A Report On THEORETICAL STUDY OF ATOMIC FORCE MICROSCOPE Final Year Project Report

UIET CSJM UNIVERSITY, KANPUR

Submitted for the partial fulfilment of Bachelor of Technology Material Science and Metallurgical Engineering

2012-2013 Submitted by GAURAV JHA Roll No-29311 Final year, MSME

Submitted To Department of Material Science and Metallurgical Engineering UIET CSJM University, Kanpur (An Autonomous Institute of Government of UP)

ACKNOWLEDGEMENT

This is to certify that the project report entitled THEORETICAL STUDY OF ATOMIC FORCE MICROSCOPY submitted by GAURAV JHA under my guidance in partial fulfilment for the award of Degree of Bachelor of Technology in Material Science & Metallurgical Engineering is a bonafide record of the project work carried out by him under my supervision during the 7th semester (August December 2012).

Project Guide Dr. ANJU DIXIT

DECLARATION

I hereby declare that this Project report is a record of my own work at UIET CSJM University, Kanpur as requirements of our Project for the award of degree of B-Tech (Material Science & Metallurgical Engineering), under the guidance of Departmental faculty Dr. Anju Dixit

GAURAV JHA MSME 4TH Yr. UIET CSJM University, Kanpur

CONTENTS
1- Introduction 1.1 Outline of the Report. 2- Background 2.1 What is Atomic Force Microscopy.... 3- Physics of AFM 3.1 3.2 3.3 3.4 3.5 Components of AFM.. Force Distance Curve.. Operating Modes. Interaction between tip and sample in AFM.. Instrumentation of AFM.

4- Applications 5- Results 5.1 5.2 Different interaction forces measurement.. Which mode is more useful? .

6- Conclusion 6.1 6.2 Why AFM is so important? Limitations of AFM

INTRODUCTION
Atomic force microscopy (AFM) is an excellent characterisation technique which can obtain high-resolution images of objects. Essentially, characterization is done when a very small cantilever is excited at its resonant frequency near the surface of a sample. Close to the surface, long range attraction and short range repulsive molecular forces act between the tip and the sample. These conditions tend the cantilever to come in contact along the surface of the sample where the displacement of the tip is being measured with the function of laser. Therefore it is possible to calculate the distance between the tip and the sample and so imaging is done. The aim of this project is to study, the working principle of different modes of atomic force microscopy, the interaction forces between the cantilever tip and the sample, the force distance curve and advantage that how it is the better than the other surface characterization technique..

OUTLINE OF THE REPORT

This project report comprises certain things that are given below in appropriate order The history of AFM Some introduction about AFM Physical construction of AFM Modes of working Instrumentation Tip sample interaction Applications of AFM Conclusion Limitations Summary

ABOUT AFM
The ATOMIC FORCE MICROSCOPE (AFM) was invented by Gerd Binning and Heinrich Rohrer in 1986 for which they got the biggest award for physics i.e. Nobel Prize. The AFM is like a part of Scanning Probe Microscopes family The AFM measures the force between the cantilever tip and the sample. Due to the interaction between the tip and the sample two kind of interaction forces exist. That are Attractive Forces Repulsive Forces Due to this interaction, Imaging is done. Everything is computerized so all the calculations and measurements are done by computer. AFM performs in three modes. That are Contact Mode Non-Contact Mode Intermittent/AC/Tapping Mode Some other modes are available but they are used in some very special applications. There are some significant advantage of AFM as an imaging tool in biology and physics. AFM is not only useful in obtaining molecular images but also in performing with fluid permitting samples. This cant be performed either by electron microscopy or optical microscopy. AFM is currently getting used in various environments air, vacuum and liquid and in different kinds of materials as metals, semi-conductors, softbiological samples, conductive and non-conductive materials.

COMPONENTS OF AFM

PIEZO-CRYSTALS
Piezo crystals are ceramic materials that expand or contract in the presence of voltage gradient and conversely, they develop an electrical potential in response to mechanical pressure. In this way, movements in x, y and z direction are possible.

PROBE
Probe represents a micro-machined cantilever with a sharp tip at one end, which is brought into interaction with the sample surface. Each probe has different specifications and shape. V-shaped cantilevers are the most popular (but also there are rectangular), providing low mechanical resistance to vertical deflection, and high resistance to lateral torsion. Cantilevers typically range from 100 to 200 m in length (l), 10 to 40 m in width (w), and 0.3 to 2m in thickness (t). Integrated cantilevers are usually made from silicon (Si) or silicon nitride (Si3N4). They are characterized by their force constant and resonant frequency, which have to be chosen according to the sample to be studied.

BEAM DEFLECTION DETECTOR

To detect the displacement of the cantilever, a laser is reflected off the back of the cantilever and collected in a photodiode. The diode is divided into four parts, When the laser is displaced vertically along the positions top (B-A) and bottom (D-C), there exists a bending due to topography, while if this movement is horizontal left (B-D) and right (A-C), it produces a torsion due to friction (lateral force).

FORCE VS DISTANCE CURVE

A force sensor in an AFM can only work if the probe interacts with the force field associated with a surface. The dependence of the van der Waals force upon the distance between the tip and the sample is shown further In the contact regime, the cantilever is held less than a few angstroms from the sample surface, and the interatomic force between the cantilever and the sample is repulsive. In the non-contact regime, the cantilever is held on the order of tens to hundreds of angstroms from the sample surface, and the interatomic force between the cantilever and sample is attractive (largely a result of the long-range Van der Waals interactions). At the right side of the curve, the scanner is fully retracted and the cantilever is un-deflected since the tip is not touching the sample (region I). As the scanner extends, the cantilever remains un-deflected until it comes close enough to the sample surface for the tip to experience the attractive van der Waals force. In the point II, the cantilever suddenly bends slightly towards the surface. As the scanner continues to extend, the cantilever deflects away from the surface, approximately linearly (region III, red color). After full extension, at the extreme left of the plot (region III, black color), the scanner begins to retract. The cantilever deflection retraces the same curve. In the point (IV), the scanner retracts enough that the tip springs free. The resolution for AFM instruments is: a) 0.1 nm on sample plane (x, y) for hard and flat surfaces and 0.7-5 nm.

OPERATING MODES

CONTACT MODE
In contact mode, AFM tip is in actual contact with the samples surface. In principle, AFM in this mode can work precisely as described above. However, if there is a bump on the surface, the cantilever will be deflected more, and consequently AFM tip scans over the surface with more force. This can result in scratching the sample surface. Moreover, if the sample surface has a trench, the cantilever may simply fly over without touching it. Both cases are not good. To exclude these bad behaviours of the cantilever, a positive-feedback system was introduced. This works as follows. When the tip comes across a bump on the surface, the deflection of the cantilever increases, and the feedback system elevates the whole cantilever holder so that the cantilevers deflection is adjusted back to it s original value, and the cantilever is returned to its original position. In the case of a trench, the same feedback system moves the cantilever down to again, maintain the same deflection. This provides the same so-called load force between the tip and the sample. The AFM working in contact mode is based on two methods that are The constant force mode The constant height mode In constant height the variation of the cantilever deflection can be used directly to measure or generate topographic data In constant force mode, the deflection of the cantilever can be used as input to a feedback circuit, that moves the circuit up and down in z direction NOTE- Constant force mode is preferred due to the positive feed-back Circuit. Pros of contact mode: This is the simplest mode of operation. It requires minimum operational skill and only basic hardware.

Allows very fast scanning (typically 0.10.5 second per scan line). The load force can be precisely controlled. Good signal-to-noise ratio even in a noisy environment. Generally cheaper and more robust cantilevers can be used. Cons of contact mode: The tip can stretch or even scratch the surface. This will lead to artefacts, therefore disrupting the sample and leading to images and measurements that are not representational of the original sample. The tip can remove poorly attached parts of the sample. Apart from just damaging the surface, this can contaminate the tip surface and prevent it from being used any further. Can provide only limited information about the surface (comparing to other modes).

Because of its simplicity, contact mode is one of the most popular modes. Contact mode is typically the best on solid and well-fixed surfaces. It normally requires rather soft cantilevers (spring constant (a characteristic measure) in the range of 0.0011 Nm1).

TAPPING/INTERMITTENT/AC MODE
To further minimize the tip impact onto the surface, dynamic or intermittent contact mode, also commonly known as Tapping mode was introduced. Another name use for this mode is AC mode. In this mode the tip taps, or oscillates up and down very fast, touching the sample surface for a very short period of time during relatively slow lateral scanning. This considerably decreases scratching (although it does not eliminate it completely). While in contact mode cantilever deflection is detected and measured, in this mode the amplitude of oscillation is typically measured. Positive feedback works in a similar manner to contact mode, by keeping amplitude constant while scanning. The force measured by AFM can be classified into long-range forces and short-range forces. The first class dominates when we scan at large distances from the surface and they can be Van der Waals force, capillary forces (due to the water layer often present in an ambient environment). When the scanning is in contact with the surface the short range forces are very important, in particular the quantum mechanical forces (Pauli Exclusion Principle forces). In tapping mode-AFM the cantilever is oscillating close to its resonance frequency. An electronic feedback loop ensures that the oscillation amplitude remains constant, such that a constant tip-sample interaction is maintained during scanning. Forces that act between the sample and the tip will not only cause a change in the oscillation amplitude, but also change in the resonant frequency and phase of the cantilever. The amplitude is used for the feedback and the vertical adjustments of the piezo-scanner are recorded as a height image. Simultaneously, the phase changes are presented in the phase image (topography). Silicon probes are used primarily. Pros of intermittent contact mode: The tip does not scratch the surface, thereby avoiding artefacts. This is extremely important for soft samples. The tip typically does not remove parts of the sample. The Tapping regime allows the collection of various kinds of information related to the properties of the surface material (phase contrast).

 Cons of intermittent contact mode: Successful use of this mode requires extensive operational skill and additional hardware. The load force typically cannot be precisely controlled, in particular in liquid environments. To attain good imaging quality, expensive cantilevers must be used. The mode does not allow for fast scanning (typically 0.52 seconds per scan line). Because of its non-destructive scanning, tapping mode is a natural choice for the imaging of soft biological surfaces. It normally requires rather stiff cantilevers (spring constants in the range of 1 Nm1 and above).

NON-CONTACT MODE
In this mode, the probe operates in the attractive force region and the tipsample interaction is minimized. The use of non-contact mode allowed scanning without influencing the shape of the sample by the tip-sample forces. In most cases, the cantilever of choice for this mode is the one having high spring constant of 20- 100 N/m so that it does not stick to the sample surface at small amplitudes. The tips mainly used for this mode are silicon probes.

TIP SAMPLE INTERACTION

INSTRUMENTATION OF AFM
The motion of the probe across the surface is controlled similarly to the STM using feedback loop and piezo-electronic scanners. (See STM basic theory) The primary difference in instrumentation design is how the forces between the probe and sample surface are monitored. The deflection of the probe is typically measure by a beam bounce method. A semiconductor diode laser is bounced off the back of the cantilever onto a position sensitive photodiode detector. This detector measures the bending of cantilever during the tip is scanned over the sample. The measured cantilever deflections are used to generate a map of the surface topography.

(Z) Z motion translator- This translator moves the AFM head towards the surface so that the force sensor can measure the force between the probe and sample. The motion of the translator is usually about 10 mm. (T) X-Y translation stage - The XY translation stage is used to place the section of the sample that is being imaged by the AFM directly under the probe. (X-P) X and Y piezoelectric transducer - With the X and Y piezoelectric transducer the (Y-P) probe is moved over the surface in a raster motion when an AFM image is measured.

 (FS) Force Sensor - The force sensor measures the force between the probe and the sample by monitoring the deflection of a cantilever. (ZP) Z piezoelectric Ceramic - Moves the force sensor in the vertical direction to the surface as the probe is scanned with the X and Y piezoelectric transducers. (FCU) Feedback control unit - The feedback control unit takes in the signal from the light lever force sensor and outputs the voltage that drives the Z Piezo-electric ceramic. This voltage refers to the voltage that is required to maintain a constant deflection of the cantilever while scanning. (SG) X-Y signal generator - The motion of the probe in the X-Y plane is controlled by the X-Y signal generator. A raster motion is used when an image is measured. (CPU) Computer - The computer is used for setting the scanning parameters such as scan size, scan speed, feedback control response and visualizing images captured with the microscope. Frame - A solid frame supports the entire AFM microscope. The frame must be very rigid so that it does not allow vibrations between the tip and the sample

APPLICATIONS
The number of applications for AFM has exploded since it was invented in 1986 and now a day this technique is involved in many fields of Nano science and nanotechnology. The remarkable feature of STM and AFM instruments is their ability to examine samples not only in an ultrahigh vacuum but also at ambient conditions or even in liquids. One of the advantages of AFM is that it can image the non-conducting surfaces, and therefore it is very suitable for biological systems. The AFM is capable of measuring nanometres scale images of insulating surfaces with little or no sample preparation as well as measuring three dimensional images of surfaces and studying the topography. Some possible applications of AFM are: Substrate roughness analysis. Step formation in thin film epitaxial deposition. Pin-holes formation or other defects in oxides growth. Grain size analysis. Phase mode is very sensitive to variations in material properties, including surface stiffness, elasticity and adhesion. Comparing the tip-samples forces curves for materials to study the ratio of Youngs Modulus (graphite as a reference for measure of the indentation). Obtaining information of what is happening under indentation at very small loads. By In situ AFM analysis with changes in temperature we can study changes in the structure.

RESULTS
Q- Which mode is more useful in surface analysis by AFM? I have already presented advantage-disadvantage for each of analysing mode. Which shows thatIn contact mode scan speed is high, atomic resolution is possible, easy to scan rough surfaces but chances of damage will be more, capillary forces can create certain problems and there is also a chance of distortion in imaging by lateral forces Similarly in non-contact mode there is no damage but slower scan speed exists and lateral resolution will also be low. But in intermittent mode lateral resolution is high found to be high, less damage forms, almost no lateral forces exists. Yes scan speed is low but quality of imaging is better than all other modes From these datas, it is clear that the INTERMITTENT mode is the the best mode which gives the most optimum result..

Q- What are the forces which get measured in this technique? Normally the measured forces are Vander-Wall Forces (attractive or repulsive) from Atomic Force Microscopy Capillary forces by Capillary Force Microscopy Magnetic forces by Magnetic Force Microscopy Electrostatic forces by Electrostatic Force Microscopy

CONCLUSION

Q-WHY AFM IS IMPORTANT?

The advantages of AFM is that it can work in ambient conditions (either air or liquid) therefore making it possible to study even living organisms. The ability to get high-resolution images on a Nano scale is important for studying of many biological applications such as drug/protein interaction. As the boundaries of science expand the demand on nanotechnology is greater than ever before as scientists require higher and higher resolution images of biological macromolecules or single DNA molecules. The variation in the force field leads the probe to undergo non-linear effects such as hysteresis and bi-stability. The aim of this report is to compare mathematical models of the cantilever to what actually happens. This is done to try and achieve a better understanding of the dynamics and behaviour of the probe.

Q- LIMITATIONS OF AFM
The AFM can be used to study a wide variety of samples (i.e. plastic, metals, glasses, semiconductors, and biological samples such as the walls of cells and bacteria). Unlike STM or scanning electron microscopy it does not require a conductive sample. However there are limitations in achieving atomic resolution. The physical probe used in AFM imaging is not ideally sharp. As a consequence, an AFM image does not reflect the true sample topography, but rather represents the interaction of the probe with the sample surface. This is called tip convolution. Commercially available probes are becoming more widely available that have very high aspect ratios. These are made with materials such as carbon nanotubes or tungsten spikes. How-ever these probes are still very expensive to use for every day image analysis.

SUMMARY