CN102200543A - AFM (Atomic Force Microscope)-based device for performing nanoindentation measurement on surface of microparticle - Google Patents
AFM (Atomic Force Microscope)-based device for performing nanoindentation measurement on surface of microparticle Download PDFInfo
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Abstract
The invention provides an AFM (Atomic Force Microscope)-based device and method for performing nanoindentation measurement on the surface of a microparticle. The device is composed of an AFM system, a sheet-shaped plane for holding a sample to be measured is arranged on a sample platform at the top of a scanatron, a double faced adhesive tape for sticking and fixing the sample to be measured is arranged on the sheet-shaped plane, and a nanoindentation needle tip for scanning and nanoindentation operation is fixed in a needle tip holder and arranged above the sample to be measured. When the device is in use, the sample to be measured is adhered to the sheet-shaped plane with the double faced adhesive tape; the sheet-shaped plane is placed on the sample platform at the top of the scanatron; and then the nanoindentation needle tip fixed in the needle tip holder performs scanning and nanoindentation operation above the sample to be measured, wherein the nanoindentation needle tip is a diamond needle tip and has an elasticity coefficient remained between 100N/m and 300N/m and an resonance frequency of 35-65khz. According to the invention, nanoindentation measurement is successfully carried on the surface of a detected powdery microparticle sample with the particle size of 20-80 micrometers.
Description
(1) technical field:
The present invention relates to atomic force microscope technology and nano impress measuring technique, particularly a kind ofly the film on minitype particle surface is carried out analysis measuring device and method of work by these two kinds of technology.
(2) background technology:
Atomic force microscope (Atomic Force Microscopy is called for short AFM) is a kind of surface imaging technology, and the lateral resolution of AFM can reach 0.2 nanometer in the ordinary course of things, and longitudinal frame can reach 0.1 nanometer.The principle of work of atomic force microscope is to utilize the interaction between needle point atom and the sample surfaces atom to carry out the imaging of figure.Needle point is an end that is fixed on the elasticity micro-cantilever, beam of laser through the backside reflection of elasticity micro-cantilever in photoelectric detector, when needle point contacts with sample surfaces, can produce extremely faint repulsion force between the atom at needle point tip and the atom of sample surfaces, because sample surfaces is uneven, needle point can be done undulatory motion in the direction perpendicular to sample surfaces, will drive micro-cantilever so small crooked deformation takes place, cause the variation of reflected light path, thereby make to reflex to laser spot generation corresponding mobile on the photoelectric detector, can obtain the information of sample surfaces pattern by the measured micro-cantilever of this optical detection corresponding to the change in location of the scanning each point on the sample surfaces.
Nano impress is on sub-micron and nanoscale, and the mechanical property of membraneous material is characterized and measures.This mechanical meaurement technology is by needle point being applied certain pressure, make itself and material surface come in contact and produce certain deformation, write down the semi-girder deformation-displacement curve that taken place of needle point in being pressed into the material surface process simultaneously, and change into force-displacement curve, thereby study the relation of the 26S Proteasome Structure and Function of membraneous material.Can measure and study the mechanical properties such as adhesion size between at the bottom of elasticity, plastic deformation and the film of the film hardness of surfaces of various materials, elastic modulus, material and the sample substrate by this technology.This The Application of Technology field relates to the various semiconductive thin films in the integrated circuit, the surface metal plating layer of magnetic storage medium, the polymeric coating layer that surface of polymer material has specific performance, film of micro electronmechanical components and parts material surface or the like at present.The thin film mechanical performance fields of measurement of nano impress technology on the block materials surface obtained using widely, and have the particle of micro-meter scale magnitude because particle diameter is little, sample position is difficult for fixing, influence the following pin process of nano impress needle point and the selection of impression position, cause the research blank in this field.
(3) summary of the invention:
The object of the present invention is to provide a kind of minitype particle nano surface impression measurement mechanism and method of work thereof based on atomic force microscope, it is measured by the thin film coating based on the minitype particle material surface of the nano impress method measurement level of atomic force microscope technology.
Technical scheme of the present invention: a kind of measurement mechanism of minitype particle nano surface impression, it is to be made of the atomic force microscope system, comprise scanning monitor, the scanning probe microscopy main body, the magnifier display system, main frame, display, keyboard and mouse, wherein the scanning probe microscopy main body comprises pedestal, scanatron, the electronic circuit linkage unit, laser optical path, needle point frame and Zoom lens system, it is characterized in that on the sample stage at scanatron top the sheet plane (3) of laying sample (2) being arranged, the double faced adhesive tape that the sample that is adhesively fixed (2) are arranged on the sheet plane (3), among being fixed in the needle point frame nano impress needle point (1) that scans with the nano impress operation is arranged, nano impress needle point (1) places the top of sample (2).
What above-mentioned said nano impress needle point (1) adopted is the adamas needle point, and the elasticity coefficient of nano impress needle point (1) remains between 100-300 ox/rice, and resonant frequency is the 35-65 KHz.
Above-mentioned said atomic force microscope system is the Nanoscope IV type equipment of U.S. VEECO company.
The adamas needle point that above-mentioned said nano impress needle point (1) is adopted is the DNISP adamas needle point that is used for nano impress/nanometer scratch experiment that U.S. VEECO company provides.
Above-mentioned said sheet plane (3) of laying sample (2) is an iron plate.
A kind of measuring method of above-mentioned minitype particle nano surface impression based on atomic force microscope is characterized in that it has following steps:
(1) take a morsel Powdered minitype particle with micro-meter scale magnitude is made sample (2) and is sticked at gently on the sheet plane (3) that is fixed with double faced adhesive tape, with ear washing bulb sticking the unstable Powdered minitype particle that blows off, in order to avoid influence measuring process, cause the inserting needle difficulty, the sheet plane (3) that will be stained with sample (2) then is positioned on the sample stage at scanatron top of scanning probe microscopy gently;
(2) with special-purpose needle point tweezers nano impress needle point (1) is put on the needle point frame, then the needle point frame is fixed on the sample stage top at scanatron top;
(3) the focusing situation of watching from the magnifier display sample surfaces by the focal position of regulating magnifier concentrates on focus point the upper surface of some minitype particle samples (2);
(4) utilize the thick inserting needle system of atomic force microscope nano impress needle point (1) progressively to be approached the upper surface of minitype particle sample (2), when the position of the roughly imaging that on the magnifier display, can watch nano impress needle point (1), stop pin down at once, prevent to bump against particle surface;
(5) select the nano impress functional module on computers, open the interface after, select pin icon down, allow the automatic inserting needle of needle point to minitype particle sample (2) surface;
(6) when nano impress needle point (1) reaches minitype particle sample (2) surface, begin to carry out the scanning process of sample surfaces pattern, regulate sweep parameter, obtain the clear feature image of sample surfaces;
(7) treat selected carry out position that nano impress measures after, enter the nano impress pattern, regulate relevant parameters, wherein the size of activation threshold value (Trigger threshold) is 0 volt-10 volts, the Z direction raises and to be of a size of 500 nanometers-3.5 micron, sweep velocity is 0.5 hertz-2 hertz, and the X-axis scanning angle is 0 degree-30 degree, begins to carry out nano impress and measures;
(8) by changing activation threshold value (Trigger threshold), regulate the size that puts on the power on the nano impress needle point, and the semi-girder deformation-displacement curve of record nano impress needle point in being pressed into minitype particle sample surface film coating process.
The thin film coating of the minitype particle sample material surface in the above-mentioned said step (1) is that the method by magnetron sputtering obtains, change different magnetron sputtering growth conditionss, the film thickness difference of minitype particle material surface, corresponding change can take place in the homogeneous degree that can observe film from the atomic force microscope images, and the semi-girder deformation-displacement curve from the nano impress experiment can observe the change of property of thin film.
Superiority of the present invention and technique effect are: owing to nano impress technology is in the past carried out on the block materials surface, so the thin film mechanical performance fields of measurement of this technology on the block materials surface obtained using very widely; And for the Powdered minitype particle sample with micro-meter scale magnitude, particle diameter by minitype particle is little, the position of this powdered samples is not easy to fix in the sample making course, thereby can influence the following pin process of nano impress needle point and carry out nano impress the choosing of suitable impression sampling point position when measuring.The present invention has overcome this technological difficulties, is that the nano impress measuring process has been carried out on the Powdered minitype particle sample surface of 20-80 micron at grain size successfully.
(4) description of drawings:
Fig. 1 is the work structuring synoptic diagram of the related a kind of minitype particle nano surface impression measurement mechanism based on atomic force microscope of the present invention.
Wherein: 1 is the nano impress needle point, and 2 is the Powdered minitype particle sample with micro-meter scale magnitude, and 3 are the sheet plane that is used for fixing the minitype particle sample above the sample stage that is positioned over the scanatron top.
Fig. 2 for the present invention related based on the atomic force microscope system, be used for the method that nano impress is measured is carried out on the Powdered minitype particle sample surface with micro-meter scale magnitude, it is that 1.5 volts nano impress is measured the semi-girder deformation-displacement curve that is then produced that activation threshold value (Trigger threshold) is carried out on the Powdered minitype particle surface that is coated with metal nickel film
Fig. 3 the present invention related based on the atomic force microscope system, be used for the method that nano impress is measured is carried out on the Powdered minitype particle sample surface with micro-meter scale magnitude, it is that 2.5 volts nano impress is measured the semi-girder deformation-displacement curve that is then produced that activation threshold value (Trigger threshold) is carried out on the Powdered minitype particle surface that is coated with metal nickel film
(5) embodiment:
Embodiment 1: a kind of measurement mechanism (see figure 1) of the minitype particle nano surface impression based on atomic force microscope, it is to be made of the atomic force microscope system, comprise scanning monitor, the scanning probe microscopy main body, the magnifier display system, main frame, display, keyboard and mouse, wherein the scanning probe microscopy main body comprises pedestal, scanatron, the needle point frame, the electronic circuit linkage unit, laser optical path and Zoom lens system, it is characterized in that on the sample stage at scanatron top the sheet plane (3) of laying sample (2) being arranged, the double faced adhesive tape that the sample that is adhesively fixed (2) are arranged on the sheet plane (3), among being fixed in the needle point frame nano impress needle point (1) that scans with the nano impress operation is arranged, nano impress needle point (1) places the top of sample (2).
What above-mentioned said nano impress needle point (1) adopted is the adamas needle point, and the elasticity coefficient of nano impress needle point (1) remains between 100-300 ox/rice, and resonant frequency is the 35-65 KHz.
Above-mentioned said atomic force microscope system is the NanoscopeIV type equipment of U.S. VEECO company.
The adamas needle point that above-mentioned said nano impress needle point (1) is adopted is the DNISP adamas needle point that is used for nano impress/nanometer scratch experiment that U.S. VEECO company provides.
Above-mentioned said sheet plane (3) of laying sample (2) is an iron plate.
A kind of measuring method of above-mentioned minitype particle nano surface impression based on atomic force microscope is characterized in that it has following steps:
(1) take a morsel Powdered minitype particle with micro-meter scale magnitude is made sample (2) and is sticked at gently on the sheet plane (3) that is fixed with double faced adhesive tape, with ear washing bulb sticking the unstable Powdered minitype particle that blows off, in order to avoid influence measuring process, cause the inserting needle difficulty, the sheet plane (3) that will be stained with sample (2) then is positioned on the sample stage at scanatron top of scanning probe microscopy gently;
(2) with special-purpose needle point tweezers nano impress needle point (1) is put on the needle point frame, then the needle point frame is fixed on the sample stage top at scanatron top;
(3) the focusing situation of watching from the magnifier display sample surfaces by the focal position of regulating magnifier concentrates on focus point the upper surface of some minitype particle samples (2);
(4) utilize the thick inserting needle system of atomic force microscope nano impress needle point (1) progressively to be approached the upper surface of minitype particle sample (2), when the position of the roughly imaging that on the magnifier display, can watch nano impress needle point (1), stop pin down at once, prevent to bump against particle surface;
(5) select the nano impress functional module on computers, open the interface after, select pin icon down, allow the automatic inserting needle of needle point to minitype particle sample (2) surface;
(6) when nano impress needle point (1) reaches minitype particle sample (2) surface, begin to carry out the scanning process of sample surfaces pattern, regulate sweep parameter, obtain the clear feature image of sample surfaces;
(7) treat selected carry out position that nano impress measures after, enter the nano impress pattern, regulate relevant parameters, wherein setting activation threshold value (Trigger threshold) is 1.5 volts, Z direction rising size is 1.608 microns, and sweep velocity is 0.9965 hertz, and the X-axis scanning angle is 22 degree, begin to carry out nano impress and measure, press down at needle point as can be seen from semi-girder deformation-displacement curve that film surface has deformation the process;
(8) by changing activation threshold value (Trigger threshold), regulate the size that puts on the power on the nano impress needle point (1), and the semi-girder deformation-displacement curve (see figure 2) of record nano impress needle point (1) in being pressed into minitype particle sample (2) surface film coating process.
The thin film coating of minitype particle sample (2) material surface in the above-mentioned said step (1) is that the method by magnetron sputtering obtains, change different magnetron sputtering growth conditionss, the film thickness difference of minitype particle material surface, corresponding change can take place in the homogeneous degree that can observe film from the atomic force microscope images, and the force-displacement curve from the nano impress experiment can observe the change of property of thin film.
Embodiment 2: a kind of measurement mechanism (see figure 1) of the minitype particle nano surface impression based on atomic force microscope, it is to be made of the atomic force microscope system, comprise scanning monitor, the scanning probe microscopy main body, the magnifier display system, main frame, display, keyboard and mouse, wherein the scanning probe microscopy main body comprises pedestal, scanatron, the needle point frame, the electronic circuit linkage unit, laser optical path and Zoom lens system, it is characterized in that on the sample stage at scanatron top the sheet plane (3) of laying sample (2) being arranged, the double faced adhesive tape that the sample that is adhesively fixed (2) are arranged on the sheet plane (3), among being fixed in the needle point frame nano impress needle point (1) that scans with the nano impress operation is arranged, nano impress needle point (1) places the top of sample (2).
What above-mentioned said nano impress needle point (1) adopted is the adamas needle point, and the elasticity coefficient of nano impress needle point (1) remains between 100-300 ox/rice, and resonant frequency is the 35-65 KHz.
Above-mentioned said atomic force microscope system is the NanoscopeIV type equipment of U.S. VEECO company.
The adamas needle point that above-mentioned said nano impress needle point (1) is adopted is the DNISP adamas needle point that is used for nano impress/nanometer scratch experiment that U.S. VEECO company provides.
Above-mentioned said sheet plane (3) of laying sample (2) is an iron plate.
A kind of measuring method of above-mentioned minitype particle nano surface impression based on atomic force microscope is characterized in that it has following steps:
(1) take a morsel Powdered minitype particle with micro-meter scale magnitude is made sample (2) and is sticked at gently on the sheet plane (3) that is fixed with double faced adhesive tape, with ear washing bulb sticking the unstable Powdered minitype particle that blows off, in order to avoid influence measuring process, cause the inserting needle difficulty, the sheet plane (3) that will be stained with sample (2) then is positioned on the sample stage at scanatron top of scanning probe microscopy gently;
(2) with special-purpose needle point tweezers nano impress needle point (1) is put on the needle point frame, then the needle point frame is fixed on the sample stage top at scanatron top;
(3) the focusing situation of watching from the magnifier display sample surfaces by the focal position of regulating magnifier concentrates on focus point the upper surface of some minitype particle samples (2);
(4) utilize the thick inserting needle system of atomic force microscope nano impress needle point (1) progressively to be approached the upper surface of minitype particle sample (2), when the position of the roughly imaging that on the magnifier display, can watch nano impress needle point (1), stop pin down at once, prevent to bump against particle surface;
(5) select the nano impress functional module on computers, open the interface after, select pin icon down, allow the automatic inserting needle of needle point to minitype particle sample (2) surface;
(6) when nano impress needle point (1) reaches minitype particle sample (2) surface, begin to carry out the scanning process of sample surfaces pattern, regulate sweep parameter, obtain the clear feature image of sample surfaces;
(7) treat selected carry out position that nano impress measures after, enter the nano impress pattern, regulate relevant parameters, wherein setting activation threshold value (Trigger threshold) is 2.5 volts, Z direction rising size is increased to 3.147 microns, and sweep velocity is 0.9965 hertz, and the X-axis scanning angle is 22 degree.After strengthening activation threshold value (Trigger threshold) as can be seen and also promptly increase the power impose on the needle point from semi-girder deformation-displacement curve, variation has taken place in the shape of curve;
(8) by changing activation threshold value (Trigger threshold), regulate the size that puts on the power on the nano impress needle point (1), and the semi-girder deformation-displacement curve (see figure 3) of record nano impress needle point (1) in being pressed into minitype particle sample (2) surface film coating process.
The thin film coating of minitype particle sample (2) material surface in the above-mentioned said step (1) is that the method by magnetron sputtering obtains, change different magnetron sputtering growth conditionss, the film thickness difference of minitype particle material surface, corresponding change can take place in the homogeneous degree that can observe film from the atomic force microscope images, and the force-displacement curve from the nano impress experiment can observe the change of property of thin film.
Claims (9)
1. measurement mechanism based on the minitype particle nano surface impression of atomic force microscope, it is to be made of the atomic force microscope system, comprise scanning monitor, the scanning probe microscopy main body, the magnifier display system, main frame, display, keyboard and mouse, wherein the scanning probe microscopy main body comprises pedestal, scanatron, the needle point frame, the electronic circuit linkage unit, laser optical path and Zoom lens system, it is characterized in that on the sample stage at scanatron top the sheet plane (3) of laying sample (2) being arranged, the double faced adhesive tape that the sample that is adhesively fixed (2) are arranged on the sheet plane (3), among being fixed in the needle point frame nano impress needle point (1) that scans with the nano impress operation is arranged, nano impress needle point (1) places the top of sample (2).
2. according to the measurement mechanism of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 1, what it is characterized in that said nano impress needle point (1) employing is the adamas needle point, the elasticity coefficient of nano impress needle point (1) remains between 100-300 ox/rice, and resonant frequency is the 35-65 KHz.
3. according to the measurement mechanism of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 1, it is characterized in that said atomic force microscope system is the Nanoscope IV type equipment of U.S. VEECO company.
4. according to the measurement mechanism of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 2, it is characterized in that the adamas needle point that said nano impress needle point (1) is adopted is the DNISP adamas needle point that is used for nano impress/nanometer scratch experiment that U.S. VEECO company provides.
5. according to the measurement mechanism of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 1, it is characterized in that said sheet plane (3) of laying sample (2) is an iron plate.
6. the measuring method of an above-mentioned minitype particle nano surface impression based on atomic force microscope is characterized in that it has following steps:
(1) take a morsel Powdered minitype particle with micro-meter scale magnitude is made sample (2) and is sticked at gently on the sheet plane (3) that is fixed with double faced adhesive tape, with ear washing bulb sticking the unstable Powdered minitype particle that blows off, in order to avoid influence measuring process, cause the inserting needle difficulty, the sheet plane (3) that will be stained with sample (2) then is positioned on the sample stage at scanatron top of scanning probe microscopy gently;
(2) with special-purpose needle point tweezers nano impress needle point (1) is put on the needle point frame, then the needle point frame is fixed on the sample stage top at scanatron top;
(3) the focusing situation of watching from the magnifier display sample surfaces by the focal position of regulating magnifier concentrates on focus point the upper surface of some minitype particle samples (2);
(4) utilize the thick inserting needle system of atomic force microscope nano impress needle point (1) progressively to be approached the upper surface of minitype particle sample (2), when the position of the roughly imaging that on the magnifier display, can watch nano impress needle point (1), stop pin down at once, prevent to bump against particle surface;
(5) select the nano impress functional module on computers, open the interface after, select pin icon down, allow the automatic inserting needle of needle point to minitype particle sample (2) surface;
(6) when nano impress needle point (1) reaches minitype particle sample (2) surface, begin to carry out the scanning process of sample surfaces pattern, regulate sweep parameter, obtain the clear feature image of sample surfaces;
(7) treat selected carry out position that nano impress measures after, enter the nano impress pattern, regulate relevant parameters, wherein the size of activation threshold value (Trigger threshold) is 0 volt-10 volts, the Z direction raises and to be of a size of 500 nanometers-3.5 micron, sweep velocity is 0.5 hertz-2 hertz, and the X-axis scanning angle is 0 degree-30 degree, begins to carry out nano impress and measures;
(8) by changing activation threshold value (Trigger threshold), regulate the size that puts on the power on the nano impress needle point (1), and the semi-girder deformation-displacement curve of record nano impress needle point (1) in being pressed into minitype particle sample (2) surface film coating process.
7. according to the measuring method of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 6, the thin film coating that it is characterized in that minitype particle sample (2) material surface in the said step (1) is that the method by magnetron sputtering obtains, change different magnetron sputtering growth conditionss, the film thickness difference of minitype particle material surface, corresponding change can take place in the homogeneous degree that can observe film from the atomic force microscope images, and the force-displacement curve from the nano impress experiment can observe the change of property of thin film.
8. according to the measuring method of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 6, after it is characterized in that said step (7) is waited to select the position of carrying out the nano impress measurement, enter the nano impress pattern, regulate relevant parameters, wherein setting activation threshold value (Triggerthreshold) is 1.5 volts, Z direction rising size is 1.608 microns, sweep velocity is 0.9965 hertz, the X-axis scanning angle is 22 degree, begin to carry out nano impress and measure, press down at needle point as can be seen from semi-girder deformation-displacement curve that film surface has deformation the process.
9. according to the measuring method of the said a kind of minitype particle nano surface impression based on atomic force microscope of claim 6, after it is characterized in that said step (7) is waited to select the position of carrying out the nano impress measurement, enter the nano impress pattern, regulate relevant parameters, wherein setting activation threshold value (Triggerthreshold) is 2.5 volts, Z direction rising size is increased to 3.147 microns, and sweep velocity is 0.9965 hertz, and the X-axis scanning angle is 22 degree.After strengthening activation threshold value (Trigger threshold) as can be seen and also promptly increase the power impose on the needle point from semi-girder deformation-displacement curve, variation has taken place in the shape of curve.
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Application publication date: 20110928 |