Name: Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition (Video) | JoVE Journal
Uploaded: 2015-12-21T15:00:00.000+00:00
Duration: 7 min 37 s
Description: Learn to prepare macroporous epitaxial quartz films on silicon using chemical solution deposition and dip-coating. This versatile method enables piezoelectric thin films for advanced sensing and electromechanical device applications.

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5 minutes

This work was partially funded by a PEPS project of Cellule Energie INSIS-CNRS (1D-RENOX) to ACG and the Spanish Government (MAT2012-35324 and PIE-201460I004).

1. Preparation of the Sol
<ol>
	<li>Prepare a solution of prehydrolyzed tetraethyl orthosilicate (TEOS) the day before the preparation of the gel films in a fume hood in which a lab balance and a magnetic stirrer are placed. In this step and throughout the protocol wear a lab coat, gloves and safety goggles.
	<ol>
		<li>In a 50 ml beaker containing a Teflon coated magnetic stirring bar weigh 1.68 g of CTAB, add 48.13 ml of ethanol and 3.00 ml of HCl 35%, cover the beaker with a watch glass and stir until the CTAB is completely dissolved.</li>
		<li>Add 7.37 ml of TEOS to the beaker dropwise (at a rate of about 1-2 drops per second) while stirring, cover the flask with a watch glass and let it stir O/N.</li>
	</ol>
	</li>
	<li>The next day, prepare a 1 M aqueous solution of Sr2+. Perform this and the following steps just before the preparation of the gel films because an aged solution is prone to re-precipitation of the Sr salt.
	<ol>
		<li>Weigh 6.6654 g of SrCl2&#183;6H2O into a 25 ml volumetric flask.</li>
		<li>Add ultrapure water (e.g., Milli-Q) up to 25 ml (meniscus tangent to the flask mark) and close the flask with a plastic cap and gently shake the flask to dissolve the strontium chloride.</li>
	</ol>
	</li>
	<li>Add 2 ml of the 1 M aqueous solution of Sr2+ to the 50 ml glass beaker containing the sol that was left stirring O/N. Stir the solution for 25 min.</li>
	<li>Dispose the residues that have been eventually generated according to the safety and environment protection protocols of the lab.</li>
</ol>
2. Gel Film Deposition on Si(100) Substrates
<ol>
	<li>Preparation of the substrates
	<ol>
		<li>Cut Si slabs of about 2 cm by 5 cm out of a 2-inch p-type (100) silicon wafer with a thickness of 200 micron by cleaving the wafer in a direction parallel or perpendicular to the wafer flat using a diamond tip or a sharp-edged object. Perform this step in advance, for instance the day before the deposition of the gel films.</li>
		<li>Just before the deposition of the gels, clean the substrates with ethanol and let them dry or use a nitrogen flow or compressed air to accelerate the drying. Perform this step while waiting for the completion of step 1.3.</li>
	</ol>
	</li>
	<li>Coat the films. In order to obtain a homogeneous macropore structure perform this step under conditions of relative humidity between 20% and 55% at RT.
	<ol>
		<li>Establish a dip coating sequence. Select the initial and final positions taking into account the actual length of the Si slab and the level of the solution in the beaker so that the slab is at least 2 cm above the solution level at the starting position and 1 cm above the bottom of the beaker at the end of the immersion. Set both the immersion and withdrawal speeds to 150 mm/min. Set the immersion time (time at the final position) to zero.</li>
		<li>Upon completion of step 1.3 place the beaker with the solution in a well-centered position beneath the Si slab hanging from the dip-coater arm.</li>
		<li>Fix one end of the Si slab to the dip-coater arm with the clip, ensuring the slab is as perpendicular as possible with respect to the horizontal.</li>
		<li>Execute the dip coating sequence and unclip the Si slab from the dip-coater arm. Repeat steps 2.2.3 and 2.2.4 with additional Si slabs to produce more films, taking care not to extend these preparations beyond 1 hr, to ensure that the stability of the solution is not compromised.</li>
	</ol>
	</li>
	<li>Dispose the solutions that have been eventually generated according to the safety and environment protection protocols of the lab.</li>
</ol>
3. Gel Film Crystallization by Thermal Treatment
<ol>
	<li>Thermal treatment of the gel films on Si(100).
	<ol>
		<li>Program a furnace to perform the following thermal treatment in air atmosphere: heating from RT to 1,000 &#176;C at 3 &#176;C/min, holding at 1,000 &#176;C for 5 hr and cooling to RT at 3 &#176;C/min.</li>
		<li>Place the dip-coated Si substrates in an alumina boat, introduce it in the furnace and execute the thermal treatment.</li>
	</ol>
	</li>
	<li>Cleaning of the crystallized films.
	<ol>
		<li>Immerse the crystallized films for 3 hr in concentrated HNO3 in order to remove the accumulations of Sr2+ that have been expulsed to the film surface during the crystallization and then rinse the films first with deionized water and then with ethanol.</li>
	</ol>
	</li>
</ol>

<ol><li>Esser, A. T., Smith, K. C., Gowrishankar, T. R., Vasilkoski, Z., Weaver, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Mechanisms+for+the+intracellular+manipulation+of+organelles+by+conventional+electroportation%5BTitle%5D)+AND+%22Biophys.+J%22%5BJournal%5D)">Mechanisms for the intracellular manipulation of organelles by conventional electroportation.</a> Biophys. J. 98 (11), 2506-2514 (2010).</li>
<li>Stava, E., Yu, M., Shin, H. C., Shin, H., Kreft, D. J., Blick, R. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Rapid+fabrication+and+piezoelectric+tuning+of+micro-+and+nanopores+in+single+crystal+quartz%5BTitle%5D)+AND+%22Lab+Chip%22%5BJournal%5D)">Rapid fabrication and piezoelectric tuning of micro- and nanopores in single crystal quartz.</a> Lab Chip. 13 (1), 156-160 (2013).</li>
<li>Varshneya, A. K. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aVarshneya%2C+AK+%22Fundamentals+of+Inorganic+Glasses%22">Fundamentals of Inorganic Glasses</a>. , Academic Press. San Diego. (1994).</li>
<li>Christov, M., Kirov, G. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((The+ratio+of+dissolving+surface+area%2Fgrowing+surface+area+in+the+hydrothermal+growth+of+quartz%5BTitle%5D)+AND+%22J.+Cryst.+Growth%22%5BJournal%5D)">The ratio of dissolving surface area/growing surface area in the hydrothermal growth of quartz.</a> J. Cryst. Growth. 131 (3-4), 560-564 (1993).</li>
<li>Bertone, J. F., Cizeron, J., Wahi, R. K., Bosworth, J. K., Colvin, V. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Hydrothermal+synthesis+of+quartz+nanocrystals%5BTitle%5D)+AND+%22Nano+Lett%22%5BJournal%5D)">Hydrothermal synthesis of quartz nanocrystals.</a> Nano Lett. 3, 655-659 (2003).</li>
<li>Jiang, Y., Brinker, C. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Hydrothermal+synthesis+of+monodisperse+single-crystalline+alpha-quartz+nanospheres%5BTitle%5D)+AND+%22Chem.+Comm%22%5BJournal%5D)">Hydrothermal synthesis of monodisperse single-crystalline alpha-quartz nanospheres.</a> Chem. Comm. 47 (26), 7524-7526 (2011).</li>
<li>Okabayashi, M., Miyazaki, K., Kono, T., Tanaka, M., Toda, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Preparation+of+Spherical+Particles+with+Quartz+Single%5BTitle%5D)+AND+%22Chem.+Lett%22%5BJournal%5D)">Preparation of Spherical Particles with Quartz Single.</a> Chem. Lett. 34 (1), 58-59 (2005).</li>
<li>Carretero-Genevrier, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Soft-Chemistry-Based+Routes+to+Epitaxial+%CE%B1-Quartz+Thin+Films+with+Tunable+Textures%5BTitle%5D)+AND+%22Science%22%5BJournal%5D)">Soft-Chemistry-Based Routes to Epitaxial α-Quartz Thin Films with Tunable Textures.</a> Science. 340 (6134), 827-831 (2013).</li>
<li>Brinker, C. J., Clem, P. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Quartz+on+Silicon%5BTitle%5D)+AND+%22Science%22%5BJournal%5D)">Quartz on Silicon.</a> Science. 340 (6134), 818-819 (2013).</li>
<li>Brinker, C. J., Lu, Y., Sellinger, A., Fan, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Evaporation-Induced+Self-Assembly%3A+Nanostructures+Made+Easy%5BTitle%5D)+AND+%22Adv.+Mater%22%5BJournal%5D)">Evaporation-Induced Self-Assembly: Nanostructures Made Easy.</a> Adv. Mater. 11 (7), 579-585 (1999).</li>
<li>Griffith, C. S., Sizgek, G. D., Sizgek, E., Scales, N., Yee, P. J., Luca, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Mesoporous+Zirconium+Titanium+Oxides.+Part+1%3A+Porosity+Modulation+and+Adsorption+Properties+of+Xerogels%5BTitle%5D)+AND+%22Langmuir%22%5BJournal%5D)">Mesoporous Zirconium Titanium Oxides. Part 1: Porosity Modulation and Adsorption Properties of Xerogels.</a> Langmuir. 24 (21), 12312-12322 (2008).</li>
<li>Lu, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Continuous+formation+of+supported+cubic+and+hexagonal+mesoporous+films+by+sol-gel+dip-coating%5BTitle%5D)+AND+%22Nature%22%5BJournal%5D)">Continuous formation of supported cubic and hexagonal mesoporous films by sol-gel dip-coating.</a> Nature. 389 (6649), 364-368 (1997).</li>
<li>Drisko, G. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Water-Induced+Phase+Separation+Forming+Macrostructured+Epitaxial+Quartz+Films+on+Silicon%5BTitle%5D)+AND+%22Adv.+Funct.+Mater%22%5BJournal%5D)">Water-Induced Phase Separation Forming Macrostructured Epitaxial Quartz Films on Silicon.</a> Adv. Funct. Mater. 24 (35), 5494-5502 (2014).</li>
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The authors have nothing to disclose.

The presented method is a bottom-up approach to produce macroporous quartz films on Si. Compared to the standard method of production of quartz films, a top down technology based on cutting and polishing of large hydrothermally grown crystals, the method described in the protocol allows obtaining much thinner films with thicknesses between 150 and 450 nm which can be controlled with the withdrawal rate. All experimental details regarding the control of quartz films thickness, and piezoelectric response are reported in re...

When a piezoelectric material like &#945;-quartz is submitted to a voltage bias it undergoes a mechanical deformation. If this material is porous, these volume changes can lead to pore expansion or contraction, creating a responsive system similar to what may be observed in living biological organelles.1 Deformable porous &#945;-quartz has been produced using microfabrication,2 but such techniques cannot yet produce 3-D pore structures, and pore diameters are on the order of hundreds of nanometers. Crystallization of structured amorphous silica has been hindered by inhomogeneous nucleation caused by high surface energies and architectural deformation due to coarsening and melting. Moreover, since all forms of silica are built upon extremely stable SiO4 tetrahedral networks, the free energies of formation of amorphous silica, &#945;-quartz and other SiO2 polymorphs are nearly equal in a wide range of temperatures, making it difficult to produce &#945;-quartz as a single polymorph from the crystallization of an amorphous silica gel.3 Another aspect that makes harder the controlled crystallization of structured amorphous silica is that quartz presents a relatively slow nucleation rate but an extremely fast growth rate, reported between 10-94 nm/sec.4,5 Slow nucleation coupled with fast growth tends to generate crystals much larger than the original nanoporous structure, thus the original morphology is lost. Alkali metals, such as Na+ and Li+, have been used to crystallize &#945;-quartz, frequently in combination with hydrothermal treatment.5,6 Also, a Ti4+/Ca2+ combination was employed to crystallize spherical particles of silica into quartz by a soft chemistry route using silicon alcoxides.7 However, the controlled crystallization of a structured amorphous silica film into quartz remained a challenge.
Recently, strontium has been found to catalyze the nucleation and growth of crystalline SiO2 under ambient pressure and relatively low temperatures.8,9 Epitaxy, arises from the favorable mismatch between &#945;-quartz and the &#60;100&#62; silicon substrate, producing oriented piezoelectric thin films. Evaporation-induced self-assembly to produce mesoporous silica films has been used since 1999.10 This technique has been studied and applied to a multitude of templating agents under various conditions to produce pores of variable sizes and mesophases. It has been found that subnanometric changes in mesopore size can have a dramatic effect on solute diffusion through porous systems11, validating this extensive attention to pore structure. Moreover, accessibility to the internal silica pore system can be obtained by controlling the micellar phase of the template.12
Here, the synthesis route that allows unprecedented control over the thickness and pore size of amorphous silica layers using a novel phase separation is demonstrated.13 These films are infiltrated with Sr(II) salts and crystallized to &#945;-quartz at 1,000 &#176;C under air at ambient pressure. The pore size retainable using this crystallization process is determined, and the effect of wall thickness and film thickness is studied. Finally the piezoelectricity and the deformability of the pore system are studied.

<table><tbody><tr><td>Dip coater</td><td>Nadetech&amp;nbsp;</td><td>ND-DC 11/150&amp;nbsp;</td><td></td></tr><tr><td>Furnace</td><td>Nabertherm&amp;nbsp;</td><td>R 50/250/12</td><td></td></tr><tr><td>Atomic Force Microscope</td><td>Agilent&amp;nbsp;</td><td>5500 LS</td><td></td></tr><tr><td>Silicon wafers</td><td>SHE Europe Ltd.</td><td></td><td></td></tr><tr><td>SrCl&lt;sub&gt;2&lt;/sub&gt;&amp;middot;6H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Aldrich</td><td>13909</td><td></td></tr><tr><td>CTAB</td><td>Aldrich</td><td>H5582</td><td></td></tr><tr><td>Ethanol Absolute&amp;nbsp;</td><td>Aldrich</td><td>161086</td><td></td></tr><tr><td>HCl 35% solution</td><td>PanReac</td><td>721019</td><td></td></tr><tr><td>TEOS</td><td>Aldrich</td><td>131903</td><td></td></tr></tbody></table>

preparation of macroporous epitaxial quartz films on silicon by chemical solution deposition

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

The progress of the material synthesis was controlled by monitoring different aspects. After the dip-coating process one can observe the aspect of the films, the eventual appearance of diffraction structures in the reflected spot of a green laser and the Scanning Electron Microscopy (SEM) images in backscattered electrons mode (Figure 1A-B). After the crystallization process it is important to record Atomic Force Microscopy (AFM) topographic images (Figure 1C</str...

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

The overall goal of this synthesis is to prepare thin epit taxal films of quartz on silicon substrates, which is important to achieve a nanoscale bottom-up integration of two relevant materials for the information and sensing technologies. The main motivation of this work was to achieve a Pentax integration of two technologically relevant materials. This is the first time that direct integration of Quas on silicone was achieved using soft chemistry.This methodology is highly versatile since it's produced meso, porous, and macroporous who are thin films, which is very advantages for sensing a Catholic and catalytic applications. The Pazo electrical properties of these thin core films are appealing for making electromechanical sensor devices as high resonance frequencies are expected for themes with things is not exceeding one micron First weigh 1.68 grams of subtle trimethyl ammonium bromide, 48.13 milliliters of ethanol. That is 37.90 grams and three milliliters of 35%hydrochloric acid.That is 3.67 grams in a 100 milliliter beaker containing a Teflon coated magnetic stirring bar. Cover the beaker with a watch glass and stir until the subtle trimethyl ammonium bromide is completely dissolved. Add 7.37 milliliters of tetraethyl ortho silicate.That is 6.88 grams to the beaker dropwise then cover the flask with a watch glass and let the solution stir overnight. The next day. Prepare a one molar st strontium chloride hexahydrate solution by dissolving 6.6654 grams of strontium chloride hexahydrate salt in milli Q water in a 25 milliliter erlenmeyer flask.Gently shake the flask with a small volume of Milli Q water to dissolve the strontium salt. Once the strontium chloride hexahydrate salt is completely dissolved, fill the flask with Milli Q water and close it with a plastic cap. Next, add two milliliters of the one molar aqueous strontium, two plus solution to the 100 milliliter glass beak containing the solution that was left stirring overnight.Stir the solution for 25 minutes. To prepare the substrates. Cut silicon slabs of about two centimeters by five centimeters out of a two inch P type silicon.1 0 0 wafer with a thickness of 200 microns by cleaving the wave in a direction. Parallel the wafer flat just before the deposition of the gels. Clean the substrates with ethanol, then use a compressed nitrogen flow to accelerate the drying process.Following this, establish a dip coating sequence by selecting the initial and final positions, taking into account the silicon slab length and the solution level so that the slab is at least two centimeters above the solution at the starting position and one centimeter above the bottom of the beaker. At the end of the immersion set the immersion and withdrawal speeds to 150 milliliters per minute and the immersion time to zero. After the solution has been prepared, place the beaker with the solution in a well-centered position beneath the silicon slab hanging from the dip coder arm.Next, execute the dip coating sequence. When finished, unclip the silicone slab from the dip coder arm. At this point, program a furnace to perform the following thermal treatment in air atmosphere.Place the dip coated silicone substrates in an Illumina boat and place it in the furnace. Then execute the thermal treatment following thermal treatment. Immerse the crystallized films for three hours in concentrated nitric acid in order to remove the accumulations of strontium, two plus that have been exposed to the film surface during the crystallization.Finally, rinse the films first with deionized water and then with ethanol after deposition. The bluish greenish appearance of the substrate is indicative of good distribution of strontium two plus over the film. If the phase separation has occurred and presents a periodicity close to that of the laser wavelength, diffraction spots can be observed.A straightforward examination of the material reveals a phase separation resulting in a macro pore structure and a strontium two plus distribution at the edge of the macro pores. This scanning electron microscopy field emission image reveals to what extent the initial macroporous structure has been preserved upon crystallization, cross-sectional, high resolution transmission electron microscopy and x-ray diffraction Studies confirm the 1 0 0 quartz orientation and the high quality epit taxal growth of quartz thin films on silicon 1 0 0 substrates. The 3D model shows the in plain epit taxal relationship between the quartz film in orange and the silicon substrate in gray viewed along the 0 1 1 zone axis.If the film is piso electric, it deforms under the applied voltage, and this can be detected through the deflection of the tip at a particular resonance frequency by using piso response force microscopy technique. This deflection amplitude is proportional to the amplitude of the applied AC field and the Piso electric coefficient is of the order of two TERs per volt. After watching this video, you should be able to prepare Aachi core films, but don't forget to use fresh extraction solution and also work under a relative humidity below 50%This methodology can provide news inside in the catalytic and kinetic role of alkaline earth metals during the diversification silica process, which enables to oppresses control over the synthesis of quats in different forms.One of the advantages of this method is that it can be combined with emerging nano fabrication techniques or conventional lithography widely used in the microelectronic industry in order to produce sensing devices.

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Learn to prepare macroporous epitaxial quartz films on silicon using chemical solution deposition and dip-coating. This versatile method enables piezoelectric thin films for advanced sensing and electromechanical device applications.

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

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