CN101995416B - Softening point measurement device and conduction of heat determinator - Google Patents

Softening point measurement device and conduction of heat determinator Download PDF

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Publication number
CN101995416B
CN101995416B CN201010258421.6A CN201010258421A CN101995416B CN 101995416 B CN101995416 B CN 101995416B CN 201010258421 A CN201010258421 A CN 201010258421A CN 101995416 B CN101995416 B CN 101995416B
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China
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probe
heat
sample
heating
conduction
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CN201010258421.6A
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Chinese (zh)
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CN101995416A (en
Inventor
安藤和德
岩佐真行
繁野雅次
百田洋海
渡边和俊
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日本株式会社日立高新技术科学
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Priority to JP2009-187479 priority Critical
Priority to JP2009187479A priority patent/JP5461917B2/en
Application filed by 日本株式会社日立高新技术科学 filed Critical 日本株式会社日立高新技术科学
Priority claimed from CN201410217170.5A external-priority patent/CN104048988B/en
Publication of CN101995416A publication Critical patent/CN101995416A/en
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Publication of CN101995416B publication Critical patent/CN101995416B/en

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Abstract

A kind of softening point measurement device and conduction of heat determinator are provided, with when using the cantilever with heating part that sample local is heated the softening point to measure sample or conduction of heat, heat exchange is carried out by only contact site at probe Yu sample, bring heat affecting to the periphery of measuring point, and can carry out only in softening point measurement and the conduction of heat mensuration of contact site.In the softening point measurement device and conduction of heat determinator of the local based on probe microscope, by making the environment of probe and sample surface be 1/100 air pressure (103Pa) below or by adiabator, probe side being applied to the thickness that thermal runaway is less than 1/100, reduce the thermal runaway from probe side, the only contact site at about probe Yu sample surface carries out heat exchange.

Description

Softening point measurement device and conduction of heat determinator

Technical field

The present invention, for sweep type probe microscope etc., is specifically related to have heating part at cantilever, and by being locally heated by the contact site with sample, the amount of bow of detection cantilever measures the sweep type probe microscope of the softening point (vitreous or fusing point) of sample.It addition, relate to the variations in temperature by detecting cantilever from the resistance change of the heating part of cantilever, measure the sweep type probe microscope of the conduction of heat of sample surface via the contact site with sample.

Background technology

The conventional sample surface that is locally heated by measure the device of the softening points such as vitreous or the melting of sample, by: there is the detector (probe) of heating part;Heat the function of this heating part;Reflecting mirror to the position detection that detector includes irradiates the light source of light;What detection was reflected from the encountering reflecting mirror of light source reflects light and is converted to the detector of the signal of telecommunication;And the output signal of this detector is constituted as the circuit of the bending displacement signal of above-mentioned detector.If detector front end contacts with sample surface; and heat heating part; then the contact site with sample surface is heated; if arrive the temperature of the softening point such as vitreous or melting according to sample material; then detector can be absorbed in sample surface; detected the bending displacement signal as detector, thus carried out the mensuration (patent documentation 1) of softening point.

It addition, the device of the conventional conduction of heat measuring sample, by: there is the detector of heating part;Measure the function of the resistance of heating part;Detector has reflecting mirror and irradiates the light source of light to reflecting mirror;What detection was reflected from the encountering reflecting mirror of light source reflects light and is converted to the detector of the signal of telecommunication;And the output signal of this detector is constituted as the circuit of the bending displacement signal of above-mentioned detector.If adding the heating part of thermal detector, detection resistance value, detector front end contacts with sample surface and scans on sample surface, then it is distributed according to the conduction of heat in sample surface and changes from detector to the hot-fluid membership of sample, the temperature of heating part can change, resistance value also can change, and by detection resistance value, the distribution etc. carrying out the conduction of heat in sample surface measures (patent documentation 1).

It addition, detector uses platinum line etc., but a diameter of 6 μm of line, the radius of curvature of detector front end are 5 μm etc., the thickest, it is impossible to realize the resolution capability of Nano grade etc..From manual manufactures such as platinum lines, the cantilever that exploitation is made by the silicon (Si) of semiconductor machining, to replace line detector.

Therefore, for the purpose of local heating or conduction of heat mensuration locally etc., the occasion of the cantilever of silicon is utilized to increase.

The silicon cantilever of local heating, has adulterant resistance in heating part manufacture.Make adulterant portion generate heat, be locally heated by sample surface, and measure the softening point of sample.Manufacture probe front to be etched and the cantilever of sharpening (patent documentation 2) by semiconductor machining.

It addition, the silicon cantilever that conduction of heat measures, constitute in cantilever front end and have the pattern wiring of metallic film.And, this cantilever is by the probe included its front end, when being heated to uniform temperature, contacts with sample surface and scans, and using the degree that enters to the hot-fluid of sample surface as the resistance variations of metal thin film patterns, carries out conduction of heat distribution etc. and measures.The cantilever of metal thin film patterns is equally by semiconductor processing and manufacturing (patent documentation 3).

Silicon cantilever uses semiconductor machining, and probe front, by sharpening to 10nmR etc., is fabricated to the mensuration of the conduction of heat of the heating for local or local, is also used for heat analysis in field of nanometer technology.

Patent documentation 1: Japanese Kohyo 11-509003

Patent documentation 2:US-20060254345

Patent documentation 3: Japanese Unexamined Patent Publication 7-325092

Summary of the invention

But, even if learning and silicon cantilever being passed through semiconductor machining by probe front sharpening to about 10nmR, it is difficult to measure by the heating of sample local being carried out the conduction of heat of softening point measurement or local.

When carrying out local and heating, heat heating part, by the conduction of heat of probe being heated the contact site with sample.The front end of probe has the radius of curvature of 10nmR, and probe side forms face for cone (pyramid) shape.Therefore, this probe side also can be heated, and the heat of heating part transmits to sample contact site from probe, and produces the thermal runaway via air from probe side, brings heat affecting also can to the periphery of probe contact site.

In the mensuration of softening point, when the characteristic of the more neighbouring measuring point of hope, because of the heating action at initial measuring point, thermal process (hot resume) can be brought to the sample surface of periphery, softening point measurement after next measuring point can become by thermal process, it is impossible to accurately carry out physical property and compare.If considering, heat spreads via air, although then the shape of probe front is by sharpening, the heat affecting caused due to heated probe, substantially identical with the detector generation of thicker diameter effect.

It addition, when measuring conduction of heat, frontier inspection surveys the resistance limit of heating part of heating makes probe scan at sample surface, but the detection range of this resistance is more than the contact site of probe and sample surface, also reach due to the thermally influenced scope of the above-mentioned heat radiation from probe side.Therefore, it is impossible to Accurate Determining conduction of heat.If it addition, there is difference of height in sample surface, then due to probe side concavo-convex close to difference of height of face, producing heat radiation same as described above, although material aspect is identical but apparent upper conduction of heat is different, it is impossible to Accurate Determining conduction of heat is distributed.

Therefore, it is an object of the invention to provide and there is probe, utilize the cantilever with heating part that sample carries out local and heat, bring softening point measurement method and the determinator thereof of heat affecting will not to the periphery beyond the measuring point of sample.Additionally, it is provided that have probe and heating part equally, measure the resistance variations of heating part, the thermal runaway beyond the contact site of removal and sample, only assay method and the determinator to the conduction of heat that the conduction of heat of contact site is accurately carried out.Heating or localized heat conduction measures additionally, it is provided that be not limited to local, the exchange of heat at the contact site of probe Yu sample surface, is only high resolution at in-plane, the highly sensitive device that the shape not caused by concavo-convex difference etc. in vertical direction is affected.

The present invention solves the problems referred to above, it is provided that following scheme.

In the present invention, about local heating, sweep type probe microscope includes: has probe in front end, and has the cantilever of heating part;Alive voltage applying unit is executed to heating part;Detect the displacement detecting unit of the displacement of this cantilever;And make the sample mobile unit that sample moves, heated probe is carried out by heating heating part, it is locally heated by the contact site with sample, the amount of bow of detection cantilever, measure the softening point of sample, wherein, by could be used without the apparatus structure escaped from the heat of probe side, the only contact site at probe Yu sample surface carries out heat exchange.By using such structure, bring heat affecting will not to the part beyond the local becoming mensuration object, the heating of highly sensitive local can be carried out.

It addition, the conduction of heat about local measures, sweep type probe microscope includes: has probe in front end, and has the cantilever of heating part;Alive voltage applying unit is executed to heating part;The current detecting unit of heating part;Detect the displacement detecting unit of the displacement of this cantilever;And make the sample mobile unit that sample moves, measure the resistance variations of heating part, by detecting the variations in temperature change as resistance value of cantilever, the conduction of heat of sample surface is measured via the contact site with sample, wherein, by could be used without the apparatus structure escaped from the heat of probe side, the only contact site at probe Yu sample surface carries out heat exchange.By using such structure, bring heat affecting will not to the part beyond the local becoming mensuration object, the mensuration of the thermal conductivity of highly sensitive local can be carried out.

Conduction of heat about the heating of above-mentioned local and local measures, one of concrete structure of thermal runaway not from probe side is, at above-mentioned basic sweep type probe microscope plus Dewar vessel and vacuum exhaust unit, by the vacuum of the environment that raising probe and sample surface are placed in, get rid of the Transfer Medium of heat.Accordingly, removing the heat from probe side and escape, heat exchange is only at the contact site of probe Yu sample surface.Vacuum is preferably at 1/100 air pressure (103Pa) below, accordingly, the thermal runaway from probe side face can be made for less than 1%, the only heat exchange at probe Yu the contact site of sample surface is more than 99%.

It addition, as other same structures, cover probe side face, particularly SiO with adiabator2Or Si3N4The thermal runaway of side of the probe from the application can also can be made for less than 1% by controlling its thickness as heat insulating coating film materials'use in semiconductor machining, the only heat exchange at probe Yu the contact site of sample surface is more than 99%.

(invention effect)

In the present invention, add hanker in local, escape by reducing the heat from probe side, only contact site at probe Yu sample surface can carry out heat exchange.Accordingly, suppressing the heat conduction to measuring point periphery, impact that each point heat each other causes disappears, and can carry out the softening point measurement at the neighbouring measuring point of submicron rank.

It addition, in the mensuration of conduction of heat, the only contact site at probe Yu sample surface carries out heat exchange, reduce the thermal runaway via air from probe side as far as possible as a result, the noise of the physical property signal that entrance can be suppressed to obtain due to this mensuration is for less than 1%.Accordingly, it is to avoid according to the shape impact of the concavo-convex difference of sample surfaces, carry highly thermally conductive measurement accuracy.

Accompanying drawing explanation

Fig. 1 is the skeleton diagram of the softening point measurement device using the sweep type probe microscope involved by the first embodiment of the present invention.

Fig. 2 be heating part be the example of the resistive type cantilever of adulterant.

Fig. 3 be heating part be the example of the cantilever of metal thin film patterns type.

Fig. 4 is the figure of step measuring the softening point such as vitreous or fusing point, and (a) is to represent that heating is initial, and (b) is to represent when adding the thermal expansion hankered, figure when (c) is to represent softening.

Fig. 5 is the actual measurement example softening curve in air.

Fig. 6 is the explanatory diagram of the movement of the heat about the probe/sample room in air, and (a) is to represent that heating is initial, and (b) is to represent when adding the thermal expansion hankered, figure when (c) is to represent softening.

Fig. 7 is the actual measurement example softening curve in a vacuum of the present invention.

Fig. 8 is the explanatory diagram of the movement of the heat of the probe/sample room in a vacuum about the present invention, and (a) is to represent that heating is initial, and (b) is to represent when adding the thermal expansion hankered, figure when (c) is to represent softening.

Fig. 9 is the actual measurement example of the local heating in air, a () is the surface configuration image after the local heating at the 9 of 5 μm spacing, b () is the measured curve softening curve at 9, c () is the surface configuration image after the local heating at the 9 of 1.5 μm spacing, (d) is the measured result of the measured curve softening curve at 9.

Figure 10 is the actual measurement example of the heating of local in a vacuum of the present invention, and (a) is the surface configuration image after the local heating at the 9 of 0.5 μm spacing, and (b) is the measured result of the measured curve softening curve at 9.

Figure 11 is the skeleton diagram of the conduction of heat determinator using the sweep type probe microscope involved by the second embodiment of the present invention.

Figure 12 is the actual measurement example of the resistance variations of the heating part comparing cantilever in air and vacuum, a () is depending on the air of the distance of probe and sample room and the comparison curves of vacuum, b () is to represent the figure that heat in an atmosphere is escaped, c () is the figure representing and not having thermal runaway in a vacuum, d () is the figure of the thermal runaway in an atmosphere representing other type of cantilever, (e) is the figure not having thermal runaway in a vacuum representing other type of cantilever.

The actual measurement example of conduction of heat image when Figure 13 is to measure concavo-convex sample, in an atmosphere, (a) is to represent surface configuration image, and (b) is to represent conduction of heat image, and (c) is the figure representing thermal runaway.

When Figure 14 is the concavo-convex sample measuring the present invention, the actual measurement example of conduction of heat image in a vacuum, (a) is to represent surface configuration image, and (b) is to represent conduction of heat image, and (c) is the figure representing thermal runaway.

Figure 15 be measure concavo-convex sample time, the actual measurement example of other kinds of cantilever conduction of heat image in an atmosphere, (a) is to represent surface configuration image, and (b) is to represent conduction of heat image, and (c) is the figure representing thermal runaway.

When Figure 16 is the concavo-convex sample measuring the present invention, the actual measurement example of other kinds of cantilever conduction of heat image in a vacuum, a () is to represent surface configuration image, b () is to represent conduction of heat image, (c) is the figure representing thermal runaway.

Figure 17 is the explanatory diagram being thermally shielded coating in the probe side of the present invention, and (a) is the figure of the state before representing heat insulation coating, and (B) is the figure of the state after representing heat insulation coating.

The actual measurement example of conduction of heat image when Figure 18 is to measure film sample, in an atmosphere, (a) is to represent surface configuration image, and (b) is to represent conduction of heat image, and (c) is the figure representing thermal runaway.

When Figure 19 is the film sample measuring the present invention, the actual measurement example of conduction of heat image in a vacuum, (a) is to represent surface configuration image, and (b) is to represent conduction of heat image, and (c) is the figure representing thermal runaway.

Figure 20 is the explanatory diagram that the film sample to the present invention carries out conduction of heat mensuration in a vacuum.

Description of reference numerals

1 cantilever

2 probes

3 cantilever installation portions

4 samples

10 heating parts

11 Dewar vessels

12 vacuum exhaust unit

15 electric current lead-ins

16 voltage applying units

17 current detecting units

173 heat insulating coats

183 absorption water

201 heating cooling stagees

Detailed description of the invention

Below, referring to the drawings, illustrate to use the softening point measurement device of the sweep type probe microscope of the present invention and the basic structure of conduction of heat determinator and measuring principle.It addition, accompanying drawing is to carry out recording centered by the structure needed for the explanation of the present invention, omit with the part of the element implementing unrelated sweep type probe microscope of the present invention.

In the present invention, sweep type probe microscope includes: has probe in front end, and has the cantilever of heating part;Alive voltage applying unit is executed to heating part;Detect the displacement detecting unit of the displacement of this cantilever;Make the sample mobile unit that sample moves;Make the sample mobile unit that sample moves;And Dewar vessel and vacuum exhaust unit, carry out heated probe by heating heating part, be locally heated by the contact site with sample, the amount of bow of detection cantilever, measure the softening point of sample, these, it is preferred to be 1/100 air pressure (10 by making the environment of probe and sample surface3Pa) below, making to escape as less than 1% from the heat of probe side, the only heat exchange at probe Yu the contact site of sample surface is more than 99%.

It addition, by the probe side covering the cantilever used with adiabator, prevent the thermal runaway from above-mentioned probe side.Accordingly, the effect identical with during the above-mentioned vacuum of raising is obtained.

Below, accompanying drawing is used to illustrate each structure.

(embodiment 1)

It is described with reference to the first embodiment of the present invention.Fig. 1 is the skeleton diagram of the softening point measurement device using sweep type probe microscope.Cantilever 1 has probe 2 and heating part 10 in front end, is arranged on cantilever erecting bed 3.Sample 4 is arranged on sample stage 5, and sample stage 5 is arranged on sample mobile unit 6.Sample mobile unit 6 can carry out action and the action of plane (horizontal) direction of above-below direction.By in above-below direction action, probe 2 can be pressed in sample surfaces or away from.In the action of in-plane, by making probe 2 and sample surface contact position relative movement, sample surfaces can be scanned.Sample mobile unit 6 is arranged in Dewar vessel 11.There is transparent window 13 at the top of Dewar vessel 11, it is ensured that vacuum-tightness, be vacuum in making Dewar vessel with vacuum exhaust unit 12.Vacuum can be confirmed by vacuometer 14.Having lasing light emitter 7 outside Dewar vessel, laser 8 is by window 13 and exposes to cantilever 1, and the reflection light of laser 8 passes through window 13, arrives displacement detecting unit 9.The displacement of the above-below direction of probe 2, is detected by the position arriving displacement detecting unit 9.It addition, at Dewar vessel 11, it is ensured that electric current lead-in 15 is installed on vacuum-tightness, electrical insulating property ground, by utilizing voltage applying unit 16, the heating part 10 of cantilever 1 is applied voltage, flows through electric current, can be with heated probe 2.It follows that have the example of the cantilever of heating part with Fig. 2 and Fig. 3 explanation.

In fig. 2, cantilever arm 21 forms channel-shaped, and the only part in probe 2 side forms adulterant resistance heating portion 22.Owing to adulterant resistance heating portion 22 is the high resistance on low-doped, electric power, cantilever arm 21 is the low resistance on highly doped, electric power, therefore, when electric current flows to the opposing party of cantilever arm from a side of cantilever arm via adulterant resistance heating portion 22, adulterant resistance heating portion is heated.Probe 2 is doped agent resistance heating portion 22 and heats through conduction of heat.

In figure 3, at cantilever arm 31 metal film pattern 32.Owing to metal thin film patterns is wider at cantilever arm, less being difficult to of resistance generates heat, and width is more the thinnest to the front end of probe 2, and the relatively big easily heating of resistance, therefore the front of probe 2 is heated.Illustrating the example of 2 cantilevers with heating part, even if being adulterant resistance heating or the mode of metal thin film resistor heating, just can use equally as long as there is the cantilever of heating part at cantilever.It follows that illustrate to measure the concept of softening point with Fig. 4.

In Fig. 4 (a), when making probe 2 contact with sample 4, detect the position of the reflection light of laser 8, the position 41 of perception reflex light with displacement detecting unit 9.In Fig. 4 (b), if utilizing heating part 10 heated probe 2, then sample 4 is heated by probe 2, produces thermal expansion 40, becomes reflecting the position 42 of light.This state is sample thermal expansion, is lifted upward by probe.In Fig. 4 (c), if improving heating-up temperature further, then sample 4 arrives the softening point such as vitreous or fusing point, becomes soft, and probe 2 is absorbed in sample 4, becomes reflecting the position 43 of light.That is, if improving heating-up temperature, then the action that the displacement of probe is carried out is, a little is moved upward and thermal expansion, until sample softens reaches maximum displacement, sample drastically declined in the softening moment.It follows that the result of curve when illustrating to automatically determine the softening point reached illustrated by Fig. 4 after Fig. 5.Be use sample be result during PET (polyethylene terephthalate, fusing point: 235 DEG C).

Fig. 5 is the example of the measured curve in air, and Fig. 6 is the schematic diagram in air.

In Fig. 5, transverse axis represents the applying voltage of the heating part to cantilever, is in along with voltage increases the relation that heating-up temperature raises.Such as, apply 6V and probe is heated to 235 DEG C.It addition, the longitudinal axis is the displacement of the above-below direction of probe.Measured curve is to heat when probe contacts with sample surface.It addition, baseline represents the characteristics such as the warpage caused by heat of cantilever monomer when probe heats in the case of not contacting with sample surface, it it is the meaning of baseline (base line, initial point).

In Fig. 6 (a), when making probe 2 contact with sample 4, if starting the heating of heating part 10, then probe 2 is heated, heat from probe 2 via the contact site with sample 4 to sample side shifting.Herein, owing to probe 2 is taper, therefore heat also can move to sample 4 via air from the side 61 of probe 2.In Fig. 6 (b), the periphery of sample side contact site beyond probe contact site also has hot-fluid to enter, and the thermal expansion 62 of sample also can reach probe contact site periphery.This state is equivalent to the curved portion steeply risen upward at the measured curve of Fig. 5.In Fig. 6 (c), if sample is heated to reach to soften the temperature of 63, then probe 2 is absorbed in sample, and curve drastically declines.Draw the part of baseline from measured curve, be that sample is thermally influenced and the part that expands.

For above-mentioned condition, next explanation is with effectiveness when carrying out in a vacuum involved in the present invention.

Fig. 7 is the example of measured curve in a vacuum, and Fig. 8 is the schematic diagram in vacuum.The measured curve of Fig. 7 is significantly different with Fig. 5.In example in the air of Fig. 5, measured curve versus baseline steeply rises, it is known that the heat affecting to sample is relatively big, and thermal expansion is bigger.On the other hand, in the example in the vacuum of Fig. 7, measured curve is with baseline with parallel metamorphosis, and when reaching to soften, probe is absorbed in, and does not has violent action.

In Fig. 8 (a), in a vacuum, heating part 10 is heated, and probe 2 is also heated, but is in the perfect condition of the thermal runaway of the side not from probe 2.Only carry out at probe contact site from probe 2 to the heat transfer of sample 4.Therefore, in Fig. 8 (b), heat is applied only to the underface of the contact site of probe 2, only has this part thermal expansion.Understand and compare with air, be less result in any case.In Fig. 8 (c), reach to soften 82.Observing measured curve, owing to it is with the form passage parallel with baseline, heat only enters immediately below probe contact site, and therefore the only thermal expansion of contact site reaches softening point with parallel natural shape.In a vacuum, it is known that only carry out the exchange of heat at probe contact site, the heat determination of local can be carried out.During it follows that illustrate to carry out multiple mensuration with accompanying drawing, actual measurement can be with which kind of degree close to the example of measuring point.

Fig. 9 is the example making the spacing of 3 × 3 measuring points be measured after changing in an atmosphere.In Fig. 9 (a), measure 5 μm spacing, 3 × 3 softening points at totally 9.Sample uses PET (polyethylene terephthalate, fusing point: 235 DEG C) equally.In Fig. 9 (b), 9 soften curve unanimously, and the heating of the most first 1 time can bring thermal process to contact site periphery, if but leave 5 μm, then becoming the softening curve on the sample surface being not affected by thermal process, curve is identical.It follows that in Fig. 9 (c), measure 1.5 μm spacing, 3 × 3 softening points at totally 9.In Fig. 9 (d), 9 softening curves are inconsistent, i.e. can be construed to owing to measuring point is the nearest, and heating action before can bring thermal process to sample, even if therefore carrying out identical heating action, also can become the softening curve of the sample surface by thermal process.Next the starting point of the present invention, example in a vacuum are described.

In Figure 10 (a), measure 0.5 μm spacing, 3 × 3 softening points at totally 9.In Figure 10 (b), 9 softening curves are consistent.Understand in a vacuum, it is difficult to bring heat affecting to the periphery of the contact site with sample.Meanwhile, can carry out measuring in the local heating that in-plane is high resolution or localized heat.Next vacuum is described.

In the figure of Fig. 6 (a), in an atmosphere, heat via air escape, arrives sample surface from the side 61 of probe 2.If being placed in vacuum environment, then in the figure of Fig. 8 (a), the thermal runaway of the side 61 from probe 2 can be removed, the heat affecting to sample surface can be suppressed.Thermal runaway from the side of probe 2 depends on the tenuity of air.In the present invention, vacuum is 1/100 air pressure (103Pa) below.If this vacuum, then the thermal runaway of the side from probe can be made for less than 1%.The heat of probe and sample contact site be exchanged for 99%, probe contact site is in dominant trait status.

(embodiment 2)

It is described with reference to the second embodiment of the present invention.Figure 11 is the skeleton diagram of the conduction of heat determinator using sweep type probe microscope.Omit in place of repeating with first embodiment.In Figure 11, except voltage applying unit 16, it is additionally provided with current detecting unit 17.While applying voltage to the heating part of cantilever, current detecting can be carried out.By detection electric current, the resistance variations of heating part 10 can be detected, the variations in temperature of heating part can be detected.If the heating part 10 at cantilever 1 applies certain voltage, make it contact with sample and scan sample surface when being heated by probe, then it is distributed according to the conduction of heat of sample surface, the heat moved to sample can change, the change of heat becomes the resistance variations of heating part, and become variations in temperature, become the amount according to conduction of heat change.Cantilever for conduction of heat mensuration can also be the type of Fig. 2 and Fig. 3.The adulterant resistance of Fig. 2 is also according to variations in temperature, and the resistance of the metal thin film patterns of Fig. 3 is also according to variations in temperature.As long as the resistance variations of heating part depends on temperature, then the cantilever with heating part is which kind of type all may be used.

In conduction of heat measures, the effectiveness in the vacuum of the present invention is obvious.With Figure 12, the effectiveness in vacuum is described.In Figure 12 (a), it is that the resistance of the heating part of cantilever changes, the most thermally influenced result with the distance of sample room according to probe.The heating part of cantilever is applied fixed voltage, is placed in the state of heating.The detection resistance value according to temperature now.If it follows that close to sample surface, then have amount of heat transfer between sample surface, the temperature of the heating part of cantilever declines, and reveals the form of resistance variations.In an atmosphere, if leaving 300 μm from sample surface, then disappear to the heat transfer of sample surface, it is impossible to observe resistance variations, but along with moving closer to from 200 μm, resistance the most slowly reduces, i.e. the temperature of heating part declines.Understand to the heat transfer of sample according to the distance between sample and probe, have heat transfer via air.On the other hand, identical with vacuum, if making probe and sample room close, then do not observe and depend on distance, only observe when probe contacts with sample that resistance reduces, i.e. temperature declines.

Represent that in air, heating part is the resistive type cantilever of adulterant in Figure 12 (b), heat via air from the state that probe front and side are escaped, if probe can change close to sample surface, amount of heat transfer.Figure 12 (c) represents in vacuum, due to not via the thermal runaway of air, therefore for only observing the curve of resistance variations when contact.

Represent that in air, heating part is the cantilever of metal thin film patterns type in Figure 12 (d), heat via air from the state that probe front and side are escaped, if probe can change close to sample surface, amount of heat transfer.Figure 12 (e) represents in vacuum, due to not via the thermal runaway of air, therefore for only observing the curve of resistance variations when contact.

It follows that illustrate to measure the example of the conduction of heat image of concavo-convex sample with accompanying drawing.

Figure 13 is to measure surface configuration image and the example of conduction of heat image in an atmosphere.Figure 13 (a) is surface configuration image, and the part 131 (square portion) being dark is the most relatively low, recessed, the sample that bright part 132 is the highest, protruding.The dark part of part bright in surface configuration image is all identical material.Figure 13 (b) is conduction of heat image.In conduction of heat image, if material is identical, then it is same color, but shows the light and shade corresponding to shape.Figure 13 (c) investigates its reason.When heating part 10 is heated, probe 2 is heated, heat from front end 122 and side 121 via air escape.When probe 2 scans bottom surface 124, close together due to heating part 10 and upper surface 123, the thermal runaway therefore from side 121 is relatively big, and the temperature of heating part 10 declines, and can error measurement be therefore that conduction of heat is preferable in bottom surface 124.Next, when probe 2 scans upper surface 123, owing to the distance of heating part 10 with upper surface 123 is left, the thermal runaway therefore from side 121 is less, the temperature of heating part 10 improves compared with during scanning bottom surface 124, can error measurement be therefore that conduction of heat is poor in upper surface 123.Upper surface 123 and bottom surface 124 are identical materials, but can mix in the signal camber information of conduction of heat.

Figure 14 is to measure surface configuration image and the example of conduction of heat image in a vacuum.Figure 14 (a) is surface configuration image, and the part 131 (square portion) being dark is the most relatively low, recessed, the sample that bright part 132 is the highest, protruding.The dark part of part bright in surface configuration image is all identical material.Figure 14 (b) is conduction of heat image.In conduction of heat image, owing to material is identical, it therefore it is same color.If the mensuration in vacuum, then can correctly measure conduction of heat image.Figure 14 (c) investigates reason.When heating part 10 is heated, probe 2 is heated, but owing to not having air therefore not have the thermal runaway from the side 121 of probe, is only from front end 122 to the amount of thermal conduction of sample 4.When probe 2 scans bottom surface 124, during scanning upper surface 123, it is only from front end 122 with the amount of heat transfer of sample 4.Therefore, bottom surface 124 and upper surface 123 are identical material, and thermal conduction characteristic is the most identical, is identical conduction of heat, can correctly measure in conduction of heat image.It follows that explanation heating part is the actual measurement example of the cantilever of metal thin film patterns type.

Figure 15 is to measure surface configuration image and the example of conduction of heat image in an atmosphere.Figure 15 (a) is surface configuration image, and the part 131 (square portion) being dark is the most relatively low, recessed, the sample that bright part 132 is the highest, protruding.The dark part of part bright in surface configuration image is all identical material.Figure 15 (b) is conduction of heat image.In conduction of heat image, if material is identical, then it is same color, but shows the light and shade corresponding to shape.Figure 15 (c) investigates reason.When heating part 10 is heated, probe 2 is heated, heat from front end 122 and side 121 via air escape.When probe 2 scans bottom surface 124, close together due to heating part 10 and upper surface 123, the thermal runaway therefore from side 121 is relatively big, and the temperature of heating part 10 declines, and can error measurement be therefore that conduction of heat is preferable in bottom surface 124.Next, when probe 2 scans upper surface 123, owing to the distance of heating part 10 with upper surface 123 is left, the thermal runaway therefore from side 121 is less, the temperature of heating part 10 improves compared with during scanning bottom surface 124, can error measurement be therefore that conduction of heat is poor in upper surface 123.Upper surface 123 and bottom surface 124 are identical materials, but can mix in the signal camber information of conduction of heat.

Figure 16 is to measure surface configuration image and the example of conduction of heat image in a vacuum.Figure 16 (a) is surface configuration image, and the part 131 (square portion) being dark is the most relatively low, recessed, the sample that bright part 132 is the highest, protruding.The dark part of part bright in surface configuration image is all identical material.Figure 16 (b) is conduction of heat image.In conduction of heat image, owing to material is identical, it therefore it is same color.If the mensuration in vacuum, then can correctly measure conduction of heat image.Figure 16 (c) investigates reason.When heating part 10 is heated, probe 2 is heated, but owing to not having air therefore not have the thermal runaway from the side 121 of probe, is only from front end 122 to the amount of thermal conduction of sample 4.When probe 2 scans bottom surface 124, during scanning upper surface 123, it is only from front end 122 with the amount of heat transfer of sample 4.Therefore, bottom surface 124 and upper surface 123 are identical material, and thermal conduction characteristic is the most identical, is identical conduction of heat, can correctly measure in conduction of heat image.Next vacuum is described.

In the figure of Figure 13 (c), in an atmosphere, heat via air escape, arrives sample surface from the side 121 of probe 2.If being placed in vacuum environment, then in the figure of Figure 14 (c), the thermal runaway of the side 121 from probe 2 can be removed, the heat affecting to sample surface can be suppressed.Thermal runaway from the side of probe 2 depends on the tenuity of air.

In the present invention, vacuum is 1/100 air pressure (103Pa) below.If this vacuum, then the thermal runaway of the side from probe can be made for less than 1%.Therefore, probe is 99% with the heat exchange of sample contact site, and probe contact site is in dominant trait status.

It addition, in mensuration in an atmosphere, in the case of sample is irregular, if being scanned with the cantilever with heating part, although then material is identical, but can be mixed into concavo-convex elevation information at conduction of heat image, this shortcoming is clearly.On the other hand, in mensuration in a vacuum, owing to only contact site at probe front and sample carries out heat exchange, conduction of heat image therefore can be measured accurately.

(embodiment 3)

In the above embodiments, illustrate when softening point measurement and conduction of heat measure, by being placed in the rarefaction of air that vacuum makes the surrounding space of probe and sample surface, remove via the conduction of heat of air, make heat exchange only remove the embodiment of thermal runaway from probe side at probe contact site.

On the other hand, in order to reduce the thermal runaway from probe side face as described above, it is described with reference to the third embodiment of the present invention as the example in addition to being placed in vacuum.Figure 17 is to suppress to be thermally shielded the example of coating from the thermal runaway of probe side.Figure 17 (a) represents the state before heat insulation coating, probe 2 for example, Si material, and probe side is by common natural oxide film 171 (SiO2) cover, its thickness is about 2.4nm.If utilizing heating part 10 heated probe 2, then produce from probe via probe side further via natural oxide film to the thermal runaway 172 of air.Now, the thermal conductivity of natural oxide film 171 becomes thermal resistance, determines the thermal runaway amount to air.Figure 17 (B) represents in probe side enforcement heat insulating coat 173, the state that probe front does not applies.Such as, utilizing semiconductor machining coating material is SiO2, about 240nm thickness time, it is big to 100 times that the thermal resistance of heat insulating coat part compares change with the thickness only having natural oxide film before coating, and heat is difficult to transmit, and can suppress the thermal runaway amount to air.The conduction of heat that thickness is 2.4nm of natural oxide film it is comparable to, if being " 100 " to the thermal runaway amount of air before coating;After coating by the SiO of identical material2Form the heat insulating coat of 240nm, then in the case of material is identical, the resistance of conduction of heat is proportional to thickness, therefore becomes 1/100 to the thermal runaway amount of air, can be set to " 1 ".Further, since probe front does not has heat insulating coat, heat therefore can be made only to exchange at probe contact site.

If replacing being evacuated to vacuum, using and being insulated the cantilever of coating to carry out the softening point measurement shown in embodiment 1, then there is not periphery to probe contact site and bring the same advantage of thermal process.If measuring it addition, carry out the conduction of heat shown in embodiment 2, then the conduction of heat that can carry out highly not affected by the concavo-convex grade of sample measures.

In the present invention, by implementing heat insulation coating, increase the resistance of the heat transfer of probe side, be 100 times by making the resistance of conduction of heat, make to the thermal runaway amount of air less than 1/100.Accordingly, can make the thermal runaway of the side from probe be less than heat insulation coating before 1%.Probe is 99% with the heat exchange of sample contact site, and in softening point measurement and conduction of heat measure, probe contact site is in dominant trait status.

In the present embodiment, illustrate to be evacuated to vacuum by replacement, and be thermally shielded coating in probe side, thus suppress the heat from probe side, only can carry out heat exchange at probe contact site, with improving vacuum, there is identical effect.

After, go on to say the embodiment improving vacuum.

(embodiment 4)

As the 4th embodiment, following description measures about the conduction of heat of thin film, the most in an atmosphere absorption water for the impact of sample surfaces and the present patent application vacuum environment under the effect of mensuration.

Figure 18 is LB film exists with island on Si substrate sample surface configuration in an atmosphere and the example measuring conduction of heat image.Figure 18 (a) is surface configuration image, and dark part is Si substrate 181, and bright part is LB film 182.LB film be thickness be the ultrathin membrane of 1 to 2nm, but in Figure 18 (b), color different (difference of heat conductivity) detected as on conduction of heat image Si with on LB film.This result is, compared with Si surface, LB film shows brighter, and the conduction of heat on Si surface is preferable.

In contrast, (1/100 air pressure (10 in the vacuum of the present patent application3Pa) in mensuration below), as shown in figure 19, result produces difference.Specifically, although result is that in surface configuration image as shown in Figure 19 (a), the brightness of Si substrate 181 and LB film 182 does not has difference, but the brightness of conduction of heat image is different as shown in Figure 19 (b).This can be described as follows.

As shown in Figure 18 (c), being hydrophilic in an atmosphere on Si substrate 181, adsorbed water 183 covers, but is hydrophobic on LB film 182, there is not absorption water.Utilizing this absorption water, the thermal runaway 184 in oriented plane direction when probe 2 contacts with the absorption water 183 on Si substrate 181, heating part 10 temperature declines.On the other hand, if probe 2 moves on LB film 182, without the thermal runaway 184 via absorption water, the temperature of heating part 10 rises.As result, in an atmosphere, more preferable than the conduction of heat on LB film 182 on Si substrate 181.

But, under vacuum conditions, as shown in Figure 19 (c), the absorption water on Si substrate 181 departs from.Therefore, in the mensuration on this Si substrate 181 utilizing probe 2, there is no heat to the absorption diffusion of water, the most so-called thermal runaway, obtain the conduction of heat image on the basis of the conduction of heat on real Si surface.In contrast, with the conduction of heat image on LB film 182 surface under equivalent environment relatively in, different from the result in air.

Therefore, in the past be contrast raw-material thermal capacitance approximation material each other, under the characteristic that hydrophilic on this raw material surface, hydrophobicity are relevant, when the conduction of heat of the ultrathin membrane being in about 1 to the 2nm of dominant trait's effect to the conduction of heat that the absorption water on this surface causes measures, the order of the raw material of contrast conduction of heat each other there will be reversion.In the present invention, it is known that by for predetermined vacuum, making the absorption water on surface evaporate, and prevent the thermal runaway from probe side via air, the face original by probe and sample surface contacts, and can correctly measure conduction of heat.

(embodiment 5)

Understanding in a vacuum, probe and sample only carry out the exchange of heat at contact site.Figure 20 is that the variations in temperature making sample side is to measure the embodiment of conduction of heat.Replace the sample stage 5 of Figure 11, heating cooling stage 201 is arranged on sample mobile unit 6.Heating cooling stage 201 is built-in with heater and temperature sensor in inside, can be heated to desired temperature.Furthermore it is possible to by cooling down with the conduction of heat of not shown cooling unit, cooling limit, limit is heated, and carries out temperature control at negative arbitrary temp.Arranging the substrate 202 with thin film 203 on heating cooling stage 201, substrate 202 is heated cooling stage 201 and controls in arbitrary temperature.Such as, heating cooling stage is heated to 100 DEG C.It follows that the heating part 10 at cantilever applies certain voltage, such as, being heated to the state of 50 DEG C, heating part 10 has the resistance of response heating-up temperature.

First, if making probe 2 directly and the upper surface of heating cooling stage 201, then due to heating cooling stage 201 be 100 DEG C, and heating part 10 is 50 DEG C, therefore heat only moves to probe 2 from probe contact site, the temperature making heating part 10 rises, and the temperature of heating part also rises, and the resistance of heating part becomes big.Can be from the temperature of the change detection heating part of resistance as it has been described above, the temperature of note heating part rises to A.It follows that make probe 2 contact on substrate 202, it is also possible to the temperature rise measuring heating part 10 is B.Then, make probe 2 contact on thin film 203, it is also possible to the temperature rise measuring heating part 10 is C.Utilize the difference of B Yu A, the ratio of the conduction of heat of substrate 202 self can be measured, furthermore with the difference of C Yu B, the ratio of the conduction of heat of thin film 203 monomer can be measured.Can measure the degree of conduction of heat, even temperature rise less, then conduction of heat is poor, and therefore amount of heat transfer is less;Otherwise, if temperature rise is relatively big, then conduction of heat is good, and therefore amount of heat transfer is bigger.Owing to carrying out the heat of self-heating cooling stage, in a vacuum not via the conduction of heat of air, heat only moves to probe 2 and heating part 10 from the contact site of probe 2, therefore can measure only in the characteristic of conduction of heat of contact site.

If it addition, make the temperature of heating cooling stage 201 be 500 DEG C wait high temperature, it is possible to measure the conduction of heat of the thin film of the condition of high temperature.If it addition, heating cooling stage to be cooled to-100 DEG C etc., it is possible to measure the conduction of heat of thin film under the state of cooling.Can be interdependent with the temperature of the conduction of heat of Accurate Determining thin film.

It is evacuated to vacuum, it is also possible to combined in an atmosphere with heating cooling stage 201 by the cantilever applying heat insulating coat 173 in probe side shown in embodiment 3 it addition, replace.Being difficult to transmit because of heat insulating coat owing to carrying out the heat of self-heating cooling stage, therefore the exchange of heat is only at probe contact site, has the effect identical with being evacuated to vacuum.

Additionally, the absorption water of sample surfaces is made to evaporate preferably by being evacuated to vacuum, measure the thermal conduction characteristic that sample surface is original, but if in air, then with heating cooling stage 201, sample can also be such as heated to more than 100 DEG C, use the cantilever applying heat insulating coat 173 in probe side shown in embodiment 3.It is difficult to transmit because of the heat insulating coat of probe side owing to carrying out the heat of self-heating cooling stage, the exchange of heat is only at probe contact site, and owing to being heated to more than 100 DEG C, the absorption water evaporation of sample surface, even if can also measure the conduction of heat of the impact not adsorbing water the most in an atmosphere.

Claims (1)

1. a softening point measurement device, based on probe microscope, this probe microscope includes: possess probe in front end, has the cantilever of heating part near it;Alive voltage applying unit is executed to heating part;Detect the displacement detecting unit of the displacement of this cantilever;Make the sample mobile unit that sample moves;For the Dewar vessel in inside by described probe and described sample placing;And the vacuum exhaust unit of this Dewar vessel, described probe is heated by heating described heating part, it is locally heated by the contact site with sample, determine that described probe is absorbed in described sample and measures the softening point of described sample by the amount of bow of detection cantilever, it is characterized in that, the surrounding making described probe and described sample is 1/100 air pressure (103Pa) below and from thermal runaway is heat less than the 1/100 of described probe side.
CN201010258421.6A 2009-08-12 2010-08-12 Softening point measurement device and conduction of heat determinator CN101995416B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6487515B1 (en) * 2000-08-18 2002-11-26 International Business Machines Corporation Method and apparatus for measuring thermal and electrical properties of thermoelectric materials

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6487515B1 (en) * 2000-08-18 2002-11-26 International Business Machines Corporation Method and apparatus for measuring thermal and electrical properties of thermoelectric materials

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Title
High resolution vacuum scanning thermal microscopy of HfO2 and SiO2;M.Hinz et al;《APPLIED PHYSICS LETTERS》;20081231;正文第1页、图1 *

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