All posts by Captain Corrosion

X-Ray Photoelectron Spectroscopy (XPS)

November 16, 2015Materials Characterization3D animation, fotoelektron, fotoelektron spektroskoopia, fotoelektronspektroskoopia, Maido Merisalu, materials characterization, materials science, photoelectric effect, photoelectron, photoelectron microscopy, photoelectron spectroscopy, scanning, scanning photoelectron microscopy, scanning probe microscopy, spektroskoopia, SPEM, synchrotron, synchrotron radiation, synchrotron xps, x-ray, X-Ray Photoelectron Microscopy, X-ray photoelectron spectroscopy, XPSCaptain Corrosion

Photoelectric effect, photoelectron spectroscopy (XPS) and scanning photoelectron microscopy (SPEM) are explained in this short lecture. The photoelectric effect occurs when the inner shell electrons of the sample atoms are kicked out by high energy electromagnetic radiation. These electrons, that were kicked out, are called photoelectrons and their energy depends on the energy of the exciting radiation, the electrons initial binding energy and on the work function. When having a radiation source with well defined energy and measuring the energy of the emitted electrons, it is possible to get information about the samples composition and chemical state. In the case of photoelectron microscopy the exciting beam is focused into a narrow spot on the sample surface. The sample is then moved in such a way that the spot moves row by row across the sample surface and as a result photoelectrons are emitted from each irradiated spot. By collecting these photoelectrons, it is possible to map the composition or chemical state across the selected sample area (for example 100 x 100 microns area on a 2 x 2 cm sample). Photoelectrons can escape the material only from near the surface and this means that these methods are very surface sensitive, which makes them extremely useful for surface studies. This also means that the surfaces need to be very clean (cleaned with ion bombardment before measurements) and therefore ultra-high vacuum is needed.

Galvanic Corrosion – Forms of Corrosion

November 5, 2015Forms of Corrosionaluminium, aluminum, anti corrosion, captain corrosion, captaincorrosion, coating, corrosion, corrosion forms, corrosion prevention, corrosion protection, electrochemical corrosion, forms of corrosion, galvaaniline korrosioon, galvanic corrosion, galvanic couple, galvanic protection, galvanic series, galvanic series in seawater, korrosioon, Maido Merisalu, roostetamine, seawaterCaptain Corrosion

Galvanic Corrosion is an accelerated form of corrosion that occurs when two dissimilar metals are in an electrical contact. The more noble metal drives the corrosion of the active metal and this can be a very fast process. For example if an aluminum frame is connected with steel bolts then aluminum rapidly corrodes and after a few months the whole construction may collapse. So how to prevent galvanic corrosion? First, one should connect only those materials that have a similar electrochemical activity. Second, dielectric corrosion resistant coatings should be applied on the metal parts so that the electrochemical processes cannot take place.

Graphene – a One Atom Thick Corrosion Resistant Coating?

November 5, 2015Novel Materialsanti corrosion, captain corrosion, captaincorrosion, coating, corrosion, corrosion prevention, corrosion protection, graphene, graphene corrosion, graphene cvd, graphite, Maido Merisalu, material, materials science, novel material, one atom thick, science newsCaptain Corrosion

Graphene – a novel material, that consists of only a single layer of oriented carbon atoms. This material is hundreds times stronger than steel and conducts heat and electricity with exceptional efficiency. A perfect sheet of graphene could actually be so strong that it could lift even a kitten! But can this one atom thick material also be the thinnest corrosion resistant coating ever made? There have been several papers over the last decade discussing this possibility and this peaked our interest. So we first prepared graphene on larger copper substrates by chemical vapor deposition (CVD). Following Raman spectroscopy and scanning electron microscopy (SEM) studies confirmed, that we had a single layer of high quality graphene, that coated the whole substrate. Now it was time to test how well this single atom thick coating can protect the underlying copper from corrosion – for that we used chemical and electrochemical methods. According to electrochemical tests, graphene actually seemed to slow down the corrosion, but additional high resolution imaging with the scanning electron microscope revealed the terrifying truth!
Graphene had started to delaminate and the areas with exposed copper had suffered severe corrosion, unlike bare copper substrates, that corroded uniformly. This severe type of copper corrosion in the defects of graphene was actually caused by graphene itself because of localized galvanic corrosion. In this galvanic couple the large area of highly conductive graphene served as a cathode and the small area of exposed copper as an anode. As a result the copper was continuously stripped from electrons, causing it to easily react with the corrosive environment. So basically it was clear that graphene may initially seem to be a corrosion resistant barrier, but eventually the graphene coated substrate would suffer much more damage than the uncoated substrate! Also, it is impossible to create a large area graphene that has no defects where chloride ions wouldnt be able to slip through. However, it was also true that if the defects in graphene were to be fixed, the galvanic couple and corrosion would be undone. In our laboratory we sealed these small defects in graphene by electrodeposition of polypyrrole. Surprisingly this polymer deposited extremely well on such defects, sealing even holes that were several microns wide. As a result we obtained a nanocomposite coating, that consisted of graphene and polypyrrole. This coating performed well both in chemical and electrochemical corrosion tests.
So what did we learn from all this? The first thing that we learned was the fact that galvanic corrosion can effectively be stopped even at nano-scale, by blocking one of its driving reactions. Second, we discovered that the electrochemical behavior of the defects of graphene is completely different from the defect free area. Third, we realised that polypyrrole may even visualize the quality of graphene for the naked eye because polypyrrole deposits only on graphene and its defects but not on copper if the defects were too big. For example if one built a CVD (chemical vapour deposition) reactor for the preparation of 1 square meter of graphene on a copper foil, then there is a need to somehow see if the foil was actually evenly coated by graphene. By depositing polypyrrole on the graphene coated copper substrate, it is possible to see even with the naked eye if the whole substrate turns black or of there are brigher areas. If there were brighter areas on this copper foil with graphene and polypyrrole, then this would mean that in those regions we dont actually have graphene where polypyrrole could deposit. This would mean that either the gas flow or temperature in the CVD process had not been ideal.
Although things get complicated in the nano-scaled world, the processes are still governed by a set of rules. One day we’ll figure them all out and then we can truly play „dice“ at the atomic scale!

X-Ray Tube Working Principle Explained

November 5, 2015Scientific Equipmentanodeerimine, cathode, characteristic x-rays, explained, how x-ray tube works, mammography, medical, medical imaging, medicine, principle, radiation, röntgen, röntgentoru, working principle, x-ray, x-ray diffraction, x-ray fluorescence spectroscopy, x-ray imaging, X-ray photoelectron spectroscopy, x-ray radiation, x-ray tube, XPS, xray, XRD, XRFCaptain Corrosion

X-ray tubes are devices that produce x-ray radiation, which is useful in various applications. For example in medicine this high energy electromagnetic radiation is used for imaging your body. In airports x-rays are used to scan your luggage for prohibited items. X-rays can also be used for materials characterization in techniques such as x-ray fluorescence spectroscopy or photoelectron spectroscopy.
An x-ray tube consists of an anode and a cathode within a casing that can hold vacuum. The cathode is heated to high temperatures, where it starts emitting electrons – this process is known as thermionic emission. A high voltage applied between the cathode and the anode accelerates the emitted electrons towards the anode. When these high energy electrons interact with the anode some of the energy is converted into x-ray radiation and some into heat. Thats why water cooling is needed to prevent the overheating of the anode.The emitted x-ray radiation consists of two components – bremsstrahlung and characteristic x-rays. In the case of bremsstrahlung the electromagnetic radiation is emitted from the negative electron when its trajectory is changed by a positively charged atoms nucleus. This radiation has a very broad energy range. Its energy and intensity depends on the voltage between the anode and the cathode, on the cathode filaments heating current and on the atomic number of the anode material. Characteristic x-rays however have a very specific energy, which strongly depends on the anode material. This radiation is generated when the accelerated electrons excite the anode atoms by kicking out inner shell electrons. In the relaxation process a higher shell electron moves to the vacant spot and the excess energy is emitted in the form of x-rays. The energy of these characteristic x-rays depend on the binding energy of the electron that was kicked out and the binding energy of the electron that occupied the vacant spot. The generated x-rays leave the tube through a beryllium window. Beryllium is used as a window material because it doesnt absorb much of the x-rays as it has a low atomic number. Be sure to follow us in youtube for more awesome videos in the future!

How to Anodize Aluminum – Do it Yourself (DIY)

November 5, 2015Corrosion PreventionAAO, aluminium, aluminum, anidizing aluminum, anodeerimine, anodic aluminium oxide, anodizing, anodizing tips, anodizing tutorial, anti corrosion, captain corrosion, captaincorrosion, corrosion, corrosion prevention, corrosion protection, DIY, do it yourself, electrochemistry, engineering, how is done, how to, how to anodize, how to anodize aluminum, Maido MerisaluCaptain Corrosion

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.

Atomic Layer Deposition – A Method for Making Ultra-Thin Invisible Corrosion Resistant Coatings

June 26, 2015Novel Materials#CVD, 3D animation, ALD, ALD process, ALD reactor, ALDep, ALE, aluminum oxide, animation, anodic aluminium oxide, anti corrosion, Atomic Layer Deposition, Atomic Layer Epitaxy, captain corrosion, captaincorrosion, ceramic, ceramic film, chemical vapour deposition, coating, corrosion, corrosion prevention, corrosion protection, corrosion resistant, corrosion resistant coating, explained, Maido Merisalu, principle, star trek replicator, thin film, thin film technology, TiO2, titanium dioxideCaptain Corrosion

Ever thought how nice it would be if the replicator (synthesizer) from Star Trek actually existed? Assembling different materials in an atomic scale however, has been possible already for decades! This exciting technique is called „Atomic Layer Deposition“ (ALD). The deposition process is carried out in a specially designed ALD reactor, where different chemicals enter the reaction chamber one at a time and react with the substrates surface in a self limiting manner. With each deposition cycle a thin layer is deposited and by repeating the cycle thicker material layers can be obtained. An easy example would be the deposition of titanium dioxide by using titanium(IV) chloride and water as reacting chemicals (precursors) and nitrogen as carrier gas.

Although this method is not suitable for creating macroscopic objects, it can be used to significantly enhance their properties such as corrosion resistance, wetting (self cleaning surfaces) or even biocompatibility (brain chips). This method is also used in the production of some solar cells, microelectronic devices and nanostructures. The huge benefit of this method is the possibility to apply films with well defined thickness and composition even on sophisticated three-dimensional objects. This makes ALDep perfect for applying ultra thin (nanometric) corrosion resistant coatings on many small devices (including jewelery), where thick coatings cannot be used.

In order to get a better understanding of this method, watch the video above.

Sony Vegas Pro 13 Suite was used for making this video – check out their website below:
Sony Creative Software Inc.

Vacuum Systems and Technologies

May 12, 2015physics, Scientific Equipment, vacuum gauges, vacuum pumps3D animation, cryopump, diaphragm pump, diffusion pump, explained, hot filament ionization gauge, ion pump, leak finder, mass analyzer, mass spectrometer, penning ionization gauge, pirani, pirani gauge, piranimõõdik, quadrupole mass analyzer, quadrupole mass spectrometer, rotary vane pump, scanning electron microscope, scroll compressor pump, SEM, sorption pump, thermocouple gauge, titanium sublimation pump, turbomolecular pump, vaakum, vaakum-meetrid, vaakummeetrid, vaakumpumbad, vaakumpump, vaakumsüsteemid, vacuum, vacuum gauge, vacuum pump, vacuum system, working principle animation, XPSCaptain Corrosion

Vacuum can be understood as space from where matter (for example air) has been removed. It naturally exists in outer space but for certain applications, like materials characterization techniques, it needs to be achieved artificially. The desired level of vacuum is obtained with the help of a suitable vacuum pump. For example low vacuum (low quality vacuum with higher pressure) can be generated with a diffusion pump, scroll compressor pump, rotary vane pump, diaphragm pump or a sorption pump. High vacuum (high quality vacuum with very low pressures) however, can be obtained with high vacuum pumps such as the turbomolecular pump, ion pump, titanium sublimation pump and cryopump. The level of vacuum is measured with devices called vacuum gauges (vacuum meters) like the thermocouple gauge, pirani gauge, penning ionization gauge and the quadrupole mass spectrometer (analyzer). The working principle of vacuum pumps and vacuum gauges is explained with 3D animations in the video lecture above.

How to Generate Hydrogen by Splitting Water

January 6, 2015Uncategorizedalternative, ampere, anode, automobile, car, cathode, chemical, chlorine, clean, corrosion, current, dollar, electric, electricity, electrochemical, electrochemistry, electrolysis, energy, environment, EUR, euro, experiment, experimental, free, fuel, fuel cell, fusion, fusion reactor, gas, generate, generator, global, global warming, green, H, H2, H2O, HHO, how to, hydrogen, hydrogen damage, oxygen, power, reaction, solar, USD, volt, voltage, water, water splittingCaptain Corrosion

Hydrogen is the most abundant substance in the universe. It fuels the starts that light the nightsky. Hydrogen will also power the future of mankind as it is already used as car fuel and within this century even in fusion reactors.

As most of you know, a water molecule consists of one oxygen atom and two hydrogen atoms. So in order to get hydrogen, it is needed to split the water molecule. This can be done for example electrochemically where an electrical potential is applied between electrodes in a salt water. For a home experiment one can simply put a 9 V battery into salt water and watch how hydrogen bubbles start to form at the cathode. At the same time oxygen is generated at the anode but since the anode on the battery is usually made of steel, it will quickly corrode as it reacts with chlorine and oxygen. This causes the salt water to go brown. So instead, you may want to use electrodes instead that are connected to an external power source. If a DC voltage is used then especially the anode needs to be made from a chemically inert conductive material such as platinum which doesnt oxidize. At this anode oxygen gas can be collected. At the same time hydrogen gas is generated at the cathode and can also be collected. If DC voltage is used then the electrode at cathodic potentials will not corrode very quickly as oxidation cannot occur. However hydrogen damage may eventually destroy the electrode.

Hydrogen damage occurs when the small atomic hydrogen generated at the cathode moves into pores and cracks inside the electrode and combines with other hydrogen atom to form molecular hydrogen. The molecular hydrogen however is too large to diffuse through metal and starts building up inside the sealed crack or pore and pressure increases until it splits the material.

In order to produce as much gas as possible, the surface area of electrodes needs to be increased. Make the electrodes rough, multilayered or highly porous for greater surface area.

If AC voltage is used to split water, then corrosion is suppressed and for some time even stainless steel can be used as both electrodes.

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Template Synthesis of Silver Nanorods

October 13, 2014Novel MaterialsAAO, aluminium, aluminum, anodic aluminium oxide, engineering, expensive, materials science, micrometre, micron, nano, nano engineered, nano engineering, nanometre, nanoparticle, nanorod, nanotechnology, nanowire, oxide, rod, science, silver, synthesis, technology, template, template synthesis, wireCaptain Corrosion

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 Microscopy (AFM)

September 30, 2014Materials Characterization3D animation, AFM, animation, atom, atomic force microscopy, c-AFM, contact, electrostatic, engineering, force, ic-AFM, image, intermitten, magnification, materials characterization, materials science, microscopy, mode, nc-AFM, non-contact, piezo, piezoelectric effect, piezotube, scanning, scanning probe microscopy, tapping, van der waalsCaptain Corrosion

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.