Name: spark plasma sintering apparatus used for the formation of strontium titanate bicrystals
Uploaded: 2017-02-09T15:00:00
Description: Watch this Scientific Journal Video about Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals at JoVE.com

LH gratefully acknowledges financial support by an US National Science Foundation Graduate Research Fellowship under Grant No. 1148897. Electron microscopy characterization and SPS processing at UC Davis was financially supported by a University of California Laboratory Fee award (#12-LR-238313). Work at the Molecular Foundry was supported by the Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231.

1. Sample Preparation of Single Crystal Strontium Titanate
NOTE: Single crystal STO is supplied with a (100) surface polished to a mirror finish.
<ol>
	<li>Section STO into 5x5 mm2 pieces using diamond wire saw.</li>
	<li>Ultrasonically clean samples at 50-60 Hz consecutively in baths of acetone, isopropanol, and methanol for fifteen minutes each.</li>
	<li>Remove STO from methanol bath to immediately place on hot plate held at a temperature of 200 &#176;C. Heating the sample afte...

<ol>
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Jpn. 109 (7), S110-S120 (2001).</li><li>Hutt, S., Kienzle, O., Ernst, F., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Processing+and+Structure+of+Grain+boundaries+in+Strontium+Titanate.">Processing and Structure of Grain boundaries in Strontium Titanate.</a> Z. Metallkd. 92 (2), 105-109 (2001).</li><li>Takahisa, Y., Ikuhara, Y., Sakuma, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Current-voltage+characteristics+across+45&#9702;+symmetric+tilt+boundary+in+highly+donor-doped+SrTiO3+bicrystal.">Current-voltage characteristics across 45&#9702; symmetric tilt boundary in highly donor-doped SrTiO3 bicrystal.</a> J. Mater. Sci. Lett. 20, 1827-1829 (2001).</li><li>Hill, A., Wallach, E. 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Mater. 4 (6), 605-611 (2003).</li><li>Hirose, S., Nishimura, H., Niimi, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resistance+switching+effect+in+Nb-doped+SrTiO[sub+3]+(100)+bicrystal+with+(100)+&#8764;45&#176;+twist+boundary.">Resistance switching effect in Nb-doped SrTiO[sub 3] (100) bicrystal with (100) &#8764;45&#176; twist boundary.</a> J. App. Phys. 106 (4), 043711-043716 (2009).</li><li>Hutt, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Doctoral Thesis. , (2002).</li><li>Brunner, D., Taeri-Baghbadrani, S., Sigle, W., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Suprising+Results+of+a+Studay+on+the+Plasticity+in+Strontium+Titanate.">Suprising Results of a Studay on the Plasticity in Strontium Titanate.</a> J. Amer. Ceram. Soc. 84 (5), 1161-1163 (2001).</li><li>Gumbsch, P., Taeri-Baghbadrani, S., Brunner, D., Sigle, W., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Plasticity+and+an+inverse+brittle-to-ductile+transition+in+strontium+titanate.">Plasticity and an inverse brittle-to-ductile transition in strontium titanate.</a> Phys. Rev. Lett. 87 (8), 085501-085504 (2001).</li><li>Taeri, S., Brunner, D., Sigle, W., Ruhle, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deformation+Behavior+of+Strontium+Titanate+between+Room+Temperature+and+1800K+under+Ambient+Pressure.">Deformation Behavior of Strontium Titanate between Room Temperature and 1800K under Ambient Pressure.</a> Z. Metallkd. 95, 433-446 (2004).</li><li>Takahashi, K., Ohtomo, A., Kawasaki, M., Koinuma, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Advanced+Processing+and+Characterization+of+SrTiO3+Single+Crystals+and+Bicrystals+for+High+Tc+Superconducting+Film+Substrate.">Advanced Processing and Characterization of SrTiO3 Single Crystals and Bicrystals for High Tc Superconducting Film Substrate.</a> Mater. Sci. Eng. B. 41, 152-156 (1996).</li><li>Rhodes, W. H., Kingery, W. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dislocation+Dependence+of+Cationic+Diffusion+in+SrTiO3.">Dislocation Dependence of Cationic Diffusion in SrTiO3.</a> J. Amer. Ceram. 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The bonding temperature of 1,200 &#176;C was chosen to maximize diffusion as small changes in temperature can greatly impact the kinetics of all diffusion bonding mechanisms. A temperature of 1,200 &#176;C is outside the brittle-ductile transition temperature range of STO. However, the sample underwent brittle fracture at this temperature. The catastrophic failure of the STO bicrystal was not unexpected as STO has ~ 0.5% ductility at 1,200 &#176;C. Also, the sample was held at a pressure of 140 MPa throughout the heating...

Spark plasma sintering (SPS) is a technique in which application of high uniaxial pressure and pulsed direct current leads to the rapid densification of powder compacts1. This technique also leads to the successful formation of composite structures from various materials, including silicon nitride/silicon carbide, zirconium boride/silicon carbide, or silicon carbide, with no additional sintering aids required2,3,4,5. The synthesis of these composite structures by conventional hot-pressing had been challenging in the past. While application of a high uniaxial pressure and fast heating rate via the SPS technique enhances consolidation of powders and composites, the phenomenon causing this enhanced densification debated in the literature2,3,6,7. There also exists only limited information regarding the influence of electric fields on grain boundary formation and the resulting atomic structures of grain boundary cores8,9. These core structures determine the functional properties of SPS sintered materials, including electric breakdown of high voltage capacitors and the mechanical strength and toughness of ceramic oxides10. Therefore, understanding the fundamental grain boundary structure as a function of SPS processing parameters, such as applied current, is necessary for the manipulation of a material&#39;s overall physical properties. One method to systematically elucidate the fundamental physical mechanisms underpinning SPS is the formation of specific grain boundary structures, i.e., bicrystals. A bicrystal is created by manipulation of two single crystals, which are then diffusion bonded with specific misorientation angles11. This method provides a controlled way to investigate the fundamental grain boundary core structures as a function of processing parameters, dopant concentration, and impurity segregation12,13,14.
Diffusion bonding is dependent on four parameters: temperature, time, pressure, and bonding atmosphere15. Conventional diffusion bonding of strontium titanate (SrTiO3, STO) bicrystals typically occurs at a pressure below 1 MPa, within a temperature range of 1,400-1,500 &#176;C, and time scales ranging from 3 to 20 hours13,14,16,17. In this study, bonding in a SPS apparatus is achieved at significantly lower temperature and time scales in comparison to conventional methods. For polycrystalline materials, reduced temperature and time scales via SPS significantly limits grain growth, thereby providing advantageous control of a material&#39;s properties through manipulation of its microstructure.
The SPS apparatus, for a 5&#215;5 mm2 sample, exerts a minimum pressure of 140 MPa. Within the conventional diffusion bonding temperature range, Hutt et al. report instantaneous fracture of STO when the bonding pressure exceeds 10 MPa18. However, STO exhibits temperature dependent plasticity behavior, indicating bonding pressure can exceed 10 MPa at specific temperatures. Above 1,200 &#176;C and below 700 &#176;C, STO exhibits some ductility, at which stresses greater than 120 MPa can be applied without instantaneous fracture of the sample. Within the intermediate temperature range of 700-1,200 &#176;C, STO is brittle and experiences instantaneous fracture at stresses greater than 10 MPa. At 800 &#176;C, STO has minor deformability prior to fracture at stresses less than 200 MPa19,20,21. Hence, bonding temperatures for STO bicrystal formation via SPS apparatus must be selected according to the plasticity behavior of the material.

<table border="0" cellpadding="0" cellspacing="0" width="1429">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Strontium titanate single crystal (100)</td>
			<td style="width:187px;">MTI Corporation</td>
			<td style="width:427px;">STOa101005S1-JP</td>
			<td style="width:443px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Buffered oxide etch, hyrofluoric acid 6:1</td>
			<td style="width:187px;">JT Baker</td>
			<td style="width:427px;">&#160;MBI 1178-03</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Scanning electron microscope (SEM)</td>
			<td style="width:187px;">FEI</td>
			<td>Model: 430 NanoSEM</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">SPS apparatus&#160;</td>
			<td>Sumitomo Coal Mining Co</td>
			<td>Model: Dr. Sinter 5000 SPS Apparatus</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">High Temperature Furnace</td>
			<td>Thermolyne</td>
			<td>Model: 41600</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Ultrasonic Cleaner</td>
			<td>Bransonic</td>
			<td>Model: 221</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Mechanical polisher</td>
			<td style="width:187px;">Allied High Tech Products</td>
			<td>15-2100-TEM</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Diamond lapping film</td>
			<td style="width:187px;">3M</td>
			<td>660XV&#160;</td>
			<td>1 um to 9 um Grit Size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Diamond lapping film</td>
			<td style="width:187px;">3M</td>
			<td style="width:427px;">661X</td>
			<td>0.5 um to 0.1 um Grit Size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Colloidal silica</td>
			<td style="width:187px;">Allied High Tech Products</td>
			<td>180-20000</td>
			<td>.05 um Grit Size</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Sputter coater</td>
			<td style="width:187px;">QuorumTech</td>
			<td>Model: Q150RES</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Focused ion beam (FIB) instrument&#160;</td>
			<td style="width:187px;">FEI</td>
			<td>Model: Scios dual-beamed focused ion beam (FIB) instrument&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nanomill TEM specimen preparation system</td>
			<td style="width:187px;">Fischione Instruments</td>
			<td>Model: 1040</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Transmission electron microscope (TEM)&#160;</td>
			<td style="width:187px;">JEOL</td>
			<td>Model: JEM2500 SE&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Scanning transmission electron microscope (STEM)</td>
			<td style="width:187px;">FEI</td>
			<td>Model: TEAM 0.5&#160;</td>
			<td></td>
		</tr>
	</tbody>
</table>

spark plasma sintering apparatus used for the formation of strontium titanate bicrystals

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with one twist grain boundary. This apparatus utilizes high uniaxial pressure and a pulsed direct current for rapid consolidation of material. Diffusion bonding of strontium titanate bicrystals without fracture, in a spark plasma sintering apparatus, is possible at high pressures due to the unusual temperature dependent plasticity behavior of strontium titanate. We demonstrate a method for the successful formation of bicrystals at accelerated time scales and lower temperatures in a spark plasma sintering apparatus compared to bicrystals formed by conventional diffusion bonding parameters. Bond quality was verified by scanning electron microscopy. A clean and atomically abrupt interface containing no secondary phases was observed using transmission electron microscopy techniques. Local changes in bonding across the boundary was characterized by simultaneous scanning transmission electron microscopy and spatially resolved electron energy-loss spectroscopy.

Bonding temperature, time, and misorientation angle were all altered to determine optimum parameters needed for the maximum possible bonded interface fraction of the STO bicrystal (Table 1). The interface was considered &#39;bonded&#39; when the grain boundary was not visible during SEM imaging (Figure 2a). A &#39;non-bonded&#39; interface was exhibited when a dark image contrast or voids were present at the boundary location (Figure 2b)....

Watch this Scientific Journal Video about Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals at JoVE.com

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

A viable technique for the formation of strontium titanate bicrystals at high pressure and fast heating rate via the spark plasma sintering apparatus is developed.

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with ...

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