Name: imaging corrosion at the metal-paint interface using time-of-flight secondary ion mass spectrometry
Uploaded: 2019-05-06T13:00:00
Description: Watch this Scientific Journal Video about Imaging Corrosion at the Metal-Paint Interface Using Time-of-Flight Secondary Ion Mass Spectrometry at JoVE.com

这项工作得到了太平洋西北国家实验室 (PNL) 支持的快速启动方案的资助。PNNL 由 Battelle 为美国能源部运营。这项工作是利用位于 PNNL 生物科学设施内的 TOF-SIMS V 进行的。JY 和 X-Y yu 还感谢 NNL 大气科学 & 全球变化司以及物理和计算科学局 (PCSD) 的支持。

1. 腐蚀样品制备
<ol><li>
树脂中的铝样品固定和抛光
	<ol>
<li>使用1.25 英寸金相样品杯中的环氧树脂安装两个铝合金优惠券 (1 厘米 x 1 厘米), 并将优惠券放置在烟罩过夜或直到树脂完全固化。</li>
		<li>从样品杯中取出铝树脂气瓶杯。用240砂砾纸在支架内用水擦亮铝树脂气瓶, 用300转/分150转/分1米的速度擦亮铝树脂气瓶1分钟。</li>
		<li>使用15微米、6μm、3μm 和1μm 水性溶液的抛光板对铝树...

<ol>
	<li>Szklarska-Smialowska, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pitting+corrosion+of+aluminum.">Pitting corrosion of aluminum.</a> Corrosion Science. 41, 1743-1767 (1999).</li><li>Liu, 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+first+quantitative+XPS+study+of+the+surface+films+formed,+by+exposure+to+water+on+Mg+and+on+the+Mg-Al+intermetallics:+Al3Mg2+and+Mg17Al12.">A first quantitative XPS study of the surface films formed, by exposure to water on Mg and on the Mg-Al intermetallics: Al3Mg2 and Mg17Al12.</a> Corrosion Science. 51 (5), 1115-1127 (2009).</li><li>Linford, M. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+introduction+to+time-of-flight+secondary+ion+mass+spectrometry+(ToF-SIMS).">An introduction to time-of-flight secondary ion mass spectrometry (ToF-SIMS).</a> Vacuum Technology &amp; Coating. , (2014).</li><li>Cushman, C., 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+pictorial+view+of+LEIS+and+ToF-SIMS+instrumentation.">A pictorial view of LEIS and ToF-SIMS instrumentation.</a> Vacuum Technology &amp; Coating. , 27-35 (2016).</li><li>Soler, L., 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=Hydrogen+generation+by+aluminum+corrosion+in+seawater+promoted+by+suspensions+of+aluminum+hydroxide.">Hydrogen generation by aluminum corrosion in seawater promoted by suspensions of aluminum hydroxide.</a> International Journal of Hydrogen Energy. 34 (20), 8511-8518 (2009).</li><li>Ahmad, Z., Abdul Aleem, B. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Degradation+of+aluminum+metal+matrix+composites+in+salt+water+and+its+control.">Degradation of aluminum metal matrix composites in salt water and its control.</a> Materials &amp; Design. 23 (2), 173-180 (2002).</li><li>Verdier, S., Metson, J. B., Dunlop, H. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Static+SIMS+studies+of+the+oxides+and+hydroxides+of+aluminium.">Static SIMS studies of the oxides and hydroxides of aluminium.</a> Journal of Mass Spectrometry. 42 (1), 11-19 (2007).</li><li>Esmaily, 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+ToF-SIMS+investigation+of+the+corrosion+behavior+of+Mg+alloy+AM50+in+atmospheric+environments.">A ToF-SIMS investigation of the corrosion behavior of Mg alloy AM50 in atmospheric environments.</a> Applied Surface Science. 360, 98-106 (2016).</li><li>Hunt, C. P., Stoddart, C. T. H., Seah, M. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+surface+analysis+of+insulators+by+SIMS:+Charge+neutralization+and+stabilization+of+the+surface+potential.">The surface analysis of insulators by SIMS: Charge neutralization and stabilization of the surface potential.</a> Surface and Interface Analysis. 3 (4), 157-160 (1981).</li><li>Stingeder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quantitative+distribution+analysis+of+B,+As+and+Sb+in+the+layer+system+SiO2/Si+with+SIMS:+elimination+of+matrix+and+charging+effects.">Quantitative distribution analysis of B, As and Sb in the layer system SiO2/Si with SIMS: elimination of matrix and charging effects.</a> Fresenius' Zeitschrift f&#252;r analytische Chemie. 327 (2), 225-232 (1987).</li><li>Cushman, C., 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=Sample+Charging+in+ToF-SIMS:+How+it+Affects+the+Data+that+are+Collected+and+How+to+Reduce+it.">Sample Charging in ToF-SIMS: How it Affects the Data that are Collected and How to Reduce it.</a> Vacuum Technology &amp; Coating. , (2018).</li><li>Dubey, M., Brison, J., Grainger, D. W., Castner, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Comparison+of+Bi(1),+Bi(3)+and+C(60)+primary+ion+sources+for+ToF-SIMS+imaging+of+patterned+protein+samples.">Comparison of Bi(1), Bi(3) and C(60) primary ion sources for ToF-SIMS imaging of patterned protein samples.</a> Surface and Interface Analysis: SIA. 43 (1-2), 261-264 (2011).</li><li>Kozole, J., Winograd, N., Smentkowski, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cluster+Secondary+Ion+Mass+Spectrometry.">Cluster Secondary Ion Mass Spectrometry.</a> Surface Analysis and Techniques in Biology. , 71-98 (2014).</li><li>Tyler, B. J., Rayal, G., Castner, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multivariate+analysis+strategies+for+processing+ToF-SIMS+images+of+biomaterials.">Multivariate analysis strategies for processing ToF-SIMS images of biomaterials.</a> Biomaterials. 28 (15), 2412-2423 (2007).</li><li>Song, W., 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=Corrosion+behaviour+of+extruded+AM30+magnesium+alloy+under+salt-spray+and+immersion+environments.">Corrosion behaviour of extruded AM30 magnesium alloy under salt-spray and immersion environments.</a> Corrosion Science. 78, 353-368 (2014).</li><li>Esmaily, 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=On+the+capability+of+in-situ+exposure+in+an+environmental+scanning+electron+microscope+for+investigating+the+atmospheric+corrosion+of+magnesium.">On the capability of in-situ exposure in an environmental scanning electron microscope for investigating the atmospheric corrosion of magnesium.</a> Ultramicroscopy. 153, 45-54 (2015).</li><li>Liao, J., Hotta, M., Motoda, S. -. i., Shinohara, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atmospheric+corrosion+of+two+field-exposed+AZ31B+magnesium+alloys+with+different+grain+size.">Atmospheric corrosion of two field-exposed AZ31B magnesium alloys with different grain size.</a> Corrosion Science. 71, 53-61 (2013).</li><li>deVries, J. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+characterization+methods-+XPS,TOF-SIMS,+and+SAM+a+complimentary+ensemble+of+tools.">Surface characterization methods- XPS,TOF-SIMS, and SAM a complimentary ensemble of tools.</a> Journal of Materials Engineering and Performance. 7 (3), 303-311 (1998).</li><li>Zhang, H., Cooper, S. L., Guan, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+characterization+techniques+for+polyurethane+biomaterials.">Surface characterization techniques for polyurethane biomaterials.</a> Advances in Polyurethane Biomaterials. , 23-73 (2016).</li></ol>

ToF-SIMS 根据离子在两个闪烁器之间的飞行时间来区分离子。地形或样品粗糙度会影响来自不同起始位置的离子的飞行时间, 这通常会导致质量分辨率低, 峰宽度增加。因此, 重要的是要被分析的 Roi 是非常平坦的, 以确保良好的信号收集8。
另一个需要避免的陷阱是充电。由于铝漆界面与绝缘树脂固定, 预计充电。当 ROI 被主离子束轰炸时, 电荷会在样品表面积聚...

铝合金由于其高强度重量比、出色的成形性和耐腐蚀性, 在工程结构中有着广泛的应用, 如海洋技术或军用汽车。然而, 铝合金的局部腐蚀仍然是一种普遍现象, 影响着铝合金在各种环境条件下的长期可靠性、耐久性和完整性1。涂料是最常见的防腐蚀手段。在金属和油漆涂层之间的界面上形成的腐蚀说明可以为确定防止腐蚀的适当补救措施提供见解。
铝合金的腐蚀可能通过几种不同的途径发生。X 射线光电子能谱 (XPS) 和扫描电子显微镜/色散 x 射线光谱 (semsedx) 是研究腐蚀的两种常用表面显微分析技术。Xps 可以提供元素映射, 但不能提供表面化学信息2,3的全息分子视图, 而 semsedx 提供形态信息和元素映射, 但灵敏度相对较低。
ToF-SIMS 是另一种具有较高质量精度和横向分辨率的化学制图表面工具。它具有较低的检测极限 (LOD), 能够揭示在金属漆界面形成的腐蚀物种的分布。通常情况下, SIMS 质量分辨率可以达到 5000-15000, 足以区分等压离子4。ToF-SIMS 具有亚微米空间分辨率, 可以对金属涂料界面进行化学成像和表征。它不仅提供了形态信息, 而且还提供了分子腐蚀物种在表面前几纳米的横向分布。ToF-SIMS 为 XPS 和 SIM/EDX 提供补充信息。
为了证明 ToF-SIMS 在腐蚀界面的表面表征和成像方面的能力, 分析了两个涂装铝合金 (7075) 优惠券, 一张只暴露在空气中, 一张暴露在盐溶液中 (图 1和图 2)。例如, 了解暴露在盐水条件下的金属漆界面的腐蚀行为对于了解铝合金在海洋环境中的性能至关重要。众所周知, 铝 (OH)3的形成发生在铝暴露于海水5,但铝腐蚀的研究仍然缺乏全面的分子鉴定的腐蚀和涂层界面。在这项研究中, 观察和识别了铝 (oh)3的碎片, 包括铝氧化物(例如, 铝 3o5-) 和氢氧化氧物 (例如, 铝 3o6 h2-).对负离子铝 3 o5 和铝3o6h2 的 sims 质谱 (图 3)和分子 图像(图 4) 的比较提供了分子在盐溶处理铝合金优惠券的金属漆界面形成的腐蚀产物的证据。SIMS 为阐明金属漆界面上发生的复杂化学提供了可能性, 有助于揭示铝合金表面处理的有效性。在这个详细的协议中, 我们演示了这种有效的方法, 用于探测金属油漆界面, 以帮助使用 ToF-SIMS 进行腐蚀研究的新实践者。

<table border="0" cellpadding="0" cellspacing="0" style="width:737px;" width="737">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">0.05 &#181;m Colloidal Silica polishing Solution</td>
			<td style="width:152px;">LECO</td>
			<td style="width:164px;">812-121-300</td>
			<td style="width:216px;">Final polishing solution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">1 &#181;m polishing solution</td>
			<td style="width:152px;">Pace Technologies</td>
			<td style="width:164px;">PC-1001-GLB</td>
			<td style="width:216px;">Water based polishing solution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">15 &#181;m polishing solution</td>
			<td style="width:152px;">Pace Technologies</td>
			<td style="width:164px;">PC-1015-GLBR</td>
			<td style="width:216px;">Water based polishing solution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">3 &#181;m polishing solution</td>
			<td style="width:152px;">Pace Technologies</td>
			<td style="width:164px;">PC-1003-GLG</td>
			<td style="width:216px;">Water based polishing solution</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">6 &#181;m polishing solution</td>
			<td style="width:152px;">Pace Technologies</td>
			<td style="width:164px;">PC-1006-GLY</td>
			<td style="width:216px;">Water based polishing solution</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">Balance</td>
			<td style="width:152px;">Mettler Toledo</td>
			<td style="width:164px;">11106015</td>
			<td style="width:216px;">It is used for measuring the chemicals.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Epothin 2 epoxy hardener</td>
			<td style="width:152px;">Buehler</td>
			<td style="width:164px;">20-3442-064</td>
			<td style="width:216px;">Used for casting sample mounts</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Epothin 2 epoxy resin</td>
			<td style="width:152px;">Buehler</td>
			<td style="width:164px;">20-3440-128</td>
			<td style="width:216px;">Used for casting sample mounts</td>
		</tr>
		<tr height="56">
			<td height="56" style="height:56px;width:205px;">Fast protein liquid chromatography (FPLC) conductivity sensor</td>
			<td style="width:152px;">Amersham&#160;</td>
			<td style="width:164px;">AKTA FPLC</td>
			<td style="width:216px;">Used to measure the conductivity of the salt solution.</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">Final B pad</td>
			<td style="width:152px;">Allied</td>
			<td style="width:164px;">90-150-235</td>
			<td style="width:216px;">Used for 1 &#181;m and 0.05 &#181;m&#160; polishing steps</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">KCl&#160;</td>
			<td style="width:152px;">Sigma-Aldrich</td>
			<td style="width:164px;">P9333</td>
			<td style="width:216px;">Used to make the salt solution.</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">Low speed saw</td>
			<td style="width:152px;">Buehler Isomet</td>
			<td style="width:164px;">11-1280-160</td>
			<td style="width:216px;">Used to cut the Al coupons that are fixed in the epoxy resin.</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:205px;">MgCl2</td>
			<td style="width:152px;">Sigma-Aldrich</td>
			<td style="width:164px;">63042</td>
			<td style="width:216px;">Used to make the salt solution.</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:205px;">MgSO4</td>
			<td style="width:152px;">Sigma-Aldrich</td>
			<td style="width:164px;">M7506</td>
			<td style="width:216px;">It is used to make the salt solution.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">NaCl</td>
			<td style="width:152px;">Sigma-Aldrich</td>
			<td style="width:164px;">S7653</td>
			<td style="width:216px;">It is used to make the salt solution.</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">NaOH</td>
			<td style="width:152px;">Sigma-Aldrich</td>
			<td style="width:164px;">306576</td>
			<td style="width:216px;">It is used for adjusting pH of the salt solution.</td>
		</tr>
		<tr height="81">
			<td height="81" style="height:81px;width:205px;">Paint</td>
			<td style="width:152px;">Rust-Oleum&#160;</td>
			<td style="width:164px;">245217</td>
			<td style="width:216px;">Universal General Purpose Gloss Black Hammered Spray Paint. It is used to spray on the Al coupons.&#160;</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">Pan-W polishing pad</td>
			<td style="width:152px;">LECO</td>
			<td style="width:164px;">809-505</td>
			<td style="width:216px;">Used for 15, 6, and 3 &#181;m polishing steps</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">pH meter</td>
			<td style="width:152px;">Fisher Scientific</td>
			<td style="width:164px;">13-636-AP72</td>
			<td style="width:216px;">It is used for measuring the pH of the salt solution.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Pipette&#160;</td>
			<td style="width:152px;">Thermo Fisher&#160;</td>
			<td style="width:164px;">Scientific&#160;</td>
			<td style="width:216px;">Range: 10 to 1,000 &#181;L</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Pipette tip 1</td>
			<td style="width:152px;">Neptune&#160;</td>
			<td style="width:164px;">2112.96.BS&#160;</td>
			<td style="width:216px;">1,000 &#181;L</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Pipette tip 2</td>
			<td style="width:152px;">Rainin</td>
			<td style="width:164px;">17001865</td>
			<td style="width:216px;">20 &#181;L</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Silicon carbide paper</td>
			<td style="width:152px;">LECO</td>
			<td style="width:164px;">810-251-PRM</td>
			<td style="width:216px;">Grinding paper, 240 grit</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Sputter coater</td>
			<td style="width:152px;">Cressington</td>
			<td style="width:164px;">108 sputter coater</td>
			<td style="width:216px;">It is used for coating the sample.&#160;&#160;</td>
		</tr>
		<tr height="41">
			<td height="41" style="height:41px;width:205px;">Tegramin-30 Semi-automatic polisher</td>
			<td style="width:152px;">Struers</td>
			<td style="width:164px;">6036127</td>
			<td style="width:216px;">Coarse/fine polishing/grinding</td>
		</tr>
		<tr height="54">
			<td height="54" style="height:54px;width:205px;">ToF-SIMS</td>
			<td style="width:152px;">IONTOF GmbH, M&#252;nster, Germany</td>
			<td style="width:164px;">ToF-SIMS V, equipped with Bi liquid metal ion gun and flood gun</td>
			<td style="width:216px;">It is used to acquire mass spectra and images of a specimen.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:205px;">Vibromet 2 vibratory polisher</td>
			<td style="width:152px;">Buehler</td>
			<td style="width:164px;">67-1635-160</td>
			<td style="width:216px;">Final polishing step</td>
		</tr>
	</tbody>
</table>

imaging corrosion at the metal-paint interface using time-of-flight secondary ion mass spectrometry

利用飞行时间二次离子质谱 (ToF-SIMS) 对铝合金的漆和铝 (铝) 金属漆界面的腐蚀进行了分析, 说明 SIMS 是研究铝合金化学分布的一种合适技术。金属油漆界面。涂装的铝合金优惠券浸入盐溶液中或只暴露在空气中。SIMS 提供界面的化学映射和二维分子成像, 允许直接显示在金属漆界面形成的腐蚀产物的形态, 并在腐蚀发生后对化学进行映射。介绍了该方法的实验过程, 以提供技术细节, 便利类似的研究, 并突出此类实验中可能遇到的陷阱。

图 3显示了用盐溶液处理的金属漆界面与暴露在空气中的界面之间的质谱比较。利用 300μm x 300μm roi 中的 25kvbi 3+离子束扫描获得了这两个样品的质谱。盐溶液处理样品的质量分辨率 (m/' m) 在 m/z-26 的峰值约为 5, 600.在对10个通道进行分接后, 导出了质谱的原始数据。应用图形软件绘制了质谱以供呈现。已知含有铝 (OH) 3 的保护层是在铝腐蚀开始6...

Watch this Scientific Journal Video about Imaging Corrosion at the Metal-Paint Interface Using Time-of-Flight Secondary Ion Mass Spectrometry at JoVE.com

Imaging Corrosion at the Metal-Paint Interface Using Time-of-Flight Secondary Ion Mass Spectrometry

与暴露在空气中的试样相比, 采用飞行时间二次离子质谱法, 在铝合金的金属漆界面上进行化学映射和腐蚀形态。

利用飞行时二次离子质谱法成像金属颜料界面的腐蚀

Corrosion developed at the paint and aluminum (Al) metal-paint interface of an aluminum alloy is analyzed using time-of-flight secondary ion mass ...

这种方法揭示了金属漆界面的腐蚀过程，提供了对高表面灵敏度界面机械和化学变化的洞察。飞行时间二次离子质谱仪（TOF-SIMS）是一种强大的表面工具。它提供具有高横向和质量分辨率的化学图，并允许在金属漆界面上进行有效的表征。因此，新从业者应该知道的一个重要提示是确保样品不接触提取锥体，以避免对仪器的潜在损坏。这种方法的可视化演示对于对 ToF-SIMS 的科研人员至关重要，并将帮助他们进行基础分析过程。首先，将准备好的盐暴露和空气暴露样品装入仪器负载块。向下泵送负载块，将样品转移到主室，并等待，直到腔室处于或低于 10 到负 8 毫巴。然后，为液体金属离子枪（LMIG、分析仪和光源）通电。使用首选金属比斯穆特将主喷枪设置为 LMIG，并使用预定义的光谱仪启动 LMIG。接下来，使用软件或手动控件将样品阶段移动到法拉第杯。然后，自动对齐离子束。之后，开始测量法拉第杯中的目标电流，然后选择"直接电流"。单击 X 空白，并调整它，直到目标电流最大化。然后，使用 Y 空白重复此过程。完成后停止测量。接下来，在主室窗口的引导下，缓慢降低样品级，直到样品顶部低于萃取器锥体的底部。然后，将舞台放在圆锥体下，以便接口程序集在软件中的宏视图中可见。之后，将仪器设置为检测负离子。加载所需的分析器设置，然后激活分析仪。接下来，切换到微比例视图，将栅格视图字段设置为 300 到 300 微米。然后，将信号设置为辅助离子，将栅格大小设置为 128 x 128 像素，将栅格类型设置为随机。通过缓慢垂直移动样本级来调整 ROI 的次离子图像，直到图像居中于导航器 GUI 中的十字线上。调整 Z 方向时，不要过快地向下移动操纵手柄，否则抽油锥将击中舞台并损坏。之后，使用直流清洁去除金涂层和表面污染物。样品表面清洁后，启用电荷补偿，并加载所需的泛洪枪设置。然后，将次离子图像重新聚焦在 ROI 上。聚焦后，增加反射器电压，直到次离子图像消失。然后，将电压降低 20 伏，然后停止调整。接下来，打开成像窗口中的质谱，并显示金属漆界面的 ROI。启动快速扫描，并在频谱出现后停止扫描。然后，在质量谱窗口中，从快速扫描中选择质量谱中的已知峰值，然后填写公式。之后，将感兴趣的峰值添加到峰值列表中。打开测量窗口，将栅格类型设置为随机，大小设置为 128 x 128 像素，速率设置为每像素一次。将仪器设置为执行 60 次扫描，然后开始测量。之后保存已完成的频谱。然后，命名并保存 ROI 位置。移动舞台以查找要分析的新 PI。接下来，加载 LMIG 所需的高分辨率 SIMS 映像设置。将样品阶段移动到法拉第杯，重新调整并重新聚焦离子束以进行成像。然后，将舞台移回保存的 ROI 位置。调整反射器电压，获取快速频谱，并执行质量校准。然后，将栅格类型设置为随机，将大小设置为 256 x 256 像素，将速率设置为每个像素一次。将扫描次数设置为 150，然后运行图像采集。完成后，导出数据，取出样品，然后关闭仪器。二次离子质谱显示，仅暴露在空气中的样品的铝漆界面上，氧化铝和氧氢氧化物峰值较小，表明轻微腐蚀。相比之下，用盐水处理的样品有更大的峰值和额外的氧氢氧化物物种。这与盐水处理样品的腐蚀比仅暴露在空气中的样品更严重一致。2D分子图像证实，氧化铝和氧化氢氧化物在用盐水处理的样品中更为普遍。了解表面损坏和腐蚀发展是非常具有挑战性的。TOF-SIMS 是此应用的完美工具，如本过程所示。除了研究腐蚀过程外，ToF-SIMS还广泛应用于放射性、生物和环境样品的材料表面表征。请注意，质谱和图像采集的设置会因 LMIG 的类型、LMIG 的剩余寿命和其他因素而异。在这种方法中，我们说明，ToF-SIMS在微观尺度上揭示面间化学，并提供高横向分布和高质量精度的化学制图是非常强大的。ToF-SIMS 是一种表面敏感技术。请始终戴上手套，并保护您正在处理的样品。

Research

JoVE Journal

Chemistry

Matrix-assisted Laser Desorption/Ionization Time of Flight (MALDI-TOF) Mass Spectrometric Analysis of Intact Proteins Larger than 100 kDa

Matrix-assisted Laser Desorption/Ionization Time of Flight MALDI-TOF Mass Spectrometric Analysis of Intact Proteins Larger than 100 kDa

基质辅助飞行的完整蛋白质（MALDI-TOF）质谱分析激光解吸/电离飞行时间大于100 kDa的

Effectively determining masses of proteins is critical to many biological studies (e.g. for structural biology investigations). Accurate mass ...

科研

化学

Analyzing Protein Dynamics Using Hydrogen Exchange Mass Spectrometry

使用氢交换质谱分析蛋白质动力学

All cellular processes depend on the functionality of proteins. Although the functionality of a given protein is the direct consequence of its unique ...

A Study of the Complexation of Mercury(II) with Dicysteinyl Tetrapeptides by Electrospray Ionization Mass Spectrometry

A Study of the Complexation of MercuryII with Dicysteinyl Tetrapeptides by Electrospray Ionization Mass Spectrometry

汞（II）与Dicysteinyl四肽的络合的电喷雾质​​谱研究

In this study we evaluated a method for the characterization of complexes, formed in different relative ratios of mercury(II) to dicysteinyl tetrapeptide, ...

Rapid High-throughput Species Identification of Botanical Material Using Direct Analysis in Real Time High Resolution Mass Spectrometry

植物材料的快速高通量物种鉴定实时高分辨质谱法直接分析

We demonstrate that direct analysis in real time-high resolution mass spectrometry can be used to produce mass spectral profiles of botanical material, ...

Analyzing the Photo-oxidation of 2-propanol at Indoor Air Level Concentrations Using Field Asymmetric Ion Mobility Spectrometry

用场不对称离子迁移光谱法分析 2-丙醇在室内空气浓度中的光氧化作用

We demonstrate a versatile protocol to be used for determining the effectiveness of photocatalysts in degrading indoor air concentration (ppb) volatile ...

Real-time Breath Analysis by Using Secondary Nanoelectrospray Ionization Coupled to High Resolution Mass Spectrometry

利用二次 Nanoelectrospray 电离耦合高分辨质谱的实时呼吸分析

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental ...

Synthesis and Mass Spectrometry Analysis of Oligo-peptoids

寡 peptoids 的合成及质谱分析

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have ...

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight MALDI-TOF Mass Spectrometry

基质辅助激光解吸电离飞行时间 (MALDI) 质谱法表征合成聚合物

There are many techniques that can be employed in the characterization of synthetic homopolymers, but few provide as useful of information for end group ...

Ion Mobility-Mass Spectrometry Techniques for Determining the Structure and Mechanisms of Metal Ion Recognition and Redox Activity of Metal Binding Oligopeptides