是幾乎相同。 As shown in FIG. 4A, the change trend and the numerical value of the viscoelastic modulus of the zirconia measured in the third embodiment and the fourth embodiment are similar, and in the frequency section of 10 0 Hz to 10 2 Hz, the third embodiment The viscoelastic modulus measured in the fourth embodiment and the second comparative example is also almost the same. As shown in FIG. 4B, the storage modulus curves of the zirconium dioxide measured in Example 3, Example 4 and Comparative Example 1 almost completely overlap. 4C shows that the dissipative modulus behavior of the zirconium dioxide measured in the third embodiment and the fourth embodiment is similar. Compared to Comparative Example 2, the dissipative modulus behavior seems to be slightly different, but in the frequency range of 10 1 Hz to 10 2 Hz, the values of the dissipative modulus are still almost the same.
根據上述實施例,本發明之流變儀的二種振動模式確實可用以量測流體的流變性質,且所得之流變性質亦 與市售儀器相近。再者,本發明之流變儀不僅可量測黏彈模數,更可量測流體之儲存模數及消散模數,且可用以進行線上量測,以即時提供流體的流變性質。 According to the above embodiment, the two vibration modes of the rheometer of the present invention can be used to measure the rheological properties of the fluid, and the resulting rheological properties are also Similar to commercially available instruments. Furthermore, the rheometer of the present invention can not only measure the viscoelastic modulus, but also measure the storage modulus and dissipation modulus of the fluid, and can be used for on-line measurement to provide the rheological properties of the fluid in real time.
雖然本發明已以數個實施例揭露如上,然其並非用以限定本發明,在本發明所屬技術領域中任何具有通常知識者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 While the invention has been described above in terms of several embodiments, it is not intended to limit the scope of the invention, and the invention may be practiced in various embodiments without departing from the spirit and scope of the invention. The scope of protection of the present invention is defined by the scope of the appended claims.
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JPH07226316A (en) * | 1994-02-14 | 1995-08-22 | Toyohisa Fujita | Magnetic electrorheology fluid and its manufacture |
TW343260B (en) * | 1996-07-02 | 1998-10-21 | Lord Coproration | Controllable vibration apparatus, magnetorheological fluid damper, damper, and single tube damper |
US6564618B2 (en) * | 2000-05-18 | 2003-05-20 | Rheologics, Inc. | Electrorheological and magnetorheological fluid scanning rheometer |
CN101923033A (en) * | 2010-07-16 | 2010-12-22 | 中山大学 | Method for measuring viscosity of low-viscosity liquid and rheometer |
CN106814007A (en) * | 2015-12-01 | 2017-06-09 | 广西大学 | A kind of flow measurements computer control system |
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JPH07226316A (en) * | 1994-02-14 | 1995-08-22 | Toyohisa Fujita | Magnetic electrorheology fluid and its manufacture |
TW343260B (en) * | 1996-07-02 | 1998-10-21 | Lord Coproration | Controllable vibration apparatus, magnetorheological fluid damper, damper, and single tube damper |
US6564618B2 (en) * | 2000-05-18 | 2003-05-20 | Rheologics, Inc. | Electrorheological and magnetorheological fluid scanning rheometer |
CN101923033A (en) * | 2010-07-16 | 2010-12-22 | 中山大学 | Method for measuring viscosity of low-viscosity liquid and rheometer |
CN106814007A (en) * | 2015-12-01 | 2017-06-09 | 广西大学 | A kind of flow measurements computer control system |
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