The overall goal of this procedure is to prepare ordered metal nanofoams, starting from a supramolecular complex, polystyrene block poly for vinyl purine penedes LPH phenol. This is accomplished by first selecting the appropriate system parameters that would give rise to the double gyro morphology in supramolecular complexes. The second step is to selectively remove one component of the complex, namely penad sylph phenol, which forms part of the gyro matrix.
Next, the porous template is backfilled with nickel via an electros plating procedure. The final step is removal of the remaining polymer by pyrolysis at 350 degrees Celsius. Ultimately, block co-polymer template directed synthesis is used to generate well ordered nano porous metal foams with inverse gyro morphology.
So the main advantage of this technique over existing methods is that we are able in a straightforward way to obtain a double GY morphology in blocker polymers. After that, once we have a double gyre morphology, we can take our sample, soak it in ethanol, and then remove Amphiphilic pandaol in a very simple way. Then when we have apor structure, we do electroless metal plating to insert metal into a complex PO pathways in a such a way, obtain metal nanofoam at the end.
This method provides an intuitive way to form ordered nano porous networks from a wide variety of metals. First dissolve polystyrene block poly for vinyl purine and penedes phenol in chloroform, and stir the solution for a couple of hours at room temperature. Pour the solution into a glass petri dish, then place the dish into a saturated chloroform atmosphere.
After approximately one week, remove the Petri dish from the saturated chloroform atmosphere. Dry the supramolecular complex film in a vacuum at 30 degrees Celsius overnight. After removing the film from the oven, place it in a specially designed container.
Then remove the air from the container and fill it with nitrogen when finished. Ane the film for four days in the oven at 120 degrees Celsius under nitrogen atmosphere with one bar over pressure. Once the an kneeling process is complete, cut a small piece of the film and embed it in epoxy.
Then cure the sample overnight at 40 degrees Celsius. Microtome the sample to a thickness of about 80 nanometers using a diamond knife at room temperature. Place the micro toed sections on copper grids.
Following this transfer, the grids containing the microtome sections to a jar with iodine. After 45 minutes, remove the stained samples. In preparation for TEM, insert the copper grids with stained sections in the transmission electron microscope.
Operating at an accelerating voltage of 120 kilovolts and image the sample. Then insert a piece of a kneeled film into the sample holder for sacks and fix it with cap on tape. Place the prepared sample holder into the machine.
Open the x-ray shutter and acquire the 2D scattering pattern. At this point, immerse another small piece of a kneeled film in ethanol for three days. Once the porous film has been dried, immerse it in an aqueous solution of tin chloride for one hour.
After removing the film from the solution, rinse it thoroughly with deionized water. Next, immerse the film in an aqueous solution of palladium chloride. After one hour, remove the film from the solution and rinse it with deionized water.
To prepare the nickel plating bath, mix a nickel sulfate hexahydrate solution with a Bo dimethyl amine complex solution at a four to one ratio and adjust the pH to seven. Using ammonium hydroxide, immerse the film in the nickel plating bath for one hour. After rinsing with deionized water, dry the film in a fume hood.
After prepare the plated sample for electron microscopy as previously described. Image it using the same conditions as before. Following this place the nickel plated film in an oven at 350 degrees Celsius for one hour to four days.
Once the film has cooled to room temperature, attach it to the sample holder using a silver paste. Then insert the sample holder into the scanning electron microscope. Acquire SEM micrographs and perform EDX analysis.
Double wave and wagon wheel. Gyro patterns represent projections through the 2 1 1 and 1 1 1 plane of the gyro unit cell respectively. Polystyrene block domains appear bright while poly.
Four vinyl purine pentyl phenol block domains appear dark from iodine. Staining the double wave pattern of another sample shows a periodicity decrease sax peaks at square root of six Q star square root of eight QStar square root of 14 QStar square root of 22 QStar and square root of 50 QStar. Confirm the bi continuous IA 3D morphology after ethanol treatment.
Penad sylph phenol proton NMR signals are absent. DSC data imply that the thermal behavior of the ethanol treated sample and DI block copolymer is identical. The porous gyro template has a high BET specific surface area of 104 square meters per gram and occupies almost 60 volume percent.
The average pore diameter is 40 nanometers with narrow pore size distribution. The contrast in the unstained nickel plate gyro, TEM micrograph originates from metal deposited in the nano channels. The wagon wheel pattern confirms preservation of the double gyro morphology.
High resolution TEM Micrographs show large interconnected nickel crystalite and EDX analysis reveals the plated sample. Chemical composition. Carbon nickel and oxygen peaks are observed, which indicates oxidation of the nickel nanofoam when stored in air.
The nickel network remains intact during polymer decomposition by isothermal heating. The exposed nickel replica preserves the inverse gyro morphology as confirmed by SEM. Using the method that we've just shown, we were able to obtain and to characterize highly ordered metal nanofoams.
These highly ordered metal nanofoams can potentially be used as actuators. This method opens a path for the investigation of the differences in the behavior of ordered and disordered nano porous metals. Don't forget that working with chemicals used for electrodes, metal plating can be extremely hazardous and one should always use personal protective equipment when performing this procedure.
