JP6330212B2 - Heating method of micro sample - Google Patents

Description

The present invention relates to heating of how to precisely measure the micro-sample.

  The present invention relates to a heating method and a heating unit for heating and keeping a sample portion containing a sample of about several tens of μl such as a micro liquid with stability of ± 0.05 ° C. or less and performing precision measurement such as resonance shear measurement. Is.

  The inventor of the present application has proposed a precision shear measurement method and apparatus (see Patent Documents 1 and 2 below).

  At present, measurement methods for small samples of several tens of μl, such as surface force measurement and resonance shear measurement, have become important as nanoscience progresses. Therefore, a heating unit that can heat only a minute sample portion with high accuracy and stability is desired.

  For example, the resonance shear measurement unit can measure the viscosity and lubricity of a liquid sandwiched between two substrates while controlling the distance between the substrates with nanometers, and is an important measurement for nanorheology and nanotribology. Taking a study of lubricating oil as an example, the temperature of lubricating oil in an actual automobile engine may be close to 100 ° C., and measurement at a high temperature as well as at room temperature is desired.

Japanese Patent No. 3032152 Japanese Patent No. 4615568

Liquid crystal, 6 (1), p. p34-41 (2002) J. et al. Chem. Soc. Faraday Trans. 1, 1986, 82, p. p2715-2746 S. H. J. et al. Idziak, I.I. Koltover, J. et al. N. Israelachvili, and C.I. R. Safinya, Phys, Rev. Lett. 76, 1477 (1996) E. Perret, K.M. Nygard, D .; K. Satapathy, T .; E. Balmer, O.M. Bunk, M.M. Heuberger and J.H. F. van der Veen, Europhys. Lett. , 88, 36004, (2009) D. Fukushi, M .; Kasuya, H .; Sakuma, K .; Kurihara, Chem. Lett. 40,776 (2011) Y. Saito, M .; Kasuya, K .; Kurihara, Chem. Lett. 41, 1282 (2012)

  When a conventional rubber heater or other normal heater is incorporated into the apparatus (see Non-Patent Document 1 above), it is heated extensively in order to change the temperature, and a drift in distance occurs. Moreover, although the measurement which makes room temperature change and equilibrate is also made, the temperature range is narrow [refer the said nonpatent literature 2]. Therefore, a temperature dependent measurement requires a compact system that can locally heat only the sample part and that can be heated while corresponding to the shape of the measurement part.

An object of this invention is to provide the heating method of the micro sample which can heat the micro liquid pinched | interposed between the board | substrates of arbitrary shapes efficiently and with high precision.

In order to solve the above-described problems of the prior art and achieve the above-described object, a heating method for a micro sample according to the present invention includes a sample unit composed of two substrates sandwiching a liquid sample, and surrounds the sample unit. And a heating unit arranged.

The present invention is, in view of the above circumstances, it is an object to provide a heating how the micro sample capable of heating the micro sample sandwiched between the substrates of any shape to efficiently accurate it can.

In order to achieve the above object, the present invention provides
[1] Two or more opposing heating systems surrounding a micro sample sandwiched between two substrates are used, a substantially arc-shaped infrared heater is used for heating, and the heat rays emitted from the infrared heater are placed on the opposite side of the micro sample. In the method of heating a micro sample that is condensed by a half-moon shaped mirror and heats the sample portion, the micro sample sandwiched between the infrared heater and the substrate is placed in a container to insulate, and the container is micro It is characterized by being divided into two or more for exchanging the sample and driving the sample part.

  [2] The method for heating a micro sample according to [1], wherein the micro sample is liquid or solid.

  [3] In the heating method of the micro sample according to [1], the temperature of the sample part is controlled by observing the temperature of the heating part and the sample part, determining a desired set temperature, and controlling the temperature of the heating part by a feedback circuit. The amount of current applied to the infrared heater is controlled to be kept constant at a desired temperature within 0.1 degree.

  [4] In the heating method of the micro sample according to [1], the heating system includes a box-shaped container for entering observation light in a direction perpendicular to the substrate, and the substrate is perpendicular to the substrate. It is connected to an external drive system that moves up and down via a spring for measuring force.

  According to the present invention, it is possible to efficiently heat a minute sample sandwiched between substrates having an arbitrary shape with high accuracy.

It is a schematic diagram which shows an example of the resonance shear measurement unit with a heating unit which shows the Example of this invention. FIG. 2 is a plan view of a heating unit located in the vicinity of an upper substrate and a lower substrate shown in FIG. 1. It is explanatory drawing of the operation example of the heating unit of this invention. It is explanatory drawing of the heater wire | line used as a heating unit of this invention. It is a block diagram of the side direction of the heating unit which concerns on this invention. It is a schematic diagram of constant temperature control using the heating unit of the Example of this invention. It is a figure which shows the measurement result (the 1) of the temperature of a heater and a board | substrate when a board | substrate is set to the heating unit which concerns on this invention, and it heats. It is a figure which shows the measurement result (the 2) of the temperature of a heater and a board | substrate at the time of setting and heating a board | substrate to the heating unit which concerns on this invention, and is an enlarged view of the part of FIG.7 (b). It is a figure which shows the measurement result (the 3) of the temperature of a heater and a board | substrate at the time of setting and heating a board | substrate to the heating unit which concerns on this invention, and is an enlarged view of the part of FIG.7 (c). It is a figure which shows the drift of the distance by the heating unit of this invention. It is a block diagram of the X-ray-diffraction apparatus with a heating unit which shows the other Example of this invention. It is an enlarged view of the X-ray-diffraction apparatus of FIG. It is a schematic diagram of a surface force / fluorescence combined measuring apparatus with a heating unit showing still another embodiment of the present invention.

  The method for heating a micro sample of the present invention uses two or more opposing heating units surrounding a micro sample sandwiched between two fixed substrates, uses a substantially arc-shaped infrared heater for heating, and exits from this infrared heater. A heat ray is condensed by a half moon-like mirror on the opposite side of the minute sample, and the sample portion is heated.

  Hereinafter, embodiments of the present invention will be described in detail.

  First, the necessity of heating a micro liquid by surface force measurement / resonance shear measurement and the prior art will be described.

  The surface force measurement is a measurement for obtaining an interaction force acting between two surfaces as a function of distance. When a surface force measuring device (SFA) is used, it can be measured with a distance resolution of 0.1 nm and a force resolution of 10 nN.

  The resonance shear measurement is a measurement in which a change in liquid properties (viscosity, elasticity, structuring, lubricity, etc.) between two surfaces is evaluated by changing the distance at the nanometer level. The change in properties of liquid confined in nanospace can be evaluated.

  It is important from the evaluation of basic physical properties and material functions to obtain temperature dependence such as interaction and liquid characteristics by performing these measurements at different temperatures. Further, in the evaluation of lubricating oil and the like, measurement under use conditions is necessary. For example, a phase change of liquid crystal or surfactant solution, typical operating temperature of automobile engine lubricant (~ 90 ° C), hard disk drive (usually operating at 45-60 ° C), and equipment that can measure up to high temperature is required It becomes.

  However, the conventional method has been performed only up to about 40 ° C., and it has been difficult to greatly change the temperature. Also, the temperature is changed by changing the room temperature or a rubber heater is used. However, the range of change is limited in the former, and the latter has a problem in that the heated portion is large and the distance drifts.

  In the present invention, as problem 1, thermal expansion due to heat transfer to the surroundings and distance fluctuation are eliminated.

  As a solution to this, heating is performed with as little heat as possible. The temperature of the sample was measured, calibration curve data with the heater temperature was created, and a closed-loop control system was established to control the sample temperature with the minimum amount of heat by controlling the heater temperature.

  In the present invention, as a second problem, with regard to local heating of the sample portion by infrared condensing heating, optimization of condensing and reduction of heat transfer are attempted by developing a thin tube infrared lamp and using a mirror.

  FIG. 1 is a schematic diagram showing an example of a resonance shear measuring unit with a heating unit according to the present invention.

  In this figure, 3 is a heater (light source), 10 is a resonance shear measurement unit, 11 is a vertical force measurement cantilever, 12 and 13 are disk holders, 14 is a lower disk substrate fixed on the lower disk holder 12, and 15 is A four-divided piezo element as a horizontal drive unit for driving the upper surface in the horizontal direction, 16 is an upper disk substrate fixed to the disk holder 13 at the bottom of the four-divided piezo element 15, and 17 supports the four-divided piezo element 15. A leaf spring, 18 is an electric cable for applying a voltage for driving the four-divided piezo element 15, 19 is a micro sample (solid, liquid, liquid crystal, etc.) to be measured for shear response, 20 is a capacitance meter, and 21 is a capacitance meter. A heating part thermocouple for monitoring the temperature (Th) of the heating part, 22 is a sample part thermocouple for monitoring the temperature (Ts) of the sample part, and 23 is heating part heat. Electrical cable leading to the pair 21, 24 is an electric cable that runs to the sample unit thermocouple 22. Here, only the sample part is heated by the infrared condensing by the heater (light source) 3. Thus, the precision temperature control SFA is configured. Here, the liquid may be not only a single component but also various solutions including two or more micelles and a colloidal dispersion system. In addition, you may make it use a motor as said horizontal drive part. Further, the substrate itself is used as a sample, and the mutual friction (lubrication) characteristics of the sample (lower disk substrate) 14 and the sample (upper disk substrate) 16 are measured without sandwiching the sample between the substrates as shown in FIG. You can also.

  In the heating unit for the micro sample of the present invention, a first heating unit 71 provided in the vicinity of one side of the micro sample 19 and provided with a substantially semicircular cylindrical portion, and on the other side of the micro sample 19 And a second heating unit 72 provided with a substantially semicircular arc-shaped cylindrical portion, and the first heating unit 71 and the second heating unit 72 are made as close as possible to each other. Before the micro sample 19 is held between the first posture (FIG. 2) and the upper surface holding body and the lower surface holding body, the micro sample 19 is positioned at a distance that can be exchanged. The second posture (FIG. 3) can be selected.

  Other shapes are possible as long as the sample 19 fits into the sample section.

  In the heating unit of the present invention, the first heating unit 71 and the second heating unit 72 are joined at one end thereof, and the heating of the first heating unit 71 and the second heating unit 72 is performed. The part (heater) is wound in a coil shape in the cylindrical part, and at least one electric wire that is a stranded wire in the other part constitutes the electric wire of the heating unit of the first heating unit 71 and the second heating unit 72 doing.

  The cylindrical part of the heating unit of the present invention is a glass tube of a resonance shear measuring device, and the electric wire is interposed between the cylindrical part of the first heating unit 71 and the cylindrical part of the second heating unit 72. Is provided with a flexible heat-resistant covering member.

  As shown in FIG. 6, the temperature (Th) of the heating part and the temperature (Ts) of the sample part are monitored by thermocouples. The relationship between Ts and Th is obtained in advance, and Th is optimized to the obtained Ts. The temperature Th of the heating part is feedback controlled by the control circuit to heat the sample part and maintain the temperature Ts at a desired constant temperature.

  According to the heating unit of the present invention, it is possible to provide a heating unit that can efficiently heat a minute sample sandwiched between substrates having an arbitrary shape with high accuracy.

  Hereinafter, the heating unit 61 that heats the minute sample 19 sandwiched between the lower disk substrate 14 and the upper disk substrate 16 will be described in detail.

  FIG. 2 is a plan view for explaining a heating unit located near the upper disk substrate and the lower disk substrate shown in FIG. FIG. 3 is an explanatory diagram of an operation example of the heating unit of the present invention, and FIG. 4 is an explanatory diagram of a heater wire used as the heating unit of the present invention. FIG. 5 is a configuration diagram of the heating unit in the side surface direction.

  As shown in FIGS. 1 and 2, a heating unit 61 is disposed in the vicinity of the upper disk substrate 16 and the lower disk substrate 14.

  As shown in FIG. 2, the heating unit 61 includes the plate 80 of the first heating unit 71 and the second heating unit in a state where the micro sample 19 is sandwiched between the lower disk substrate 14 and the upper disk substrate 16. 72 in which the plate 90 is joined, that is, the substantially arcuate glass tubes 53 and 93 are closest to the micro sample 19.

As shown in FIG. 2, the 1st heating unit 71 has the substantially circular arc-shaped glass tube 53 and the linear glass tubes 54 and 56 located in the both ends. A substantially circular arc-shaped glass tube 53, the lower half of the portion of the glass tube 53 side of the straight glass tube 54 is accommodated in a recess formed in the plate 80.

  One end of a flexible cylindrical member 83 is attached to one end of the glass tube 54 opposite to the glass tube 53 side. One end of a flexible cylindrical member 81 is attached to one end of the glass tube 56 opposite to the glass tube 53 side.

  As shown in FIG. 2, the second heating unit 72 includes a substantially arcuate glass tube 93 and linear glass tubes 94 and 96 located at both ends thereof. The substantially arcuate glass tube 93 and the lower half of the glass tubes 94, 96 on the glass tube 93 side are accommodated in a recess formed in the plate 90.

  The other end of the cylindrical member 83 is attached to one end of the glass tube 94 opposite to the glass tube 93 side. One end of a flexible cylindrical member 91 is attached to one end of the glass tube 96 opposite to the glass tube 93 side.

  The cylindrical member 81, the glass tubes 56, 53, 54, the cylindrical member 83, the glass tubes 94, 93, 96, and the cylindrical member 91 accommodate one heater wire 100 shown in FIG.

  As shown in FIG. 4, the heater wire 100 includes, for example, a stranded wire 101, a joint portion 102, a heating wire 103, a stranded wire 104, a heating wire 105, a joining portion 106, and a stranded wire 107.

  The stranded wire 101 is accommodated in the cylindrical member 81 shown in FIG. 2 and is fixed to the vicinity of the opening inside the glass tube 56 by the joint portion 102. The stranded wire 101 is heat-resistant coated.

  The heating wire 103 has a coil shape and is accommodated in the substantially arc-shaped glass tube 53.

  One end of the stranded wire 104 is fixed near the opening inside the glass tube 54. Most of the stranded wire 104 is accommodated in the cylindrical member 83.

  The other end of the stranded wire 104 is fixed in the vicinity of the opening inside the glass tube 94. The stranded wire 104 is heat-resistant coated.

  The heating wire 105 has a coil shape and is accommodated in a substantially arc-shaped glass tube 93.

  The stranded wire 107 is accommodated in the cylindrical member 91 and is fixed to the vicinity of the opening inside the glass tube 96 by the joining portion 106. The stranded wire 107 is heat-resistant coated.

  As shown in FIG. 5, a plate 180 is provided on the upper side of the plate 80 so as to sandwich glass tubes 56, 53, and 54 (see FIG. 2) between the plate 80. The plate 180 has a shape symmetrical to the plate 80, and is provided with a recess for receiving the glass tubes 56, 53, and 54 (see FIG. 2).

  A plate 190 is provided on the upper side of the plate 90 so as to sandwich the glass tubes 96, 93, 94 between the plate 90. The plate 190 has a shape symmetrical to the plate 90 and is provided with a recess for accommodating the glass tubes 96, 93, 94.

  Here, the concave portions of the plates 80, 180, 90, and 190 are shaped and mirror-finished so as to be focused on the sample portion. It can be replaced with an equivalent mirror.

  The plate 80 and the plate 90 can be moved in the direction of the arrow in FIG. 2 by driving means (not shown). In conjunction with the movement of the plate 80, the glass tubes 56, 53, 54 and the plate 180 also move. In conjunction with the movement of the plate 90, the glass tubes 96, 93, 94 and the plate 190 also move.

  By the movement, the heating unit 61 is in the state shown in FIG.

  That is, the heating unit 61 is in a state before the micro sample 19 is sandwiched between the lower disk substrate 14 and the upper disk substrate 16, and the plate 80 and the plate 90 are separated by a distance L1 as shown in FIG. Become posture.

  In the posture shown in FIG. 3, the plates 80 and 180 and the plates 90 and 190 are separated by a distance L1 that can secure a region 92 necessary for sandwiching the micro sample 19 between the lower disk substrate 14 and the upper disk substrate 16. Separated.

  After the micro sample 19 is sandwiched between the lower disk substrate 14 and the upper disk substrate 16, the plates 80 and 180 and the plates 90 and 190 are joined. As a result, the region 92 shown in FIG. 3 becomes smaller than the region shown in FIG. 2, and the glass tubes 53 and 93 can be brought close to the micro sample 19.

  The size of the region 92 in the state shown in FIG. 2 can accommodate the micro sample 19 inside.

  As described above, the glass sample 53 and 93 are brought close to the minute sample 19 after the minute sample 19 is sandwiched between the lower disk substrate 14 and the upper disk substrate 16 as compared with the case where such movement is not performed. Thus, the distance between the glass tubes 53 and 93 and the micro sample 19 can be shortened, and the heating efficiency can be greatly improved.

  FIG. 6 is a schematic diagram of constant temperature control using the heating unit of the embodiment of the present invention.

  First, the desired set temperature y0 is input to the controller 1. The controller 1 controls the power source 2, controls the temperature of the heater 3, and heats the sample 4. The temperature of the heater 3 at that time: Th and the temperature of the sample 4: Ts are monitored by thermocouples 5 and 6 installed in the vicinity thereof, and their correlation is measured. Desired sample 4 (thermocouple 6) temperature: Heater temperature corresponding to Ts: Th is input to the controller 1, and the heater is heated to a constant temperature by PID control. The sample temperature Ts is made constant.

  When the substrate is set in the above heating unit and heated, and the temperature of the heater and the substrate is measured, data as shown in FIGS. 7, 8, and 9 is obtained. Here, when the heater temperature is set to be kept at 100 ° C. for 30 minutes to 390 minutes and 60.0 ° C. for 420 minutes to 730 minutes, the sample temperatures are 72.21 ± 0.03 ° C. and 48.48 respectively. Constant at 28 ± 0.02 ° C.

  Thus, it was confirmed that there was no drift in the temperature stability of the sample part and the distance between the surfaces under the heater temperature control.

  In the currently manufactured heating unit, it was confirmed that the sample part temperature could be increased to 190 ° C. This can be further increased by changing the heater.

  Further, as shown in FIG. 10, according to the heating unit of the present invention, the distance drift was the same as that at room temperature even when the sample part temperature was controlled at 50 ° C., and there was no change. This indicates that heat does not leak from the heating system to the entire apparatus.

  The configuration of the heating unit 61 described above can be changed, for example, as shown below.

  That is, in the example shown in FIG. 1, as shown in FIG. 2, the case where the single heater wire 100 is accommodated in both the glass tubes 53 and 93 is illustrated, but the individual heater is composed of the glass tube 53 and the glass tube 93. You may make it accommodate a line.

  Further, a plurality of heater wires may be accommodated in the glass tubes 53, 93, or the glass tubes 53, 93 may be arranged in a double layer or in a plurality of stages in the vertical direction.

  According to the present invention, a sample (solid, liquid, liquid crystal, etc.) is sandwiched between two solid substrates, and the viscoelasticity change, friction / lubricating characteristics of the sample and the coupling between the sample and the solid substrate are changed while changing the thickness. It is possible to evaluate the temperature dependence such as the strength. In addition, the substrate itself can be used as a sample, and the friction (lubrication) characteristics of each other can be measured without sandwiching the sample therebetween. The surface can also be modified by adsorption or chemical modification [LB (Langmuir Brochette) modification]. In addition to vibrating the surface on one side in the horizontal direction, the frequency response of the sample can also be measured by vibrating in the direction perpendicular to the surface.

[Second Embodiment]
The heating unit of the present invention can be applied to an X-ray diffraction (X-ray diffraction) apparatus.

  FIG. 11 is a configuration diagram of an X-ray diffraction apparatus with a heating unit showing another embodiment of the present invention, and FIG. 12 is an enlarged view of the X-ray diffraction apparatus.

  In FIG. 11, 201 is an X-ray diffractometer, 202 is an X-ray, 203 is a heating unit, 204 is a drive side device, and 205 is a drive system.

  In FIG. 12, it consists of a cylindrical disk 210, gold 211, a substrate (mica) 212, an X-ray 217, and a distance (D) between the surfaces.

  Here, an X-ray diffraction apparatus for a liquid nano thin film will be described.

  First, a structure evaluation method by X-ray diffraction of a liquid nano thin film is established using synchrotron radiation X-ray (SPring-8). We aim to elucidate the correlation between the liquid structure in the nanospace and the molecular structure and surface properties.

SPring-8 BL40B2: Energy: 8 keV or 15 keV, beam diameter: 100 or 200 μm
Here, the sample configuration and instrument layout were improved to reduce background scattering such as air and window kapton.

Incidentally, the direct evaluation of the structure in the conventional liquid thin film is
(1) SFA and X-ray diffraction measurement: Evaluation of smectic liquid crystal 8CB thin film, but with a film thickness of about 0.5 μm (see Non-Patent Document 3 above)
(2) SFA and X-ray reflectivity method: electron density profile in the thickness direction of pseudospherical molecule (TTMSS) in nano space, but there are very many fitting parameters (see Non-Patent Document 4 above)
In the X-ray diffraction apparatus of the present embodiment, the heating unit 61 (203, 213) is disposed in the vicinity of the upper disk substrate 16 (212) and the lower disk substrate 14 (214) as in the first embodiment.

  Also in this embodiment, after the micro sample 19 is sandwiched between the lower disk substrate 14 and the upper disk substrate 16, the glass tubes 53 and 93 are brought close to the micro sample 19 so that such movement is not performed. As compared with the above, the distance between the glass tubes 53 and 93 and the micro sample 19 can be shortened, and the heating efficiency can be greatly improved.

  FIG. 13 is a schematic view of a combined surface force / fluorescence measurement apparatus with a heating unit (see Non-Patent Documents 5 and 6) showing still another embodiment of the present invention.

  In this figure, 301 is a lower substrate, 302 is an upper substrate, 303 is a dye solution as a micro sample, 304 is a twin pass unit (driven by a motor through a horizontal spring), 305 is a spectroscope (streak camera), and 306 is A ps pulse laser, 307 is an objective lens, and 308 is a heating unit, which has the following implementation contents.

(1) Evaluation of the viscosity of the confinement liquid with a viscous probe The viscous probe is a cyanine dye (Cy1),

  Increasing the viscosity of the solvent limits the non-radiative transition and increases the fluorescence lifetime.

(2) pH evaluation with a pH-sensitive probe at the solid-liquid interface The pH-sensitive probe is fluorescein (FL),

  Important in vivo and at functional material interfaces.

  (3) Observation of pyrene excimer formation / annihilation dynamics in confined liquid

  Those skilled in the art can make various modifications, combinations, sub-combinations, and alternatives for the components of the above-described embodiments within the technical scope of the present invention or an equivalent scope thereof.

  The heating unit of the present invention can be applied to various systems in the case of heating a sample of a resonance shear measurement device, an X-ray diffraction device, and a fluorescence lifetime measurement device.

  The present invention is applicable to a heating unit that can efficiently heat a micro liquid sandwiched between substrates of arbitrary shapes with high accuracy.

  In addition, this invention is not limited to the said Example, Based on the meaning of this invention, a various deformation | transformation is possible and these are not excluded from the scope of the present invention.

  The heating method for a micro sample of the present invention can be used as a heating method for a micro sample that can efficiently and accurately heat a micro sample sandwiched between substrates having an arbitrary shape.

1 Controller 2 Power supply 3 Heater (light source)
4, 19 Small sample 5 Thermocouple for heater temperature measurement 6 Thermocouple for sample temperature measurement 10 Resonant shear measurement unit 11 Cantilever for vertical force measurement 12 Lower disk holder 13 Upper disk holder 14 Lower disk substrate 15 Four-part piezo element 16 Upper disk Substrate 17 Leaf spring 18 Electric cable 20 Capacitance meter 21 Thermocouple for heating part 22 Thermocouple for sample part 23, 24 Electric cable 53, 54, 56, 93, 94, 96 Glass tube 61, 203, 308 Heating unit 71 First heating unit 72 Second heating unit 80, 90, 180, 190 Plate 81, 83, 91 Flexible cylindrical member 92 Area necessary for sandwiching minute sample 100 Heater wire 101, 104, 107 Stranded wire 102, 106 Joint 103, 105 Heating wire 201 X-ray diffractometer 202, 217 X-ray 204 drive side device 205 drive system 210 first cylindrical disk 211 first gold 212 substrate (mica)
D Distance between surfaces 301 Lower substrate 302 Upper substrate 303 Dye solution as a minute sample 304 Twin pass unit 305 Spectrometer (streak camera)
306 ps pulse laser 307 Objective lens

Claims (4)

  Two or more opposing heating systems surrounding a micro sample sandwiched between two substrates are used, a substantially arc-shaped infrared heater is used for heating, and a heat ray emitted from the infrared heater is placed on the opposite side of the micro sample. In a method for heating a micro sample that is focused by a mirror and heating the sample part, the micro sample sandwiched between the infrared heater and the substrate is placed in a container to insulate it, and the container is used for exchanging the micro sample. And a method of heating a micro sample, which is divided into two or more for driving the sample part.   2. The method of heating a micro sample according to claim 1, wherein the micro sample is a liquid or a solid.   2. The method of heating a micro sample according to claim 1, wherein the temperature of the sample part is controlled by observing the temperature of the heating part and the sample part, determining a desired set temperature, and setting the temperature of the heating part to the infrared heater by a feedback circuit. A method for heating a micro sample, characterized in that the amount of current applied is controlled and kept constant at a desired temperature within 0.1 degrees.   2. The method for heating a micro sample according to claim 1, wherein the heating system is a box-shaped container for allowing observation light to enter in a direction perpendicular to the substrate, and the substrate measures a normal force applied to the substrate. A heating method for a micro sample characterized by being connected to an external drive system that moves up and down via a spring.

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