Atomic oxygen is one of the leading candidates which causes the degradation of materials in space. That’s because atomic oxygen is highly reactive and will oxidize anything that can be oxidized. This means that most vulnerable to this type of corrosion are polymers, carbon fiber materials and unprotected electronics. So in order to extend the lifespan of a spacecraft, one first needs to counter the corrosion caused by atomic oxygen. This can be done by using proper materials for making the spacecrafts components and by avoiding the exposure of sensitive electronics to space.
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Here is a list of some common techniques used in our daily research and their possible applications:
Scanning electron microscopy (SEM) – Used to obtain high resolution images of a materials surface with a magnification far greater than in the case of optical microscopes. SEM can also be used to study the distribution of different elements in a microscopic scale or even locally (few microns area) measure the elemental composition of a material. SEM is also a valuable tool to visualize microscopic cracks and defects in a material that affect its mechanical properties. Another useful application of SEM is to study the individual grain size of powders and also evaluate the size distribution. Learn more by watching our educational video and visiting our gallery.
X-ray fluorescence spectroscopy (XRF) – Quick and easy way to precisely study the average elemental composition of various materials such as a metal alloys, ceramics and polymers. For instance, we can use XRF to verify if your supplier provides you with the metal alloy that you requested and also see if it contains any unwanted impurities. Learn more by watching our educational video.
Atomic force microscopy (AFM) – Allows to measure the roughness and surface details of extremely smooth surfaces such as glass or various fine polished materials. For example, the nano scaled roughness plays a significant role in the performance of self-cleaning windows. Learn more by watching our educational video.
X-ray diffraction (XRD) – Gives information about the crystal structure of bulk materials, powders and thin films. For instance, XRD allows to verify if a titanium dioxide powder is amorphous, anatase, rutile or a mixture. It can also give information about the effect of different thermal treatments on a metal.
Anodizing aluminum is the ultimate technique for enhancing the corrosion resistance of automobile and aircraft parts, creating nanoporous templates for nanotechnological applications and making scratch resistant casings for electronic devices (cell phones, laptops etc). Anodizing is basically a 3 step process, that consists of a pretreatment for preparing the metal surface, anodizing for creating the anodic oxide layer and sealing the pores for enhancing the corrosion resistance. In the following steps youll need to use protection like gloves and goggles in order to keep yourself safe and also to prevent the contamination of the metal that will be anodized. Anodizing should also be performed in a very well ventilated room – the acidic vapours will cause severe damage to lungs during a prolonged exposure. These vapours also quickly corrode vulnerable parts in nearby electronic systems – so dont keep any valuable devices in the anodizing room.
Before starting with the pretreatment i recommend attaching the aluminum piece on a holder (aluminum wire for example) made out of the same aluminum alloy – that way youll prevent the contamination of the metal piece in the next steps as you no longer need to touch it. This holder will later also serve as the electrical connection in the anodizing process.
In order to remove the organic contamination, soap and water can be used for cleaning away most of the dirt. After rinsing the aluminum piece with deionized water, the final cleaning needs to be done with acetone. Before anodizing however, we need to remove the natural aluminum oxide layer from the metal surface. For that purpose the aluminum piece is dipped into a sodium hydroxide solution for a short time. The bubbling of hydrogen indicates that the oxide layer has been removed and that sodium hydroxide is reacting with aluminum. After removing the natural oxide layer the aluminum piece is rinsed with distilled water. If you have freshly polished the aluminum substrate, then you can likely skip the chemical cleaning and can go straight to anodizing – that saves you a lot of money. Just be sure you dont contaminate the freshly polished surface.
For anodizing a two-electrode setup is used, where the anodizable aluminum piece is the anode. The aluminum object is connected to the positive lead (usually red). The negative lead is connected to the cathode which can be made of stainless steel. Both electrodes need to be seperated and parallel to each other. However, in order to get a uniform oxide layer all over the anodized plate, i recommend using a stainless steel bath as a cathode instead. The bath should match the size and shape of the anodizable substrates.
The anodizable substrate needs to be completely immersed into the electrolyte before starting the process. The porosity and thickness of this oxide layer depends on the electrical parameters, type of electrolyte, its temperature and anodizing time. For example hard – scratch resistant oxide layers are done with type III anodizing in sulphuric acid, at near freezing temperatures and with lower current densities.
In our experiment we used a 10% sulphuric acid solution, a current density of 2 A / dm2 and the anodizing time was 30 minutes. Since the total surface area of the substrate was 3 dm2, the anodizing current was set to 6 ampers. The temperature of the solution was around 22C at start but it had significantly increased when we measured it again after anodizing. So if there is a need to use higher current densities for anodizing, i recommend using a cooling bath around the anodizing bath. In industrial processes a constant anodizing temperature needs to be ensured.
During the anodizing process a nanoporous oxide layer is generated at the cost of aluminum and this alters the appearance of the aluminum piece. These pores are so small, that they are only visible with a powerful scanning electron microscope. For making corrosion resistant coatings, these pores need to be completely sealed and there are several ways to do it. One such method is hydrothermal sealing, which is basically keeping the anodized substrate in boiling water. As a result aluminum oxide is partially turning into aluminum hydroxide, which takes up more space and seals the small pores. Another popular method is dipping the freshly anodized substrate into paint, which is immediatelly sucked into the pores. This significantly increases the metals corrosion resistance and also gives it an awesome appearance.
The nanoporous aluminum oxide can also be used as a template in nanotechnologial applications. In our case we electrochemically deposited silver into these pores and then removed the aluminum oxide with sodium hydroxide. As a result we got silver nanowires with well defined length and diameter.
Anodizing is quite easy and with some practice, its a powerful technique for treating aluminum objects for personal or commercial purposes.
Silver nanorods / nanowires with well defined length (up to tens micrometers) and diameter (around 10 nanometers) can easily be prepared by template synthesis method.
First a template is created by anodizing aluminum. In this process a porous oxide layer is created on top of the metal. The distribution, diameter and length of the pores depends on the anodizing solution and electrical parameters.
In the next step the pores are filled with silver by electrochemical deposition. The growth starts at the bottom of the pores where the pores are connected to the conductive metal. Eventually the whole pore is filled with silver and the deposition is stopped.
In order to get the silver nanorods out of the aluminum oxide matrix, the oxide needs to be etched away. The oxide matrix is removed almost instantly when dipping the substrate into an alkaline solution. As a result the silver nanorods escape into the solution. The amount, diameter and length of the nanorods depends on the oxide template that was used in the preparation process.
Large quantities of silver nanorods can be prepared in that way since in the pores in the oxide matrix are very close to each other which means that after deposition the substrate surface mostly consists of silver in the pores. Also in the etching process only the thin oxide layer is removed from the substrate to extract the nanowires and this means one can easily tune the amount of silver nanorods in a solution by the amount of substrates dipped into the same solution. For example for preparing a solution with a small concentration of silver nanowires only one sample is dipped into the solution. All the nanorods on that sample then go into the solution. By dipping the next sample into the same solution all of the nanowires on the second sample also go into the solution and the concentration is doubled. This process can be repeated as long as aluminium oxide etching is still possible. Note that the sample needs to be removed from the solution once its oxide layer is removed (this may take only a few seconds).
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Atomic force microscope (AFM) is a powerful tool that is used to study materials by scanning over the surface with a very sharp tip. When a sharp tip approaches a surface then first Van der Waals attractive forces apply that pull the tip closer to the surface and therefore also bend the cantilever. When the tip is close enough then electrostatic repulsive forces apply. The bending of the cantilever is monitored with a lazer beam that is focused on the cantilever and reflected into the detector.This method allows to obtain greatly magnified high resolution 3D images of the studied substrates (even atomic resolution is possible). The main working modes are contact, non-contact and tapping mode. In then case of contact mode the tip is in direct contact with the material. This is suitable for studying hard surfaces. In the case of non-contact mode the tip is vibrating close to the surface. This mode is used for studying sticky and soft surfaces. In the tapping mode the tip vibrates with a greater amplitude and briefly touches the sample at its lowest point of the trajectory. This method is useful for obtaining a “real” image of the studied surface as the tip penetrates the thin film of water that is always present on substrates when measuring in open air. There are also other types of scanning probe microscopes where different information can be obtained from the sample. For example a if one uses a thermocouple as a sharp tip for scanning then it is possible to study heat distribution on microscopic electronic devices in order to detect possible spots where oveheating occurs. In the case of scanning tunnel microscopy an electric potential is applied between the tip and the sample, which causes the movement of electrons from one to other. By measuring the tunneling current, it is possible to obtain valuable information about the state of the surface. Even atomic resolution is possible in STM and therefore can be used to study novel materials such as graphene. It is also possible to use magnetic needles or thin optical cables as tip for scanning over the studied surface.
Anodizing is an electrochemical process where a thicker oxide layer is grown on the material. This is useful for improving an objects corrosion and wear resistance, manufacture nanoporous templates or give the material a decorative appearance. Not all materials can be anodized however as their oxides are not dense and hard but the technique has been widely used on aluminum, titanium, zinc, magnesium and their alloys.
The anodizing system consists of a power source, anodizing bath, electrolyte and anodizable material. The bath is usually made from a chemically resistant conductive material such as stainless steel and serves as a cathode. The anodizable material serves as an anode and is placed inside the anodizing bath with the electrolyte. Both the anode and the cathode need to be connected to the power source. The grown oxide layers properties depend on the material, used electrolyte, temperature and electrical parameters used for anodizing.
In order to produce a uniform oxide layer, the substrates are also treated before the process. The main problem is usually organic contamination of the surface, which prevents growth of the oxide layer. This is removed with organic solvents such as acetone. Often the thin native oxide layer is also removed via etching before the anodizing.
X-ray tubes are widely used for generating X-ray radiation. This radiation has a shorter wavelength than visible light and can easily penetrate through different materials. It can be used in different applications such as materials characterization (XRF, XPS, XRD etc), medicine (x-ray tomography) or security in airports.
The radiation is generated with the help of accelerated electrons. These electrons are first generated on a tungsten cathode via thermoionic emission. Then these electrons are accelerated towards the anode due to a high electric potential between the anode and the cathode. When the electrons interact with the anode, x-rays are emitted. The radiation consists of two components – characteristic x-rays and bremsstrahlung. Characteristic x-rays are generated during the relaxation process of excited anode atoms. This radiation has a specific energy. Bremsstrahlung with a broad range of energy however is emitted from the primary electrons when they slow down or change trajectory during interaction with the anode.
The generated x-rays leave the tube through a beryllium window. This material is used as it has a low atomic number and doesnt absorb much of the emitted radiation.
There are also other types of x-ray tubes, such as the twin anode x-ray tube and the rotating anode x-ray tube.
In the case of twin-anode system, the anodes are made from different materials and only one of them is bombarded with electrons at the same time. This allows fast and easy switching between two excitation energies. The other anode will also serve as a backup if one should fail.
Using a rotating anode allows the heat to distribute on a larger surface area and therefore it is possible to get x-rays with much higher energies and intensities.