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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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. 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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, ...

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