We acknowledge financial support by the Zernike Institute for Advanced Materials, University of Groningen.

1. Preparation and Characterization of PS-b-P4VP(PDP) Complexes with Double Gyroid Morphology
<ol>
	<li>Weigh out polystyrene-block-poly(4-vinylpyridine) (PS-b-P4VP) and pentadecylphenol (PDP, Mr = 304.51 g/mol). In order to obtain the gyroid morphology, carefully select the amount of PDP should be (the weight fraction of P4VP(PDP) block (fP4VP(PDP))should be ca. 0.6 according to the phase diagram of linear AB diblock copolymers). Usually, 0.15-0.2 g of...

<ol>
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The authors declare no competing financial interests.

Supramolecular complexes are successfully applied as precursors for well-ordered metal nanofoams. In this method, the crucial step is to acquire the appropriate template, i.e.&#160;a template with gyroid morphology. In the phase diagram of block copolymers the gyroid region is very small and it is rather difficult to target. This means that if conventional block copolymers are used as starting materials, the quite elaborate synthesis has to be repeated until the desired composition, that gives rise to the gyroid...

There are several techniques available for the preparation of metal nanofoams: dealloying1-3, sol-gel approaches4,5, nanosmelting6,7, and combustion synthesis8. In the dealloying process, the starting material is usually a binary alloy, for example, an alloy of silver and gold. The less noble metal, silver in this case, can be removed either chemically or electrochemically resulting in a disordered porous gold foam with nanosized ligaments. In combustion synthesis, metal is mixed with an energetic precursor that releases energy during its decomposition and drives the formation of metal nanofoam8. Studies on the mechanical behavior of metal foams indicate that in disordered architectures stresses cannot be transmitted effectively from the ligament nanoscale to the overall macroscale9-11.&#160;Thus well-ordered metal nanofoams are expected to have superior mechanical properties in comparison to the disordered ones.
The idea represented here is to employ block copolymers that self-assemble into ordered nanostructures as precursors to metal nanofoams. Depending on the composition of a block copolymer, the total number of monomer units and the extent of repulsion between the chemically connected blocks, various morphologies appear such as: spherical, cylindrical, lamellar, double gyroid, hexagonally perforated lamellar, and others12-14. Furthermore, polymer blocks can be degraded selectively leading to nanoporous materials15. The most common methods include: ozonolysis16-18, UV irradiation19, reactive ion etching20-22, and dissolution23-26. The generated porous structures can be backfilled with various inorganic materials. Metal oxides (e.g.&#160;SiO2, TiO2) are usually introduced via sol-gel method into the template&#39;s channels27-29. Electrochemical and electroless plating are commonly used to deposit metal into or onto templates30-33. Finally, the remaining polymer can be removed from the polymer/inorganic nanohybrid via pyrolysis2, dissolution34,35, UV degradation28,29, etc.
In our approach, we start from a supramolecular complex of polystyrene-block-poly(4-vinylpyridine) (PS-b-P4VP) diblock copolymer and amphiphilic pentadecylphenol (PDP) molecules. This complex is a result of the hydrogen bonding between PDP and pyridine rings (Figure 1a). The composition of the starting block copolymer and the amount of added PDP are chosen in such a way that the obtained system self-assembles in the bicontinuous double gyroid morphology with a PS network and a P4VP(PDP) matrix (Figure 1b). PDP molecules become selectively dissolved in ethanol and P4VP chains collapse onto the PS network (Figure 1c). Subsequently, using electroless plating method, nickel is deposited into the pores of the template (Figure 1d). After the removal of the remaining polymer via pyrolysis, a well-ordered gyroid nickel nanofoam is obtained (Figure 1e).

<table border="1">
 <tbody>
 <tr>
 <td>REAGENTS:</td>
 <td></td>
 <td></td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP, CAS: 26222-40-2</td>
 <td>Polymer Source Inc.</td>
 <td>P9009-S4VP 
 P136-S4VP 
 P5462-S4VP 
 P3912-S4VP</td>
 <td>additional information are provided in a separate table</td>
 </tr>
 <tr>
 <td>PDP</td>
 <td>Aldrich</td>
 <td>P4402-100G-A</td>
 <td>recrystallized twice from petroleum ether</td>
 </tr>
 <tr>
 <td>SnCl2</td>
 <td>Acros Organics</td>
 <td>196981000</td>
 <td></td>
 </tr>
 <tr>
 <td>PdCl2</td>
 <td>Aldrich</td>
 <td>76050</td>
 <td></td>
 </tr>
 <tr>
 <td>NiSO4 x H2O</td>
 <td>Sigma-Aldrich</td>
 <td>227676</td>
 <td></td>
 </tr>
 <tr>
 <td>lactic acid</td>
 <td>Aldrich</td>
 <td>W261106</td>
 <td></td>
 </tr>
 <tr>
 <td>citric acid trisodium salt</td>
 <td>Sigma-Aldrich</td>
 <td>C3674</td>
 <td></td>
 </tr>
 <tr>
 <td>borane dimethyl amine complex</td>
 <td>Aldrich</td>
 <td>180238</td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP catalogue number</td>
 <td>Mn (PS), g/mol</td>
 <td>Mn(P4VP), g/mol</td>
 <td>PDI</td>
 </tr>
 <tr>
 <td>P9009-S4VP</td>
 <td>24000</td>
 <td>9500</td>
 <td>1.1</td>
 </tr>
 <tr>
 <td>P136-S4VP</td>
 <td>31900</td>
 <td>13200</td>
 <td>1.08</td>
 </tr>
 <tr>
 <td>P5462-S4VP</td>
 <td>37500</td>
 <td>16000</td>
 <td>1.3</td>
 </tr>
 <tr>
 <td>P3912-S4VP</td>
 <td>41500</td>
 <td>17500</td>
 <td>1.07</td>
 </tr>
 </tbody>
</table>

gyroid nickel nanostructures from diblock copolymer supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, have high porosity, high surface-to-volume and strength-to-weight ratio. Unfortunately, common approaches for preparation of metallic nanostructures render materials with highly disordered architecture, which might have an adverse effect on their mechanical properties. Block copolymers have the ability to self-assemble into ordered nanostructures and can be applied as templates for the preparation of well-ordered metal nanofoams. Here we describe the application of a block copolymer-based supramolecular complex - polystyrene-block-poly(4-vinylpyridine)(pentadecylphenol) PS-b-P4VP(PDP) - as a precursor for well-ordered nickel nanofoam. The supramolecular complexes exhibit a phase behavior similar to conventional block copolymers and can self-assemble into the bicontinuous gyroid morphology with two PS networks placed in a P4VP(PDP) matrix. PDP can be dissolved in ethanol leading to the formation of a porous structure that can be backfilled with metal. Using electroless plating technique, nickel can be inserted into the template&#39;s channels. Finally, the remaining polymer can be removed via pyrolysis from the polymer/inorganic nanohybrid resulting in nanoporous nickel foam with inverse gyroid morphology.

The morphology of supramolecular complexes PS-b-P4VP(PDP)x is examined by TEM and SAXS. Figures 2a and 2b display typical gyroid patterns of a representative supramolecular complex: the double-wave and the wagon-wheel patterns that are known to represent projections through the (211) and the (111) plane of the gyroid unit cell, respectively. The PS block domains appear bright while the P4VP(PDP)x block domains appear dark due to iodine staining. Figure 2c repres...

Watch this Scientific Journal Video about Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules at JoVE.com

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

This article describes the preparation of well-ordered nickel nanofoams via electroless metal deposition onto nanoporous templates obtained from self-assembled diblock copolymer based supramolecules.

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

gyroid-nickel-nanostructures-from-diblock-copolymer-supramolecules

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12.3K visualizações.  University of Groningen.  Este artigo descreve a preparação de nanofoams níquel bem ordenadas por deposição química de metal para modelos nanoporous obtidos a partir supramoléculas base de copolímeros diblock auto-montados. 