Name: localized bathless metal-composite plating via electrostamping
Uploaded: 2020-09-22T12:30:00
Description: Watch this Scientific Journal Video about Localized Bathless Metal-Composite Plating via Electrostamping at JoVE.com

This work was supported by the Aircraft Equipment Reliability and Maintainability Improvement Program and the Patuxent Partnership. Townsend was supported by an ONR Faculty Research Fellowship. The authors also acknowledge the general support of the SMCM Chemistry and Biochemistry Department faculty and students, including support from the SMCM football team.

1. Preparing coating salts
CAUTION: Nickel salts and boric acid are toxic and should be handled with proper personal protective equipment including nitrile gloves, goggles and a lab coat. Strong acids and bases should be handled in the fume hood, and all waste chemicals should be disposed of as hazardous waste.
<ol>
	<li>Using a balance, weigh out the following powders in these ratios: 10.000 g of NiSO4&#183;6H2O, 2.120 g of NiCl2&#183;6H2O, 1.600 ...

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T. J., Wills, R. G. A., Walsh, F. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposition+of+composite+coatings+containing+nanoparticles+in+a+metal+deposit.">Electrodeposition of composite coatings containing nanoparticles in a metal deposit.</a> Surface and Coatings Technology. 201 (1), 371-383 (2006).</li><li>Gerwitz, C. N., David, H. M., Yan, Y., Shaw, J. P., Townsend, T. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bathless+Inorganic+Composite+Nickel+Plating:+Dry-Cell+Stamping+of+Large+Hygroscopic+Phosphor+Crystals.">Bathless Inorganic Composite Nickel Plating: Dry-Cell Stamping of Large Hygroscopic Phosphor Crystals.</a> Advanced Materials Interfaces. 7 (4), (2020).</li><li>Bite, I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Novel+method+of+phosphorescent+strontium+aluminate+coating+preparation+on+aluminum.">Novel method of phosphorescent strontium aluminate coating preparation on aluminum.</a> Materials and Design. 160 (15), 794-802 (2018).</li><li>Feldstein, M. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Coatings+with+identification+and+authentication+properties.">Coatings with identification and authentication properties.</a> US Patent. , (2012).</li><li>Rose, I., Whittingham, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nickel Plating Handbook. , (2014).</li><li>Anderson, D. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electroplating Engineering Handbook. , (1996).</li><li>Helle, K., Walsh, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposition+of+Composite+Layers+Consisting+of+Inert+Inclusions+in+a+Metal+Matrix.">Electrodeposition of Composite Layers Consisting of Inert Inclusions in a Metal Matrix.</a> Transactions of the Institute of Metal Finishing. 75 (2), 53-58 (1997).</li><li>Kerr, C., Barker, D., Walsh, F., Archer, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Electrodeposition+of+Composite+Coatings+based+on+Metal+Matrix-Included+Particle+Deposits.">The Electrodeposition of Composite Coatings based on Metal Matrix-Included Particle Deposits.</a> Transactions of the Institute of Metal Finishing. 78 (5), 171-178 (2000).</li><li>Walsh, F. C., Wang, S., Zhou, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+electrodeposition+of+composite+coatings:+Diversity,+applications+and+challenges.">The electrodeposition of composite coatings: Diversity, applications and challenges.</a> Current Opinion in Electrochemistry. 20, 8-19 (2020).</li><li>Feldstein, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Functional+coatings+comprising+light+emitting+particles.">Functional coatings comprising light emitting particles.</a> US Patent. , (1996).</li><li>Feldstein, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Composite+plated+articles+having+light-emitting+properties.">Composite plated articles having light-emitting properties.</a> US Patent. , (1998).</li><li>Zimmerman, E. 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Critical steps of electrostamping. Bathless electrostamping shares many of the same critical steps with traditional bath electroplating. These include proper cleaning of the electrodes, mixing metal ions into the electrolyte and applying and external or chemical (electroless plating) potential to cause reduction of metal onto the cathode. In addition, the oxidation of the anode and cathode should be avoided after acid activation by quickly rinsing with water and adding these electrodes to the setup.
...

Traditional electroplating is widely used to deposit thin films of a variety of metals, alloys, and metal-composites onto conductive surfaces to functionalize them for the intended application1,2,3,4,5,6,7,8,9,10,11,12. This method adds a metal finish to parts used in the manufacturing of aerospace, automotive, military, medical, and electronic equipment. &#173;&#173;&#173;&#173;The object to be plated, the cathode, is submerged in an aqueous bath containing metal salt precursors, which are reduced to metal at the surface of the object by the application of a chemical or electrical potential. Non-charged composite particles can be incorporated into the metal film by adding these to the bath during coating to enhance the film properties for increased hardness in the case of metal oxides and carbides, smoothness with polymers or lubrication with liquid oils12,13. However, because these particles lack an inherent attraction to the cathode, the ratio of composite that is incorporated into the metal remains low for bath plating13,14,15. This is especially problematic for large particles that do not adsorb to the cathode long enough to be embedded by the growing metal film. Additionally, hygroscopic particles solvate in aqueous solutions and their hydration shell acts as a physical barrier impeding contact with the cathode16.
Some promising methods have been shown to mitigate this effect by using dry non-polar solvents to remove the hydration barrier completely17, or by decorating the composite particles with charged surfactant molecules16 that disrupt the hydration shell to allow contact between the particle and the cathode. However, because these methods involve organic materials, carbon contamination is possible in the film and breakdown of these organic materials could occur at the electrodes. For example, the organic solvents used (DMSO2 and acetamide) are heated to 130 &#176;C in an inert atmosphere for air-free coating; however, we found them to be unstable during coating in air. Due to resistive heating at the electrodes, redox reactions with organic materials may result in impurities or sites for heterogeneous nucleation and growth of metal nanoparticles18. As a result, there is a need for an organic-free aqueous electroplating method that addresses the long-standing challenge of particle-cathode adsorption. So far, metal-composite bath coating has been shown to embed particles up to a few micrometers in diameter19 and as high as 15 % loading16,17.
In response to this, we describe an inorganic bathless electrostamping method that forces composite particles to become embedded into the film at high surface coverages despite their large size and hygroscopic nature20. By removing the bath, the process does not involve containers of hazardous coating liquids and the object to be plated does not need to be submerged. Therefore, large, cumbersome or otherwise corrosion- or water-sensitive objects, can be plated or &#8220;stamped&#8221; in select areas with the composite material. In addition, the removal of excess water requires less clean-up of liquid hazardous waste.
Here, we demonstrate this method to produce bright fluorescent metal films by co-depositing non-toxic and air-stable europium and dysprosium doped, strontium aluminate (87 &#177; 30 &#181;m) with nickel at high loadings (up to 80%). This comes in contrast to previous examples that were plated in a bath and therefore were limited to small (nanometers to a few micrometers) phosphors12. In addition, previously reported electrodeposited films fluoresce only under short-wave UV-light, with the exception of a recent report that grew 1 &#8211; 5 &#181;m luminescent strontium aluminate crystals in an alumina film with plasma electrolyte oxidation21. Fluorescent metal films could have far-reaching applications in many industries involving dim-light environments including road sign illumination21, aircraft maintenance equipment location and identification20, automobile and toy decorations, invisible messages, product authentication22, safety lighting, mechanochromic stress identification10 and tribological wear visual inspection12,16. Despite these potential uses for glowing metal surfaces, this method could also be expanded to include additional large and/or hygroscopic composite particles to produce a new variety of metal-composite functional coatings that were previously not possible via electroplating.

<table>
	<tbody>
		<tr>
			<td>37% M Hydrochloric Acid (aq)</td>
			<td>SigmaAldrich</td>
			<td>320331-500ML</td>
			<td>corrosive - handle in fume hood</td>
		</tr>
		<tr>
			<td>70% Nitric Acid (aq)</td>
			<td>SigmaAldrich</td>
			<td>438073-500ML</td>
			<td>corrosive - handle in fume hood</td>
		</tr>
		<tr>
			<td>Barium magnesium aluminate, europium doped (s)</td>
			<td>SigmaAldrich</td>
			<td>756512-25G</td>
			<td>fine powder</td>
		</tr>
		<tr>
			<td>Boric Acid (s)</td>
			<td>SigmaAldrich</td>
			<td>B6768-500G</td>
			<td>toxic</td>
		</tr>
		<tr>
			<td>Cotton Swab</td>
			<td>Q-tips</td>
			<td>Q-tips Cotton Swabs</td>
			<td></td>
		</tr>
		<tr>
			<td>ImageJ</td>
			<td>National Institutes of Health</td>
			<td>IJ 1.46r</td>
			<td>free software</td>
		</tr>
		<tr>
			<td>Nickel (II) chloride hexahydrate (s)</td>
			<td>SigmaAldrich</td>
			<td>223387-500G</td>
			<td>toxic</td>
		</tr>
		<tr>
			<td>Nickel (II) sulfate hexahydrate (s)</td>
			<td>SigmaAldrich</td>
			<td>227676-500G</td>
			<td>toxic</td>
		</tr>
		<tr>
			<td>Nickel foil (s)</td>
			<td>AliExpress</td>
			<td>Ni99.999</td>
			<td></td>
		</tr>
		<tr>
			<td>Nitrile gloves</td>
			<td>Fisher Scientific</td>
			<td>19-149-863B</td>
			<td></td>
		</tr>
		<tr>
			<td>nylon membrane (s)</td>
			<td>Tisch Scientific</td>
			<td>RS10133</td>
			<td></td>
		</tr>
		<tr>
			<td>Optical Microscope equipped with FTIC filter (470 &#177; 20 nm)</td>
			<td>Nikon</td>
			<td>Eclipse 80i</td>
			<td></td>
		</tr>
		<tr>
			<td>Plastic Wrap</td>
			<td>Fisher Scientific</td>
			<td>22-305654</td>
			<td></td>
		</tr>
		<tr>
			<td>Porcelain Mortar</td>
			<td>Fisher Scientific</td>
			<td>FB961A</td>
			<td></td>
		</tr>
		<tr>
			<td>Porcelain Pestle</td>
			<td>Fisher Scientific</td>
			<td>FB961K</td>
			<td></td>
		</tr>
		<tr>
			<td>Potassium Hydroxide (s)</td>
			<td>SigmaAldrich</td>
			<td>221473-25G</td>
			<td>corrosive</td>
		</tr>
		<tr>
			<td>Potentiostat with platinum wire</td>
			<td>Gamry Instruments</td>
			<td>1000E</td>
			<td></td>
		</tr>
		<tr>
			<td>Scoopula</td>
			<td>Fisher Scientific</td>
			<td>14-357Q</td>
			<td></td>
		</tr>
		<tr>
			<td>Spectrofluorometer</td>
			<td>Photon Technology International</td>
			<td>QM-40</td>
			<td></td>
		</tr>
		<tr>
			<td>Strontium aluminate, europium and dysprosium doped (s)</td>
			<td>GloNation</td>
			<td>756539-25G</td>
			<td>powder</td>
		</tr>
		<tr>
			<td>Variable linear DC power supply</td>
			<td>Tekpower</td>
			<td>TP3005T</td>
			<td></td>
		</tr>
		<tr>
			<td>Yttrium oxide, europium doped (s)</td>
			<td>SigmaAldrich</td>
			<td>756490-25G</td>
			<td>fine powder</td>
		</tr>
	</tbody>
</table>

localized bathless metal-composite plating via electrostamping

Composite plating with particles embedded into the metal matrix can enhance the properties of the metal coating to make it more or less conductive, hard, durable, lubricated or fluorescent. However, it can be more challenging than metal plating, because the composite particles are either 1) not charged so they do not have a strong electrostatic attraction to the cathode, 2) are hygroscopic and are blocked by a hydration shell, or 3) too large to remain stagnate at the cathode while stirring. Here, we describe the details of a bathless plating method that involves anode and cathode nickel plates sandwiching an aqueous concentrated electrolyte paste containing large hygroscopic phosphorescent particles and a hydrophilic membrane. After applying a potential, the nickel metal is deposited around the stagnant phosphor particles, trapping them in the film. The composite coatings are characterized by optical microscopy for film roughness, thickness and composite surface loading. In addition, fluorescence spectroscopy can be used to quantify the illumination brightness of these films to assess the effects of various current densities, coating duration and phosphor loading.

After following this protocol, a thin coating of metal should become plated onto the cathode surface and contain the composite particles that were added to the coating paste. Fluorescent or colored particle incorporation can be observed by visual inspection as a result of a change in appearance compared to the uncoated surface (Figure 1A1-A3). To investigate the percent surface coverage of the composite particles and to observe the surface morphology of the coating, optical ...

Watch this Scientific Journal Video about Localized Bathless Metal-Composite Plating via Electrostamping at JoVE.com

Localized Bathless Metal-Composite Plating via Electrostamping

Presented here is a protocol of bathless electroplating, where a stagnant metal salt paste containing composite particles are reduced to form metal composites at high loading. This method addresses the challenges faced by other common forms of electroplating (jet, brush, bath) of embedding composites particles into the metal matrix.

Composite plating with particles embedded into the metal matrix can enhance the properties of the metal coating to make it more or less conductive, hard, ...

Electro stamping works by trapping composite particles in the electrolyte, forcing them to plate with the metal. With this new technique, high composite particle loadings are possible even on water sensitive objects. Unlike typical electroplating, this technique does not require submerging the object in a liquid bath.Any conductive object, regardless of its size or shape. Can be coated with functional materials. Fluorescent metal composite coatings have far reaching applications for dim light environments including aircraft maintenance equipment location, road sign illumination and travel logical markings in mechanically machine parts.To begin weigh nickel sulfate, nickel chloride hexahydrate and boric acid as mentioned in the text manuscript and combine them in a vial together. Grind this salt mixture thoroughly to a fine powder. Make sure to use proper protective equipment, fume hoods and a hazardous waste disposal system.Next, Weigh 1.8 grams of europium dysprosium doped strontium aluminate, europium doped yttrium oxide or europium doped barium, magnesium aluminate and grind it into a fine powder using a porcelain mortar and pestle for approximately 10 minutes. Combine the ground composite powder with the salt mixture in a container for storage. Weigh 0.188 grams of this mixture per square centimeter of the coating area and add it to an open top container add 40 microliters of water per square centimeter of coating area to this mixture and stir to dissolve the salt and form a thick paste.Using a scissor, cut the anode to a size and shape that matches the object to be plated in order to remove organic material from the surface of the anode foil and the cathode clean it with 10 Mueller potassium hydroxide or sodium hydroxide using a cotton swab or cloth. Rinse the surface with water to remove the excess base then activate the metal surface to receive the coating by wiping it with a selective concentrated acid using a cotton swab or cloth, following the recommendations for activating specific metal surfaces and alloys. perform this in the fume hood to avoid exposure to hydrogen chloride vapors quickly deposit the prepared coating paste onto the cathode object, covering the entire area and making sure to avoid gaps.Activate the anode surface by wiping it with concentrated acid using a cotton swab or cloth. If calculation of current efficiency is required record the mass of the anode and cathode using an analytical balance. preset a power supply to the desired current or voltage mode.Cut a piece of a hydrophilic membrane such as a nylon sheet and place it on top of the anode coating paste to avoid direct contact with the cathode. Add a small amount of paste or dry salt mixture onto the sheet. Next, add two drops of water to partially dissolve the salt.This process makes the nylon sheet conductive to allow the mass transport of ions through the electrolyte which is necessary to balance charge in the coating reaction. This can also be accomplished by dipping the nylon membrane in an aqueous nickel salt mixture. Place the activated anode on top and attach both the negative and positive leads to the cathode object.Cover the entire system with plastic to help retain water and apply moderate pressure. Turn on the power supply and continue coating for a desired duration. Turn off the power supply and expose the system.Disconnect the leads and rinse the cathode object with water wash the other components of the system by soaking them in water and then discard this aqueous solution in the properly labeled hazardous waste container. To remove any uncoated composite particles gently rubbed the cathode object by hand wearing gloves. Record the mass of the anode and cathode using an analytical balance and calculate the difference with their original mass.Observe fluorescent coatings with an ultraviolet lamp to verify the brightness and consistency of the metal composite. Use chronopotentiometry to monitor changes in voltage under constant current and chronoamperometry to monitor changes in current under constant voltage. Turn on the potential stud and designate the duration and the applied current or voltage.prepare the coating as previously described. Normalize the voltage to a reference standard using a calibrated three electrode system. Place a platinum wire as a pseudo reference electrode between the anode and the nylon sheet.And to cover it with a separate nylon sheet to avoid contact. Deposit a few drops of water and a small amount of coating paste on the anode. Finally connect the leads to the electrodes then seal press and begin coating as described in the text manuscript.Monitor the changes in voltage or current. Fluorescent or colored particle incorporation can be observed due to a change in appearance compared to the uncoated surface. Optical microscopy was used to investigate the surface coverage and to observe the surface morphology of the coating.Samples were observed top-down or cut to reveal the cross section the percent composite particle surface coverage as a function of time for Chronoamperometry and as a function of current density for chronopotentiometry increases during coating. Surface coverage is also correlated with thickness. Coating parameters can be monitored under constant voltage using chronoamperometry and under constant current using chronopotentiometry The brightness of the metal composite coatings was quantified with fluorescent spectroscopy and the calculation for luminescence quantum yield was done using the ratios of the peak areas.When attempting this protocol, it is important to properly clean and activate the electrodes before coating. In addition, thoroughly grinding the precursor electrolyte mixture will help lead to a smooth even coating. The precursor composite electrolyte paste can also be deposited by spray coating or powder coating to save time and materials.This way objects can be coated at a larger scale. This new technique may stimulate scientific exploration to incorporate other large or hygroscopic composite particles which were previously incompatible with bath, jet or brush plating.

Research

JoVE Journal

Chemistry

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The ...

Fluorescence-based Monitoring of PAD4 Activity via a Pro-fluorescence Substrate Analog

Post-translational modifications may lead to altered protein functional states by increasing the covalent variations on the side chains of many protein ...

Facile and Efficient Preparation of Tri-component Fluorescent Glycopolymers via RAFT-controlled Polymerization

Synthetic glycopolymers are instrumental and versatile tools used in various biochemical and biomedical research fields. An example of a facile and ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Synthesizing Sodium Tungstate and Sodium Molybdate Microcapsules via Bacterial Mineral Excretion

We present a method, the bacterial mineral excretion (BME), for synthesizing two kinds of microcapsules, sodium tungstate and sodium molybdate, and the ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Membrane Remodeling of Giant Vesicles in Response to Localized Calcium Ion Gradients

In a wide variety of fundamental cell processes, such as membrane trafficking and apoptosis, cell membrane shape transitions occur concurrently with local ...