CN108445260B - Multiband sample irradiation system based on atomic force microscope - Google Patents
Multiband sample irradiation system based on atomic force microscope Download PDFInfo
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- CN108445260B CN108445260B CN201810316260.8A CN201810316260A CN108445260B CN 108445260 B CN108445260 B CN 108445260B CN 201810316260 A CN201810316260 A CN 201810316260A CN 108445260 B CN108445260 B CN 108445260B
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- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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Abstract
The invention discloses a multiband sample irradiation system based on an atomic force microscope. The device system mainly comprises an irradiation device, an external light source and an optical fiber, wherein the irradiation device comprises a shell, a point light source, a lens and a light shield, when the device system is used, the irradiation device is partially matched with an atomic force microscope and is arranged below an objective table, the external light source emits incident light beams with specific wave bands, the light beams are transmitted to the point light source inside the irradiation device through the optical fiber and upwards spread in a point shape, and divergent light is constrained by the lens to be parallel light to irradiate the surface of a material sample. The device system is independent of a laser system of the atomic force microscope and does not interfere with the laser system, the irradiation wave band is adjusted by adopting different external light sources or adding light filters, and the real-time detection of various performance indexes such as sample force, electricity, magnetism, heat and the like is realized by changing the mode of an atomic force microscope scanning probe module and a software scheme.
Description
Technical Field
The invention belongs to the technical field of testing surface appearance and force, electricity, magnetism and thermal properties of materials, and particularly relates to a multiband sample irradiation device based on an atomic force microscope.
Background
The surface appearance and the force, electric, magnetic and thermal properties of the material under irradiation at different wave bands can be changed to different degrees. Specifically, when the high molecular material is irradiated in an ultraviolet band (100-400nm), because the energy of the short wavelength of the ultraviolet light is concentrated, the covalent bond in the molecular chain segment can be broken, so that the molecular weight of the material is reduced, and the surface erosion and the mechanical property of the material are reduced; photovoltaic Materials show different electromagnetic properties under visible light (400-; in addition, some studies such as the Journal of biomedical optics (Journal of biomedical optics,2000,5(4):383-391) report the effect of near infrared radiation with wavelengths longer than 760nm on the thermal conductivity of biological tissue materials.
The atomic force microscope can obtain the surface appearance and basic mechanical characteristic information of the sample by analyzing the interaction force between the probe tip and the surface of the detected sample. In addition, the special probe can be combined to obtain the relevant performance parameters of the surface electricity, magnetism, heat and the like of the material sample. Compared with a scanning electron microscope, the method has the advantages of high resolution, wide applicable sample range, multiple detection indexes and the like, and is suitable for detecting and analyzing related performance changes of sample materials under irradiation conditions.
At present, for the research on the relevant characteristics of sample materials under the irradiation condition, such as reports of RSC Advances journal (RSC Advances 7.1(2017): 112) 120) and Chinese patent CN102721601A, etc., the method of irradiation first and then analysis is adopted. The method can not analyze the surface performance index change of the sample in real time in the irradiation process, and can not ensure that the related performance of the irradiated sample is not changed in the storage and test stages, thereby limiting the accuracy of analysis. Therefore, there is a need to develop a device for irradiating a material sample in situ in an atomic force microscope and testing the change of the related performance index in real time.
Disclosure of Invention
The invention aims to provide a multiband sample irradiation device based on an atomic force microscope.
The purpose of the invention is realized by the following steps: a method for measuring surface force, electric, magnetic and thermal properties of a sample material under a specific wave band light irradiation condition in real time based on an atomic force microscope comprises the following steps:
(1) firstly, mounting an irradiation device below a sample table of an atomic force microscope, and connecting the irradiation device and an external light source by using an optical fiber;
(2) scanning an original sample material under a non-irradiation condition by using an atomic force microscope to obtain related performance data of the material under the non-irradiation condition;
(3) using an external light source with a specific wave band to generate incident beams, introducing the beams into a light irradiation device through an optical fiber and irradiating a sample to be detected in the form of parallel light, and continuously scanning the sample by using an atomic force microscope to obtain real-time data of the related performance of the surface of the material sample under the irradiation of the wave band;
(4) selecting a plurality of time points from the real-time data, and analyzing and comparing the change condition of the relevant performance of each time point of the material sample under the irradiation of the wave band;
(5) changing the wave band of the irradiation light beam by changing an external light source or a filter lens, and repeating the steps (3) and (4) to obtain the influence of ultraviolet, visible light and infrared wave band irradiation on the relevant performance of the material sample;
(6) and (3) repeating the steps (2), (3) and (4) by changing the mode of scanning the probe module and the software scheme of the atomic force microscope, so as to realize the real-time detection of the surface morphology of the sample and the multiple performance indexes of force, electricity, magnetism, heat and the like.
The irradiation of the sample material by the light beams with different wave bands such as an ultraviolet wave band (100-.
The real-time detection of the force, electricity, magnetism and heat multiple performance indexes such as the surface appearance, the elastic modulus, the material phase, the resistance, the piezoelectric power, the magnetic force, the heat conduction and the like of the sample is realized by changing the atomic force microscope scanning probe module and the software scheme.
The light beam with specific wave band is fed into the light irradiation device by means of optical fibre, and the parallel light beam with certain size light spot formed by lens in the light irradiation device is irradiated on the bottom surface of sample material on the atomic force microscope stage.
The adjustment of the size of the irradiation light spot on the surface of the material to be measured is realized by adjusting the focal length of the lens.
The invention has the following beneficial effects:
(1) the invention can utilize the atomic force microscope to carry out real-time test on various performance indexes of the material sample such as force, electricity, magnetism, thermal property and the like while irradiating the sample, compared with the prior technology of 'irradiation first and test later', the real-time test can more accurately reflect the change condition of the relevant performance of the material in the irradiation process, and simultaneously avoid the result error caused by sample storage and subsequent test;
(2) the invention realizes the adjustment of the irradiation wave band by replacing the external light source or the optical filter, and has the advantages of wide wave band range, adjustable power and strong flexibility;
(3) the incident beam is adjusted by the light irradiation device to irradiate the sample from the bottom in a parallel light mode, so that the interference of the irradiation beam on the atomic force microscope self-contained laser detection system is avoided;
(4) the irradiation light spot can be adjusted, and the effect of adjusting the power density of the irradiation light beam on the surface of the material can be realized.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention.
FIG. 2 is a flow chart of a method for detecting the performance index of a sample in real time under a specific wave band irradiation condition by using the method.
FIG. 3 is a flow chart of a method for detecting the performance index of a sample in real time under different wave band irradiation conditions by using the invention.
FIG. 4 is a flow chart of a method for detecting different performance indexes of a sample in real time under a specific wave band irradiation condition by using the method.
FIG. 5 is a schematic view of irradiation spot adjustment according to the present invention
Detailed Description
Example 1:
in example 1, the process of the method for measuring the surface morphology and the elastic modulus change of the polylactic acid film under 355nm ultraviolet band irradiation for 5 minutes is shown in fig. 2, and specifically includes the following steps:
(1) as shown in FIG. 1, the light irradiation apparatus 3 was connected to an atomic force microscope 9 as shown in the figure, and a 2X 2cm polylactic acid film 8 was fixed to a microscope stage 7. An external light source 1 emits 355nm ultraviolet light, the ultraviolet light is transmitted into a light emitting head 4 through an optical fiber 2, light beams are upwards diffused in a point shape and constrained to be parallel light through a lens 5;
(2) the atomic force microscope was set to contact mode, the polylactic acid film was continuously scanned using a conventional probe, and the light shield 6 was opened to start the experiment until 5 minutes of irradiation. The surface appearance and elastic modulus distribution diagram of a plurality of continuous polylactic acid films are obtained through software synthesis analysis;
(3) and selecting surface morphology and elastic modulus distribution maps of the polylactic acid film at 6 time points of 0 minute, 1 minute, 2 minutes, 3 minutes, 4 minutes, 5 minutes and the like from the obtained data, and comparing and analyzing the continuous change conditions of the surface morphology and the elastic modulus of the polylactic acid film for 5 minutes under 355nm ultraviolet irradiation.
Example 2:
in embodiment 2, the process of measuring the surface morphology and the elastic modulus change of the polylactic acid film in the 488nm, 546nm and 800nm wave band irradiation for 5 minutes is shown in fig. 3, and specifically includes the following steps:
(1) as shown in FIG. 1, a 2X 2cm polylactic acid film (note: group A1) was fixed to a microscope stage by attaching a light irradiation apparatus to an atomic force microscope as shown in the figure. Connecting a visible light external light source and adjusting the filter to emit 488nm visible light, transmitting the visible light into the light emitting head through the optical fiber, upwardly spreading the light beam in a point shape, and constraining the light beam in parallel light through the lens;
(2) the atomic force microscope was set to contact mode and the polylactic acid film was continuously scanned using a conventional probe until 5 minutes of irradiation. Through software synthesis analysis, a plurality of continuous A1 groups of polylactic acid film surface morphology and elastic modulus distribution maps are obtained;
(3) changing the polylactic acid film sample (record A2 group) of the parallel group of the object stage, and adjusting an external light source filter to enable the external light source filter to emit 546nm visible light;
(4) the atomic force microscope was set to contact mode, the polylactic acid film was continuously scanned using a conventional probe, and the light shield was opened to start the experiment until 5 minutes of irradiation. Through software synthesis analysis, a plurality of continuous A2 groups of polylactic acid film surface morphology and elastic modulus distribution maps are obtained;
(5) replacing the polylactic acid film sample (recorded as A3 group) in the parallel group of the object stage, and replacing an external light source to enable the sample to emit 800nm near-infrared light waves;
(6) the atomic force microscope was set to contact mode, the polylactic acid film was continuously scanned using a conventional probe, and the light shield was opened to start the experiment until 5 minutes of irradiation. Through software synthesis analysis, a plurality of continuous A3 groups of polylactic acid film surface morphology and elastic modulus distribution maps are obtained;
(7) and selecting the surface morphology and the elastic modulus distribution map of the polylactic acid film at a specific time point from the obtained group data of A1, A2 and A3, and comparing and analyzing the differences of the surface morphology and the elastic modulus of the polylactic acid film for 5 minutes under the irradiation of three different wave bands of 488nm, 546nm and 800 nm.
Example 3:
in embodiment 3, a flow chart of the method for measuring real-time changes of the surface morphology, the resistance and the thermal resistance of the monocrystalline silicon film in 5 minutes under 488nm wave band irradiation is shown in fig. 4, and the method specifically includes the following steps:
(1) as shown in FIG. 1, the light irradiation apparatus was connected to the atomic force microscope as shown in the figure, and a 2X 2cm single-crystal silicon thin film (note as group B1) was fixed to the stage of the microscope. Connecting a visible light external light source and adjusting the filter to emit 488nm visible light, transmitting the visible light into the light emitting head through the optical fiber, upwardly spreading the light beam in a point shape, and constraining the light beam in parallel light through the lens;
(2) the atomic force microscope was set to contact mode and the single crystal silicon thin film was continuously scanned using a conventional probe until 5 minutes of irradiation. Through software synthesis analysis, a plurality of continuous B1 groups of monocrystalline silicon thin film surface morphology and elastic modulus distribution maps are obtained;
(3) changing the monocrystalline silicon film samples of the parallel group of the object stage (record B2 group);
(4) the atomic force microscope was set to contact mode, the monocrystalline silicon thin film was continuously scanned using the conductive probe module, and the light shield was opened to start the experiment until 5 minutes of irradiation. Through software synthesis analysis, a plurality of continuous B2 groups of monocrystalline silicon thin film resistance distribution maps are obtained;
(5) changing the monocrystalline silicon film samples of the parallel group of the object stage (record B3 group);
(6) the atomic force microscope was set to the contact mode, the monocrystalline silicon thin film was continuously scanned using the thermal analysis module, and the light shield was opened to start the experiment until 5 minutes of irradiation. Through software synthesis analysis, a plurality of continuous B3 groups of monocrystalline silicon thin film surface thermal resistance distribution maps are obtained;
(7) and selecting the surface morphology, the resistance and the thermal resistance distribution diagram of the monocrystalline silicon film at a specific time point from the obtained group of data B1, B2 and B3, and comparing and analyzing the differences of the surface morphology, the resistance and the thermal resistance of the monocrystalline silicon film for 5 minutes under 488nm wave band irradiation.
Claims (3)
1. A multiband sample irradiation system based on an atomic force microscope is characterized in that: the irradiation system comprises an irradiation device, an external light source and an optical fiber; the irradiation device is arranged below the sample stage of the atomic force microscope and consists of a shell, a point light source, a lens and a light shield, wherein light beams emitted by the point light source are refracted into parallel light through the lens and are used for irradiating a sample to be measured; the external light source is arranged beside the atomic force microscope, incident light beams are transmitted into the irradiation device through the optical fiber, and the incident light beams with different ultraviolet, visible light and infrared wave bands can be obtained by replacing the external light source and adopting a filter; the light beam with specific wave band enters the light irradiation device through the optical fiber, and the lens in the light irradiation device forms a parallel light beam with certain size of light spot to irradiate on the bottom surface of the sample material on the atomic force microscope objective table; the adjustment of the size of the irradiation light spot on the surface of the material to be detected is realized by adjusting the focal length of the lens, and the adjustment of the power density of the irradiation light beam on the surface of the material can be realized; the device can realize the real-time test of the relative force, the electric property, the magnetic property and the thermal property of the surface of the tested sample by using the atomic force microscope while irradiating the sample material.
2. The multiband sample irradiation system based on atomic force microscope as claimed in claim 1, wherein irradiation of sample material by ultraviolet band, visible band and infrared band different band light beams is realized by replacing external light source or adopting different optical filter.
3. The multiband sample irradiation system based on atomic force microscope as claimed in claim 1, wherein the incident beam is adjusted by the light irradiation device to irradiate the sample from the bottom of the microscope sample stage in the form of parallel light, avoiding the interference of the irradiation beam to the own laser detection system of the atomic force microscope.
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| JPH0612907U (en) * | 1992-07-15 | 1994-02-18 | オリンパス光学工業株式会社 | Scanning tunneling microscope and its sample stage |
| JP3093145B2 (en) * | 1995-12-13 | 2000-10-03 | 科学技術振興事業団 | Light irradiation switching method |
| EP1116932A3 (en) * | 2000-01-14 | 2003-04-16 | Leica Microsystems Wetzlar GmbH | Measuring apparatus and method for measuring structures on a substrat |
| US20070196815A1 (en) * | 2000-08-02 | 2007-08-23 | Jason Lappe | Positive Selection Procedure for Optically Directed Selection of Cells |
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