WO2001075427A1 - Procedes et appareil de microscopie a force atomique - Google Patents

Procedes et appareil de microscopie a force atomique Download PDF

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Publication number
WO2001075427A1
WO2001075427A1 PCT/GB2001/001470 GB0101470W WO0175427A1 WO 2001075427 A1 WO2001075427 A1 WO 2001075427A1 GB 0101470 W GB0101470 W GB 0101470W WO 0175427 A1 WO0175427 A1 WO 0175427A1
Authority
WO
WIPO (PCT)
Prior art keywords
probe
sample
cantilever
atomic force
tip
Prior art date
Application number
PCT/GB2001/001470
Other languages
English (en)
Inventor
Terence James Mcmaster
Mervyn John Miles
Massimo Antognozzi
Andrew David Laver Humphris
Original Assignee
University Of Bristol
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University Of Bristol filed Critical University Of Bristol
Priority to CA002404604A priority Critical patent/CA2404604A1/fr
Priority to AU2001244350A priority patent/AU2001244350A1/en
Priority to JP2001572856A priority patent/JP2003529761A/ja
Priority to EP01917266A priority patent/EP1269168A1/fr
Priority to US10/240,259 priority patent/US20030160170A1/en
Publication of WO2001075427A1 publication Critical patent/WO2001075427A1/fr

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q20/00—Monitoring the movement or position of the probe
    • G01Q20/02—Monitoring the movement or position of the probe by optical means

Definitions

  • This invention has to do with methods and apparatus for atomic force microscopy ("AFM”) , and in particular to new arrangements and modes of use for cantilever probes i atomic force microscopes.
  • AFM atomic force microscopy
  • Atomic force microscopes image the surface of the sample by means of a minute cantilever probe with a sharp tip which is brought into extreme proximity, and sometimes contact, with the sample surface. The interaction between sample and probe is observable by monitoring the deflection of the cantilever as the latter is scanned over the sample surface.
  • the cantilever probes are very delicate and sensitive objects, typically projecting one or two hundred ⁇ m from a chip substrate on which they are created by microfabrication- techniques such as etching. Usual materials are silicon and silicon nitride.
  • FIG. 1 One conventional AFM head arrangement in shown in Fig 1.
  • An arch-shaped optical head block 1 is mounted over a sample support arrangement including a sample stage 21.
  • a sample for investigation is positioned on the sample stage 21 and can be moved (scanned) relative to the optical head by means of coarse adjustment screws 22 and a piezoelectric scanning drive of a known kind, not shown.
  • a probe holder 3 here in the form of a flat metal locating plate, fits into the arch of the optical head block 1 over the sample stage 21.
  • the chip substrate 33 carrying the cantilever probe is mounted to the probe holder 3. This may be mounted on a piezoelectric element (not shown) or other suitable means by ' which a driving force on the cantilever probe can be applied. In this set-up the probe is fixed (in the XY plane) in use, scanning being by XY movements of the sample stage 21.
  • Other forms of AFM apparatus exist which scan the probe holder rather than the sample.
  • the conventional disposition of the cantilever probe relative to the sample/sample stage is shown in Fig 2.
  • the cantilever 4 is a straight, flat silicon nitride projection with a downwardly-directed pyramidal or conical point 41 at its end, perhaps 5 ⁇ m deep.
  • the chip substrate 33 is mounted to bring the probe 4 as near parallel to the sample surface/sample platform as the . necessary clearance for the holder and chip substrate permits; usually this involves ..about a 10° tilt from horizontal.
  • the thickness of the cantilever perpendicular to the sample is usually only about 0.5 ⁇ m and it undergoes significant deflections under very small forces.
  • the angular orientation of the cantilever probe 4 is observed via a so-called optical lever arrangement.
  • the top surface of the' cantilever 4 is made reflective - e.g. by deposition of a gold layer - and a laser beam from a laser 5 mounted in the optical head is trained on this reflection surface, ' to reflect away over a distance of a few cm to a segmented photodetector 6. Because of the long optical travel, minute angular movements of the probe tip cause substantial movements of the light beam across the photodetector 6.
  • the photodetector is sensitive to changes in the relative intensity of light incident on its respective segments. The difference between the outputs from different segments is used to observe the deflection of the cantilever probe.
  • the probe axis direction is arranged substantially perpendicular to the sample presentation plane, the probe driver then being operable to move the probe tip across the sample surface rather than towards and away from it.
  • the probe has a reflection surface for directing an incident light beam towards a detector and a normal of the reflection surface has a rearward component back along the probe axis, away from the sample in use.
  • the incident beam of a beam-reflection position detector system can approach the sample stage and be reflected back away from it, e.g. as in the optical pathway of known arrangements using a horizontal cantilever.
  • the rearwardly-directed reflection surface may be inclined e.g. at an angle of at least 30° from the probe axis. Typically it is formed to act as a planar mirror.
  • a cantilever probe having a reflection surface so oriented relative to the probe axis is an independent aspect of the invention.
  • Another independent aspect is a probe holder carrying a cantilever probe with its probe axis extending substantially perpendicularly to a sample presentation plane and with the probe having a reflection surface with a normal directed back i.e. having a rearward component relative to the probe axis, as proposed herein.
  • the cantilever preferably .incorporates the reflection surface on an integral rearwardly-directed surface portion, e.g. on a laterally projecting portion.
  • a projection can routinely be formed by microfabrication techniques such as etching; in this case the rearwardly- directed reflection surface is conveniently oblique although it may be perpendicular to the probe axis direction.
  • Such a lateral projection may be formed in a similar way, and indeed in a similar shape, to the pyramidal projections which in conventional cantilevers are used as the sharp probe tip.
  • the reflection surface may be given a reflective coating e.g. of gold or aluminium.
  • the fine probe tip itself shaped for interaction with the sample surface, is generally positioned forward of the reflection surface. In most cases it is at the distal extreme of the cantilever probe, although for certain special uses it may be laterally directed relative to the cantilever axis. This is described later.
  • the probe tip can be provided as a sharp formation on the main shaft of the cantilever, e.g. a whisker.
  • the novel disposition of the reflection beam relative to the cantilever axis in the present proposal can be associated with advantageous modes of microscopic investigation of a sample.
  • the cantilever probe can be presented to a sample surface essentially perpendicularly.
  • the probe can then be oscillated laterally across the sample surface and the resulting movements of. the probe tip detected by the observation of the reflected beam.
  • This provides a new and convenient way of carrying out shear force microscopy (ShFM) or transverse dynamic force microscopy (TDFM) exploiting reflected-beam detection methods/apparatus which in themselves are conventional and familiar to a skilled person.
  • a cantilever arrangement according to the present proposal i.e. with a perpendicularly-oriented cantilever having a rearwardly-directed reflection surface, can be substituted for the conventional cantilever and the existing optical detection system exploited substantially unchanged.
  • the range of investigative techniques available with that microscope system is therefore significantly enhanced.
  • Conventional cantilever set-ups cannot access such steep formations.
  • the cantilever probe of the invention may be used with a probe tip directed axially, as the extreme end of the probe, and/or directed laterally so that the . probe can be used against a steep surface beside it e.g. in a tapping mode.
  • Another advantageous feature of a microscope operating with the cantilever perpendicular to the sample surface is the availability of true probe tip - sample surface distance control.
  • the spring constant along the cantilever axis is much higher than the spring constant for lateral bending.
  • the degree of bend relates directly to both the tip-sample separation and the monitored force at the tip, so these cannot be independently determined.
  • the degree of bend scarcely affects the tip-sample separation, which can be therefore be set effectively independently by axial adjustment of the probe. This offers significant advantages for TDFM over conventional AFM, in particular for force displacement experiments.
  • Fig 1 is a perspective schematic view of a known AFM head arrangement
  • Fig 2 is a schematic view of the cantilever probe disposition in the conventional AFM head arrangement
  • Fig 3 shows a cantilever probe arrangement in accordance with our invention
  • Figs 4 (a) , (b) , (c) show different cantilever probe shapes, and the disposition of probes on a chip substrate;
  • Figs 5 and 6 show two arrangements of a cantilever probe holder embodying our proposals
  • Figs 7 and 8 show the tips of cantilever probes operating according to a variant procedure.
  • Figs 1 and 2 have already been described and relate to prior ' art .
  • Fig 3 shows a cantilever probe with its probe axis arranged perpendicular to the sample plane SP, in accordance with our new proposal.
  • a lateral projection 42 is formed by etching/deposition.
  • it is made similarly to the contact points on conventional probes, i.e. as a generally pyramidal formation with a flat rearwardly- directed oblique face 43. It need not have a sharp tip, however.
  • a gold coating is deposited on the oblique face 43 for function as a reflection surface.
  • the angle which the reflection surface 43 makes with the probe axis is not critical insofar as detection of probe movements is concerned, but is significant in providing for a convenient disposition ' of the sources, reflectors and detectors for the incident and reflected beams 51 of the optical system which is used for that detection.
  • the present embodiment has the incident laser beam 51 substantially perpendicular to the sample plane SP and reflecting away obliquely to the detection arrangement with its four-quadrant photodetector 6, i.e. as in the conventional module seen in Fig 1.
  • the cantilever probe 4 makes oscillations substantially parallel to the sample plane by means of a piezoelectric driver, oscillating magnetic field or other suitable means.
  • These drives may be applied to the chip substrate 33 from which the cantilever probe 4 is mounted, in a manner which is itself conventional. Alternatively drive may be via a magnetic field applied to the cantilever directly, or via acoustic coupling through a liquid.
  • the pyramid projection 42 functions only to carry the reflection surface.
  • the probe tip itself - which may comprise a fine probe extension 45 - is at the extreme distal end of the probe and is oscillated in close proximity to the sample surface so as for example to carry out shear force or transverse dynamic force microscopy.
  • the present technique using a single deflected beam in this novel arrangement is simple to use and furthermore can be implemented in apparatus which may in other respects be conventional.
  • Fig 4 (a) shows that the probe 4 may take the form of a flat V bisected by the probe axis A, with the reflector projection formed near ' the tip. Such a construction is typically of silicon nitride.
  • Fig 4(b) shows an essentially linear probe e.g. of silicon. These general forms are known, but in the present embodiment the tip of the pyramid projection need not be refined for interaction with the sample; on the contrary the pyramid or other-shaped lateral projection can be blunt and may be made relatively large for its new role as a reflection surface. By contrast the axially-directed tip of the probe is made with a fine point or whisker for interaction with the sample surface.
  • Fig 4(c) shows how more than one probe 4, e.g. of different shapes, sizes or spring constant, may be formed on a single substrate chip 33. Again, this is known in itself.
  • Fig 5 shows a cantilever probe holder 3 in accordance with one aspect of the present invention, designed for substitution for the conventional probe holder of a known AFM optical head e.g. as seen in Fig 1.
  • the cantilever probe chip substrate 33 is mounted, e.g. via an insulated piezoelectric driver pad 35, on a mounting 36 so that the probe axis is directed down onto the area on the sample platform 21. In fact it need not be exactly orthogonal in relation to the surrounding microscope construction. Particularly when modifying existing apparatus a slight angle may be preferable because it reduces possible difficulties of obstruction of the incident laser beam. Since conventional sample supports provide for the possibility of slightly inclining a supported sample, there is no problem in achieving an operating set-up with the actual sample presentation plane truly perpendicular to the probe axis.
  • This embodiment is a scanned-sample type in which a piezoelectrically-drivable scanning module 38 carries the sample platform 21.
  • Fig 6 shows an alternative mounting of the scanned-tip type, with the piezoelectric scanning drive 38 carying the probe chip 33 and the sample platform 21 static.
  • the incident laser may need to be brought in at an inclination, i.e. non-vertically.
  • Fig 7 shows (more greatly enlarged) a variant mode of operation in which a probe whisker tip 45' is laterally-directed at the probe end.
  • This enables the investigation, e.g. by tapping mode microscopy, of sample surface portions which are steeply inclined or vertical or are next to such features, e.g. trenches or walls in etched semi-conductor products.
  • Conventional AFM arrangements cannot access such surfaces at all.
  • Fig 8 shows a different variant where the sample surface is actually undercut. It also shows that the probe may combine a laterally-directed tip 45' with a longitudinally-directed tip 45.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Radiology & Medical Imaging (AREA)
  • Length Measuring Devices With Unspecified Measuring Means (AREA)

Abstract

L'invention concerne un module sonde permettant la microscopie à force atomique, qui présente un substrat et une sonde (4) en porte-à-faux orientable faisant saillie à partir de celui-ci. Dans la tête du microscope à force atomique, la sonde est montée de telle sorte que son axe soit perpendiculaire à la surface d'échantillon, par exemple de façon qu'il soit possible de réaliser une microscopie à force de cisaillement ou une microscopie à force dynamique transversale. La sonde (4) à porte-à-faux présente une surface (43) réfléchissante qui est dirigée vers le haut le long de la sonde de sorte que la pointe de la sonde peut être suivie au moyen d'un dispositif à faisceau lumineux qui en lui-même peut être classique. Par ce moyen, les opérations de microscopie à force atomique (AFM) en mode perpendiculaire peuvent être réalisées au moyen de têtes AFM avec peu de modification à partir du dispositif à mode quasi parallèle classique. La sonde peut être utilisée également en mode vertical pour l'examen de caractéristiques des parois latérales sur une surface d'échantillon.
PCT/GB2001/001470 2000-03-30 2001-03-30 Procedes et appareil de microscopie a force atomique WO2001075427A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CA002404604A CA2404604A1 (fr) 2000-03-30 2001-03-30 Procedes et appareil de microscopie a force atomique
AU2001244350A AU2001244350A1 (en) 2000-03-30 2001-03-30 Methods and apparatus for atomic force microscopy
JP2001572856A JP2003529761A (ja) 2000-03-30 2001-03-30 原子間力顕微鏡のための装置および方法
EP01917266A EP1269168A1 (fr) 2000-03-30 2001-03-30 Procedes et appareil de microscopie a force atomique
US10/240,259 US20030160170A1 (en) 2000-03-30 2001-03-30 Methods and apparatus for atomic force microscopy

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GBGB0007747.9A GB0007747D0 (en) 2000-03-30 2000-03-30 Methods and apparatus for atomic force microscopy
GB0007747.9 2000-03-30

Publications (1)

Publication Number Publication Date
WO2001075427A1 true WO2001075427A1 (fr) 2001-10-11

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PCT/GB2001/001470 WO2001075427A1 (fr) 2000-03-30 2001-03-30 Procedes et appareil de microscopie a force atomique

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EP (1) EP1269168A1 (fr)
JP (1) JP2003529761A (fr)
KR (1) KR20030015220A (fr)
AU (1) AU2001244350A1 (fr)
CA (1) CA2404604A1 (fr)
GB (1) GB0007747D0 (fr)
WO (1) WO2001075427A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009000885A1 (fr) 2007-06-27 2008-12-31 Technische Universität Ilmenau Dispositif et procédé d'étude des propriétés de surface de matériaux de types différents
CN111077347A (zh) * 2019-12-25 2020-04-28 北京航空航天大学 原子力显微术探针夹持装置

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100626222B1 (ko) * 2004-12-22 2006-09-21 한양대학교 산학협력단 주사 탐침 현미경의 기능성 디스크 및 이것을 이용하여 탐침과 기판 간의 전기적 특성을 측정하는 방법
US8528110B2 (en) * 2008-06-06 2013-09-03 Infinitesima Ltd. Probe detection system
KR101607606B1 (ko) 2015-08-17 2016-03-31 한국표준과학연구원 원자간력 현미경의 측정 방법
JP6936964B2 (ja) * 2016-08-26 2021-09-22 大日本印刷株式会社 走査型プローブ顕微鏡

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0422548A2 (fr) * 1989-10-09 1991-04-17 Olympus Optical Co., Ltd. Microscope à forces atomiques
EP0564088A1 (fr) * 1992-03-04 1993-10-06 Topometrix Microscope à force atomique avec système d'optique et support pour un cantilever
US5294804A (en) * 1992-03-11 1994-03-15 Olympus Optical Co., Ltd. Cantilever displacement detection apparatus
US5408094A (en) * 1992-05-07 1995-04-18 Olympus Optical Co., Ltd. Atomic force microscope with light beam emission at predetermined angle
US5509300A (en) * 1994-05-12 1996-04-23 Arizona Board Of Regents Acting For Arizona State University Non-contact force microscope having a coaxial cantilever-tip configuration
US5982009A (en) * 1997-03-01 1999-11-09 Korea Advanced Institute Of Science & Technology Integrated device of cantilever and light source

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0422548A2 (fr) * 1989-10-09 1991-04-17 Olympus Optical Co., Ltd. Microscope à forces atomiques
EP0564088A1 (fr) * 1992-03-04 1993-10-06 Topometrix Microscope à force atomique avec système d'optique et support pour un cantilever
US5294804A (en) * 1992-03-11 1994-03-15 Olympus Optical Co., Ltd. Cantilever displacement detection apparatus
US5408094A (en) * 1992-05-07 1995-04-18 Olympus Optical Co., Ltd. Atomic force microscope with light beam emission at predetermined angle
US5509300A (en) * 1994-05-12 1996-04-23 Arizona Board Of Regents Acting For Arizona State University Non-contact force microscope having a coaxial cantilever-tip configuration
US5982009A (en) * 1997-03-01 1999-11-09 Korea Advanced Institute Of Science & Technology Integrated device of cantilever and light source

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ALBRECHT T R ET AL: "MICROFABRICATION OF CANTILEVER STYLI FOR THE ATOMIC FORCE MICROSCOPE", JOURNAL OF VACUUM SCIENCE AND TECHNOLOGY: PART A,US,AMERICAN INSTITUTE OF PHYSICS. NEW YORK, vol. 8, no. 4, 1 July 1990 (1990-07-01), pages 3386 - 3396, XP000148046, ISSN: 0734-2101 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009000885A1 (fr) 2007-06-27 2008-12-31 Technische Universität Ilmenau Dispositif et procédé d'étude des propriétés de surface de matériaux de types différents
US8689359B2 (en) 2007-06-27 2014-04-01 Nano Analytik Gmbh Apparatus and method for investigating surface properties of different materials
CN111077347A (zh) * 2019-12-25 2020-04-28 北京航空航天大学 原子力显微术探针夹持装置

Also Published As

Publication number Publication date
KR20030015220A (ko) 2003-02-20
GB0007747D0 (en) 2000-05-17
AU2001244350A1 (en) 2001-10-15
JP2003529761A (ja) 2003-10-07
CA2404604A1 (fr) 2001-10-11
EP1269168A1 (fr) 2003-01-02

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