Paul K. Hansma

A nondestructive method for determining the spring constant of cantilevers for scanning force microscopy

The spring constant of microfabricated cantilevers used in scanning force microscopy (SFM) can be determined by measuring their resonant frequencies before and after adding small end masses. These masses adhere naturally and can be easily removed before using the cantilever for SFM, making the method nondestructive. The observed variability in spring constant—almost an order of magnitude for a single type of cantilever—necessitates calibration of individual cantilevers in work where precise knowledge of forces is required. Measurements also revealed that the spring constant scales with the cube of the unloaded resonant frequency, providing a simple way to estimate the spring constant for less precise work.

Molecular mechanistic origin of the toughness of natural adhesives, fibres and composites

Natural materials are renowned for their strength and toughness,,,,. Spider dragline silk has a breakage energy per unit weight two orders of magnitude greater than high tensile steel,, and is representative of many other strong natural fibres,,. The abalone shell, a composite of calcium carbonate plates sandwiched between organic material, is 3,000 times more fracture resistant than a single crystal of the pure mineral,. The organic component, comprising just a few per cent of the composite by weight, is thought to hold the key to nacres fracture toughness,. Ceramics laminated with organic material are more fracture resistant than non-laminated ceramics,, but synthetic materials made of interlocking ceramic tablets bound by a few weight per cent of ordinary adhesives do not have a toughness comparable to nacre. We believe that the key to nacres fracture resistance resides in the polymer adhesive, and here we reveal the properties of this adhesive by using the atomic force microscope to stretch the organic molecules exposed on the surface of freshly cleaved nacre. The adhesive fibres elongate in a stepwise manner as folded domains or loops are pulled open. The elongation events occur for forces of a few hundred piconewtons, which are smaller than the forces of over a nanonewton required to break the polymer backbone in the threads. We suggest that this ‘modular’ elongation mechanism might prove to be quite general for conveying toughness to natural fibres and adhesives, and we predict that it might be found also in dragline silk.

Tapping mode atomic force microscopy in liquids

Tapping mode atomic force microscopy in liquids gives a substantial improvement in imaging quality and stability over standard contact mode. In tapping mode the probe‐sample separation is modulated as the probe scans over the sample. This modulation causes the probe to tap on the surface only at the extreme of each modulation cycle and therefore minimizes frictional forces that are present when the probe is constantly in contact with the surface. This imaging mode increases resolution and reduces sample damage on soft samples. For our initial experiments we used a tapping frequency of 17 kHz to image deoxyribonucleic acid plasmids on mica in water. When we imaged the same sample region with the same cantilever, the plasmids appeared 18 nm wide in contact mode and 5 nm in tapping mode.

Measuring the viscoelastic properties of human platelets with the atomic force microscope

We have measured force curves as a function of the lateral position on top of human platelets with the atomic force microscope. These force curves show the indentation of the cell as the tip loads the sample. By analyzing these force curves we were able to determine the elastic modulus of the platelet with a lateral resolution of approximately 100 nm. The elastic moduli were in a range of 1-50 kPa measured in the frequency range of 1-50 Hz. Loading forces could be controlled with a resolution of 80 pN and indentations of the platelet could be determined with a resolution of 20 nm.

An atomic-resolution atomic-force microscope implemented using an optical lever

We present the first atomic‐resolution image of a surface obtained with an optical implementation of the atomic‐force microscope (AFM). The native oxide on silicon was imaged with atomic resolution, and ≊5‐nm resolution images of aluminum, mechanically ground iron, and corroded stainless steel were obtained. The relative merits of an optical implementation of the AFM as opposed to a tunneling implementation are discussed.

Forces in atomic force microscopy in air and water

A new atomic force microscope, which combines a microfabricated cantilever with an optical lever detection system, now makes it possible to measure the absolute force applied by a tip on a surface. This absolute force has been measured as a function of distance (=position of the surface) in air and water over a range of 600 nm. In the absolute force versus distance curves there are two transitions from touching the surface to a total release in air caused by van der Waals interaction and surface tension. One transition is due to lifting off the surface; the other is due to lifting out of an adsorbed layer on the surface. In water there is just one transition due to lifting off the surface. There is also a transition in air and water when the totally released tip is pulled down to touch the surface as the surface and tip are brought together. Based on the force versus distance curves, we propose a procedure to set the lowest possible imaging force. It can now be as low as 10−9 N or less in water and 10−7 N...

Scanning tunneling microscopy

A scanning tunneling microscope (STM) can provide atomic‐resolution images of samples in ultra‐high vacuum, moderate vacuum, gases including air at atmospheric pressure, and liquids including oil, water, liquid nitrogen, and even conductive solutions. This review contains images of single‐crystal metals, metal films, both elemental and compound semiconductors, superconductors, layered materials, adsorbed atoms, and even DNA. A discussion of results on lithography leads into speculations on a bright future in which STMs may not only observe, but also manipulate surfaces, right down to the atomic level.

Short cantilevers for atomic force microscopy

We have designed and tested a family of silicon nitride cantilevers ranging in length from 23 to 203 μm. For each, we measured the frequency spectrum of thermal motion in air and water. Spring constants derived from thermal motion data agreed fairly well with the added mass method; these and the resonant frequencies showed the expected increase with decreasing cantilever length. The effective cantilever density (calculated from the resonant frequencies) was 5.0 g/cm3, substantially affected by the mass of the reflective gold coating. In water, resonant frequencies were 2 to 5 times lower and damping was 9 to 24 times higher than in air. Thermal motion at the resonant frequency, a measure of noise in tapping mode atomic force microscopy, decreased about two orders of magnitude from the longest to the shortest cantilever. The advantages of the high resonant frequency and low noise of a short (30 μm) cantilever were demonstrated in tapping mode imaging of a protein sample in buffer. Low‐noise images were tak...

Bone indentation recovery time correlates with bond reforming time

Despite centuries of work, dating back to Galileo, the molecular basis of bones toughness and strength remains largely a mystery. A great deal is known about bone microsctructure and the microcracks that are precursors to its fracture, but little is known about the basic mechanism for dissipating the energy of an impact to keep the bone from fracturing. Bone is a nanocomposite of hydroxyapatite crystals and an organic matrix. Because rigid crystals such as the hydroxyapatite crystals cannot dissipate much energy, the organic matrix, which is mainly collagen, must be involved. A reduction in the number of collagen cross links has been associated with reduced bone strength and collagen is molecularly elongated (‘pulled’) when bovine tendon is strained. Using an atomic force microscope, a molecular mechanistic origin for the remarkable toughness of another biocomposite material, abalone nacre, has been found. Here we report that bone, like abalone nacre, contains polymers with ‘sacrificial bonds’ that both protect the polymer backbone and dissipate energy. The time needed for these sacrificial bonds to reform after pulling correlates with the time needed for bone to recover its toughness as measured by atomic force microscope indentation testing. We suggest that the sacrificial bonds found within or between collagen molecules may be partially responsible for the toughness of bone.

Reproducible Imaging and Dissection of Plasmid DNA Under Liquid with the Atomic Force Microscope

Reproducible images of uncoated DNA in the atomic force microscope (AFM) have been obtained by imaging plasmid DNA on mica in n-propanol. Specially sharpened AFM tips give images with reproducible features several nanometers in size along the DNA. Plasmids can be dissected in propanol by increasing the force applied by the AFM tip at selected locations.