Criador A. foi apoiada por uma Fundação Annenberg Graduate Research Fellowship, e este trabalho foi financiado pela National Science Foundation [085281 e 1028440].

1. Fabricação de microesferas <ol><li> Seleccionar uma pequena quantidade (cerca de 5 polegadas) de fibra óptica, tira ~ 1,5 revestimento &quot;a partir de uma extremidade e limpar com metanol ou etanol (Figura 1a, b). </li><li> Se disponível, decompor o fim com um cutelo de fibra óptica. Se não estiver disponível, cortado com cortadores de arame ou tesouras tais que ~ 0,5 &quot;é deixado. A vantagem de usar um cutelo de fibra óptica é que produz um corte muito lisa, uniforme como na Figura 1b. Rugosidade excessiva ou defeitos de um corte pode causar refluxo desigual, baixando o factor de qualidade das esferas resultantes. </li><li> Expor a extremidade da fibra limpos para 3W de CO potência do laser focado 2 para um tamanho de mancha ~ 500μm diâmetro para ~ 1 segundo (Figura 1c, d, e). Isto produz esferas do ~ 200μm de diâmetro, no entanto, o tamanho pode ser sintonizado pelo aumento ou diminuição do diâmetro da fibra óptica. Ajustando levemente a intensidade do laser pode também be necessário para esferas de refluxo maiores ou menores. </li></ol> 2. Fabricação Microtoroid <ol><li> Projetar e fazer um fotomáscara com escuras, círculos sólidos, no espaçamento e diâmetro de sua escolha. É importante notar que os toros produzidos serão 25-30% menor do que os círculos sobre a máscara. Por exemplo, um círculo sólido com um diâmetro de 100 micra irá produzir um toróide com um diâmetro de aproximadamente 75 microns. Além disso, recomenda-se para deixar pelo menos 1-2 milímetros de espaço entre cada círculo e, pelo menos, 5 mm de espaço entre as matrizes de círculos e em torno das bordas da máscara. Uma vez que as bolachas de amostra deve ser cuidadosamente tratada com uma pinça, é importante para deixar espaço para as pinças para aperto sem danificar os toros. O espaço extra também proporciona espaço para uma fibra óptica para luz afunilada par para os dispositivos acabados, e permite que as amostras para ser cortado em matrizes menores mais facilmente. Para este procedimento, foi utilizada uma máscara com linhas de 160 mM dicírculos ameter ~ um milímetro de distância, com ~ 5 mm de espaço entre cada fileira de círculos. Os toros acabados são cerca de 110 um de diâmetro. </li><li> Comece com wafers de silício com uma camada grossa de 2 mM de sílica termicamente crescido. Clivam as bolachas para atender ao padrão desejado microdisco sobre a máscara de fotolitografia, deixando espaço para fotorresiste borda talão. Note-se que, no início de fabricação, é geralmente mais conveniente para o etch várias matrizes de círculos em pedaços maiores de bolachas de silício (~ cm vários centímetros x vários). Wafers maiores permitir fotolitografia e BOE de gravação do mais amostras de cada vez, e são mais facilmente manuseado com uma pinça. Mais tarde, antes do passo de condicionamento XeF 2, é recomendado para clivar as bolachas maiores em matrizes menores para permitir que mais rápida, mais uniforme XeF 2 condicionamento. </li><li> Em um fumehood, limpar cuidadosamente as bolachas, por lavagem com metanol, acetona, isopropanol, e água desionizada. Soprar as amostras secas usando um azoto ou comp filtradapistola de ar pri me num, e colocá-las sobre um placa quente ajustado para 120 ° C durante pelo menos 2 minutos para secar. </li><li> Depois de deixar as bolachas arrefecer, coloque em um fumehood inflamável / solvente e expor a HMDS por 2 minutos, utilizando o método de deposição de vapor. Um método simples deposição de vapor: ponha algumas gotas de HMDS num copo de 10 ml pequena e, em seguida cobrir as bolachas e pequeno copo com um recipiente de vidro maior para manter o vapor. </li><li> Coloque uma amostra em um spinner com uma montagem de tamanho adequado. Usando um frasco conta-gotas ou de uma seringa e filtro, aplicar fotossensíveis para a amostra. Girar fotorresiste revestimento S1813 para cada amostra durante 5 segundos a 500 rpm, seguidos por 45 segundos a 3000 rpm. Aresta de remoção do grânulo não é necessário se a bolacha é suficientemente grande para que o grânulo borda não interfere com o padrão. </li><li> Cozer mole do material fotosensitivo sobre uma placa quente a 95 ° C durante 2 minutos. </li><li> Usando um alinhador de máscara UV e da fotomáscara desejado, expor as amostras fotorresiste-coberto a umatotal de 2 80mJ/cm de radiação UV. </li><li> Imergir as amostras em MF-321 revelador para remover o material fotosensitivo que foi exposta à luz UV. Ao desenvolver, estreitamente ver como o material fotosensitivo é removida da bolacha e dissolveu-se. É importante a agitar / bochechar o recipiente constantemente durante este processo para garantir o material fotosensitivo é removida de modo uniforme. Para os parâmetros fornecidos, o fotorresiste leva aproximadamente 30 segundos para se desenvolver. </li><li> Quando a maior parte do material fotosensitivo indesejado se dissolveu no revelador, lavar as amostras com água corrente, suavemente secar as amostras utilizando um azoto ou pistola de ar, e inspeccionar as amostras com um microscópio para garantir que todo material fotosensitivo indesejada foi removido. Se necessário, as amostras podem ser imersos novamente em desenvolvedor, no entanto, deve-se ter cuidado para não revelar demasiadamente as amostras como dos padrões desejados fotossensíveis também pode ser danificado. (Se os padrões desejados são danificado ou defeituoso, o material fotosensitivo pode serremovidos com acetona e as etapas de 2,1-2,9 podem ser repetidos de novo). </li><li> Depois de desenvolver, lave bem as amostras em água corrente, seque suavemente as amostras, e difícil fazê-los em um prato quente a 110 ° C por 2 minutos. Esta etapa aquece o fotorresiste acima de sua temperatura de transição vítrea, reflui o fotorresiste e rugosidade parcialmente reparar que ocorreu durante o processo de desenvolvimento. </li><li> Usando Teflon recipientes eo equipamento de protecção necessário, imergir as amostras em melhor tamponado óxido etchant (BOE). BOE contém HF, que grava a sílica não coberta por material fotosensitivo para formar almofadas de sílica circulares sobre a bolacha de silício (Figura 2a-c). Melhorou HF tampão produz uma suave etch rugosidade, minimizando os círculos de sílica resultantes. Embora seja possível misturar tamponada HF começando com HF 49%, isso pode levar a resultados altamente variáveis ​​como tipicamente apenas pequenas quantidades são feitas. </li><li> Após cerca de 15-20 minutos (dNa sequência da eventual padrões, tamanhos de amostra e número de amostras), retirar as amostras do BOE usando uma pinça de teflon. Com cuidado, lavar as amostras em água corrente. A sílica foi removida quando as amostras se tornar hidrofóbica. </li><li> Após o condicionamento, enxaguamento e secagem, as amostras, inspeccionar os usando um microscópio óptico. Verifique se os padrões desejados tenham sido gravados completamente e todos os indesejados de sílica foi removido. Se necessário, retornar as amostras para o BOE para gravação posterior. Deve-se ter cuidado para não overetch das amostras, ou os padrões circulares debaixo do fotorresiste pode estar danificado. </li><li> Depois ataque BOE é completo, enxaguar as amostras em água deionizada e seque. Se as amostras são em grandes pedaços de bolacha de silício, é também recomendado para cortá-los (usando uma serra de corte em cubos ou escriba diamante) em pequenos pedaços com linhas individuais de círculos de sílica. Linhas individuais de círculos são gravados de forma mais rápida e uniformemente no XeF2 passo gravura (2,16). Pó de silício produzido pelo corte é removido durante a limpeza no passo seguinte. </li><li> Remover o material fotosensitivo por lavagem com metanol, acetona, isopropanol, e água desionizada, e secar as amostras utilizando uma pistola de azoto e aquecimento em uma ° C 120 de placa quente durante pelo menos 2 minutos. </li><li> Usando um XeF etcher 2, minar o silício sob as almofadas de sílica circulares para formar microdiscos de sílica (Figura 2d-f). A quantidade gravado deve ser de aproximadamente 1/3 do tamanho do círculo de sílica, de modo que o pilar microdisco resultante é de aproximadamente 1/3-1/2 do diâmetro total do disco, tal como determinado por inspecção com um microscópio óptico. O número de XeF 2 pulsos e da duração de cada pulso depende da quantidade de silício na câmara e do tipo de XeF etcher 2 utilizado. </li><li> Após condicionamento XeF 2, expor as amostras a um feixe de laser focado CO 2 a cerca de 12W intensidade para ~ 3 segundos ou até um toróide liso é formado (Figura 2g-i). Dependendo do tamanho exacto do disco e da quantidade de XeF 2 minar, uma intensidade ligeiramente superior ou inferior e tempo de exposição pode ser necessário para formar uma microtoroid. É importante que o centro do feixe de laser e do centro do microdisco estão alinhados, de modo que o microdisco sílica irá formar uma microtoroid, liso circular. </li></ol> 3. Os resultados representativos Os dispositivos de microesferas e microtoroid pode ser fotografada usando microscopia óptica e microscopia eletrônica de varredura (2h Figura E 1d, e Figura, i). Em todas as imagens, a uniformidade da superfície do dispositivo é claramente evidente. Para verificar que a abordagem pormenorizada cria ultra-high-Q dispositivos, também caracterizado o factor Q de vários dispositivos através da realização de uma largura de linha de medição (Δλ) e calculando a carregadaQ a partir da simples expressão: Q = λ / Δλ = ωτ, onde λ = comprimento de onda ressonante, = freqüência ω, e τ = tempo de vida do fóton. Os espectros de representativas de cada dispositivo fabricado utilizando os procedimentos anteriormente pormenorizados 1,9 e um gráfico de comparação de vários dispositivos é mostrado na Figura 3. Os fatores de qualidade de todos os dispositivos estão acima de 10 milhões, sendo a maioria acima de 100 milhões. O espectro da microesfera era uma ressonância única, indicando que a luz acoplado em quer o dos ponteiros do relógio ou anti-horário modo de propagação óptica. No entanto, o espectro do toróide exibiram uma ressonância de divisão, o que indica que a luz acoplada em ambos os modos no sentido horário e anti-horário simultaneamente. Este fenómeno ocorre quando existe uma pequena imperfeição no local de acoplamento. Ao ajustar o espectro de uma dupla Lorentziana, o factor Q de ambos os modos pode ser determinada. O fenômeno de ressonância divisãond pode ocorrer tanto na esfera e toróide ressonadores, mas é mais freqüentemente observada em toróides como eles são mais suscetíveis a falhas e têm menos modos ópticos em comparação com as esferas. <img src="/files/ftp_upload/4164/4164fig1.jpg" alt="A Figura 1"/> Figura Fluxograma 1. Do processo de microesfera cavidade de fabricação. a) de processamento e, b) micrografia óptica de uma fibra limpos e clivado óptico. c) Prestação, d) micrografia óptica e e) micrografia eletrônica de varredura de um microspere ressonador. <img src="/files/ftp_upload/4164/4164fig2.jpg" alt="A Figura 2"/> Figura Fluxograma 2. Do processo de fabricação microtoroid cavidade. um processamento), b) micrografia topo vista óptico e c) vista lateral-micrografia electrónica de varredura da almofada de óxido de circular, tal como definido por fotolitografia e corrosão BOE. Note-se a ligeira cunha-forma do óxido de que é formada pela BOE. d) Rendering, e) top-viewmicrografia óptica e f) de visão lateral micrografia electrónica de varredura da almofada de óxido após o passo de condicionamento XeF 2. Note-se que o disco de óxido mantém a periferia em forma de cunha. g) Prestação, h) top-view micrografia óptica e i) visão lateral micrografia eletrônica de varredura da cavidade microtoroid. <img src="/files/ftp_upload/4164/4164fig3.jpg" alt="A Figura 3"/> Figura 3. Representativas espectros factor de qualidade da uma microesfera) eb) microtoroid cavidades de ressonância, conforme determinado utilizando o método de medição da largura de linha. Em dispositivos muito elevados Q, pode-se observar o modo de divisão ou um pico duplo, no qual a luz se reflete em um pequeno defeito e circula em ambas as direções no sentido horário e anti-horário. c) o gráfico de comparação mostrando os fatores Q de microesferas e várias microtoroid cavidades de ressonância. <a href="http://www.jove.com/files/ftp_upload/4164/4164fig3large.jpg" target="_blank">Clique aqui para ampliar a figura</a> . Figura 4. Esquemática do refluxo laser de CO 2 set-up. O CO 2 feixe de laser (linha azul sólido) é reflectida e então concentrou-se sobre a amostra. Ele passa através dos 10,6 mM / 633 nm feixe combinador, que transmite 10,6 mM e reflecte a 633 nm. As imagens de coluna ópticos de reflexão da amostra fora do combinador de feixe e, portanto, a imagem é um pouco vermelho. A lista dos elementos necessários para esta configuração é na Tabela 4. <img src="/files/ftp_upload/4164/4164fig5.jpg" alt="A Figura 5"/> Figura 5. Incorrectamente refluído uma microesfera) eb) microtoroid cavidades de ressonância. Devido à colocação incorrecta dentro do feixe, o dispositivo é mal-formado. c) Como resultado de uma fotomáscara pobres ou litografia pobres, o toróide é em forma de lua.

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Tal como acontece com qualquer estrutura óptica, manutenção da limpeza em cada passo do processo de fabricação é de importância crítica. Como existem vários livros escritos sobre o tema da litografia e fabricação, as sugestões abaixo não pretende ser exaustiva, mas destacar algumas das questões mais comuns pesquisadores enfrentaram. 19-20 Devido a uniformidade da periferia do microtoroid é determinada pela uniformidade do disco inicial, é muito importante para os d...

<table border="1"><tbody><tr><td> Nome da peça </td><td> Companhia </td><td> Número de catálogo </td><td> Comentários </td></tr><tr><td> Escriba Fibra </td><td> Newport </td><td> F-RFS </td><td> Opcional </td></tr><tr><td> Fibra ótica </td><td> Newport </td><td> F-SMF-28 </td><td> Qualquer tipo de fibra óptica podem ser usadas. </td></tr><tr><td> Extractor revestimento de fibra </td><td> Newport </td><td> STR-F-175 </td><td> Decapantes fio podem também ser utilizados </td></tr><tr><td> Etanol </td><td> Qualquer vendedor </td><td> Solventes grau de pureza </td><td> Metanol ou isopropanol são substitutos </td></tr></tbody></table> Tabela 1. Materiais de fabrico de microesfera. <table border="1"><tbody><tr><td> Nome do reagente </td><td> Companhia </td><td> &lt;Número de catálogo strong&gt; </td><td> Comentários </td></tr><tr><td> Wafers de silício com sílica termicamente crescido 2μm </td><td> Materiais sobre o mesmo tema </td><td> n / a </td><td> Usamos intrínseca 8, &lt;100&gt;, 4 &quot;de diâmetro </td></tr><tr><td> HMDS (hexametildisilazano) </td><td> Aldrich </td><td> 440191 </td><td></td></tr><tr><td> Fotossensíveis </td><td> Shipley </td><td> S1813 </td><td></td></tr><tr><td> Revelador </td><td> Shipley </td><td> MF-321 </td><td></td></tr><tr><td> Buffered HF - Melhor </td><td> Transene </td><td> n / a </td><td> O HF melhor buffer dá uma suave qualidade, melhor do que simples etch BOE ou HF </td></tr><tr><td> Metanol, acetona, isopropanol </td><td> Qualquer vendedor </td><td> Pureza de 99,8% </td><td></td></tr></tbody></table> Tabela 2. Microtoroid Materiais de fabricação. <table border="1"><tbody><tr><td> Nome Equipamento </td><td> Fabricante </td><td> Número de catálogo </td><td> Comentários </td></tr><tr><td> Fiandeiro </td><td> Solitec </td><td> 5110-ND </td><td> Qualquer giratório pode ser usado. </td></tr><tr><td> Alinhador </td><td> Suss Microtec </td><td> MJB 3 </td><td> Qualquer alinhador pode ser usado. </td></tr><tr><td> XeF 2 etcher </td><td> Avançado Comunicação Devices, Inc. </td><td> # ADCETCH2007 </td><td></td></tr></tbody></table> Tabela 3. Microtoroid equipamento de fabricação. <table border="1"><tbody><tr><td> Nome da peça </td><td> Companhia </td><td> Número de catálogo </td><td> Comentários </td></tr><tr><td> CO 2 </sub&gt; Laser </td><td> Synrad </td><td> Série 48 </td><td></td></tr><tr><td> 3-Eixos estágio </td><td> OptoSigma </td><td> 120-0770 </td><td> Disponível a partir de outros fornecedores também. </td></tr><tr><td> Si Reflector 1 &quot;de diâmetro) </td><td> II-VI </td><td> 308325 </td><td> Disponível a partir de outros fornecedores também. </td></tr><tr><td> Montagem em cardan cinemática (para Si refletor) </td><td> Thor Labs </td><td> KX1G </td><td> Disponível a partir de outros fornecedores também. </td></tr><tr><td> Feixe combinador (1 &quot;de diâmetro) </td><td> Meller Optics </td><td> L19100008-B0 </td><td> Disponível a partir de outros fornecedores também. </td></tr><tr><td> 4 &quot;Lente Distância focal (1&quot; de diâmetro) </td><td> Meller Optics ou II-VI </td><td></td><td> Disponível a partir de outros fornecedores, bem </td></tr><tr><td> Mensagens sortidas, montagens de lentes </td><td> Thor Labs, Newport, Edmund Optics ou Optosigma </td><td></td><td></td></tr><tr><td> Zoom 6000 sistema de visão de máquina </td><td> Navitar </td><td> n / a </td><td> Requer câmera USB genérico e computador de imagens em tempo real. Este é adquirido como um kit. </td></tr><tr><td> Focalizador para o sistema 6000 Zoom </td><td> Edmund Optics </td><td> 54-792 </td><td> Disponível a partir de outros fornecedores também. </td></tr><tr><td> Posicionadores Eixo XZ para 6000 Zoom </td><td> Parker Daedal </td><td> CR4457, CR4452, 4499 </td><td> CR4457 é eixo X, CR4452 é eixo Z, 4499 é o suporte de montagem. </td></tr></tbody></table> Tabela 4. CO 2 Refluxo Laser Set-up.

fabrication of silica ultra high quality factor microresonators

Whispering gallery resonant cavities confine light in circular orbits at their periphery.1-2 The photon storage lifetime in the cavity, quantified by the quality factor (Q) of the cavity, can be in excess of 500ns for cavities with Q factors above 100 million. As a result of their low material losses, silica microcavities have demonstrated some of the longest photon lifetimes to date1-2. Since a portion of the circulating light extends outside the resonator, these devices can also be used to probe the surroundings. This interaction has enabled numerous experiments in biology, such as single molecule biodetection and antibody-antigen kinetics, as well as discoveries in other fields, such as development of ultra-low-threshold microlasers, characterization of thin films, and cavity quantum electrodynamics studies.3-7
The two primary silica resonant cavity geometries are the microsphere and the microtoroid. Both devices rely on a carbon dioxide laser reflow step to achieve their ultra-high-Q factors (Q&gt;100 million).1-2,8-9 However, there are several notable differences between the two structures. Silica microspheres are free-standing, supported by a single optical fiber, whereas silica microtoroids can be fabricated on a silicon wafer in large arrays using a combination of lithography and etching steps. These differences influence which device is optimal for a given experiment.
Here, we present detailed fabrication protocols for both types of resonant cavities. While the fabrication of microsphere resonant cavities is fairly straightforward, the fabrication of microtoroid resonant cavities requires additional specialized equipment and facilities (cleanroom). Therefore, this additional requirement may also influence which device is selected for a given experiment.
Introduction
An optical resonator efficiently confines light at specific wavelengths, known as the resonant wavelengths of the device. 1-2 The common figure of merit for these optical resonators is the quality factor or Q. This term describes the photon lifetime (&tau;o) within the resonator, which is directly related to the resonator's optical losses. Therefore, an optical resonator with a high Q factor has low optical losses, long photon lifetimes, and very low photon decay rates (1/&tau;o). As a result of the long photon lifetimes, it is possible to build-up extremely large circulating optical field intensities in these devices. This very unique property has allowed these devices to be used as laser sources and integrated biosensors.10
A unique sub-class of resonators is the whispering gallery mode optical microcavity. In these devices, the light is confined in circular orbits at the periphery. Therefore, the field is not completely confined within the device, but evanesces into the environment. Whispering gallery mode optical cavities have demonstrated some of the highest quality factors of any optical resonant cavity to date.9,11 Therefore, these devices are used throughout science and engineering, including in fundamental physics studies and in telecommunications as well as in biodetection experiments. 3-7,12
Optical microcavities can be fabricated from a wide range of materials and in a wide variety of geometries. A few examples include silica and silicon microtoroids, silicon, silicon nitride, and silica microdisks, micropillars, and silica and polymer microrings.13-17 The range in quality factor (Q) varies as dramatically as the geometry. Although both geometry and high Q are important considerations in any field, in many applications, there is far greater leverage in boosting device performance through Q enhancement. Among the numerous options detailed previously, the silica microsphere and the silica microtoroid resonator have achieved some of the highest Q factors to date.1,9 Additionally, as a result of the extremely low optical loss of silica from the visible through the near-IR, both microspheres and microtoroids are able to maintain their Q factors over a wide range of testing wavelengths.18 Finally, because silica is inherently biocompatible, it is routinely used in biodetection experiments.
In addition to high material absorption, there are several other potential loss mechanisms, including surface roughness, radiation loss, and contamination loss.2 Through an optimization of the device size, it is possible to eliminate radiation losses, which arise from poor optical field confinement within the device. Similarly, by storing a device in an appropriately clean environment, contamination of the surface can be minimized. Therefore, in addition to material loss, surface scattering is the primary loss mechanism of concern.2,8
In silica devices, surface scattering is minimized by using a laser reflow technique, which melts the silica through surface tension induced reflow. While spherical optical resonators have been studied for many years, it is only with recent advances in fabrication technologies that researchers been able to fabricate high quality silica optical toroidal microresonators (Q&gt;100 million) on a silicon substrate, thus paving the way for integration with microfluidics.1
The present series of protocols details how to fabricate both silica microsphere and microtoroid resonant cavities. While silica microsphere resonant cavities are well-established, microtoroid resonant cavities were only recently invented.1 As many of the fundamental methods used to fabricate the microsphere are also used in the more complex microtoroid fabrication procedure, by including both in a single protocol it will enable researchers to more easily trouble-shoot their experiments.

Watch this Scientific Journal Video about Fabrication of Silica Ultra High Quality Factor Microresonators at JoVE.com

Fabrication of Silica Ultra High Quality Factor Microresonators

Nós descrevemos a utilização de uma técnica de carbono refluxo dióxido de laser para fabricar cavidades de sílica ressonantes, incluindo autónoma microesferas e no chip microtoroids. O método de refluxo remove imperfeições superficiais, permitindo longos tempos de vida de fotões dentro ambos os dispositivos. Os dispositivos resultantes têm ultra-fatores de alta qualidade, permitindo aplicações que vão das telecomunicações à biodetection.

Fabricação de Sílica Ultra microresonators alto fator de qualidade

Whispering gallery resonant cavities confine light in circular orbits at their periphery.1-2 The photon storage lifetime in the cavity, quantified by the ...

fabrication-of-silica-ultra-high-quality-factor-microresonators

Research

JoVE Journal

Engineering

16.0K visualizações.  University of Southern California. Nós descrevemos a utilização de uma técnica de carbono refluxo dióxido de laser para fabricar cavidades de sílica ressonantes, incluindo autónoma microesferas e no chip microtoroids. O método de refluxo remove imperfeições superficiais, permitindo longos tempos de vida de fotões dentro ambos os dispositivos. Os dispositivos resultantes têm ultra-fatores de alta qualidade, permitindo aplicações que vão das telecomunicações à biodetection.

Vídeo: Fabrication of Silica Ultra High Quality Factor Microresonators

Angle-resolved Photoemission Spectroscopy At Ultra-low Temperatures

The physical properties of a material are defined by its electronic structure. Electrons in solids are characterized by energy (&omega;) and momentum (k) and the probability to find them in a particular state with given &omega; and k is described by the spectral function A(k, &omega;). This function can be directly measured in an experiment based on the well-known photoelectric effect, for the explanation of which Albert Einstein received the Nobel Prize back in 1921. In the photoelectric effect the light shone on a surface ejects electrons from the material. According to Einstein, energy conservation allows one to determine the energy of an electron inside the sample, provided the energy of the light photon and kinetic energy of the outgoing photoelectron are known. Momentum conservation makes it also possible to estimate k relating it to the momentum of the photoelectron by measuring the angle at which the photoelectron left the surface. The modern version of this technique is called Angle-Resolved Photoemission Spectroscopy (ARPES) and exploits both conservation laws in order to determine the electronic structure, i.e. energy and momentum of electrons inside the solid. In order to resolve the details crucial for understanding the topical problems of condensed matter physics, three quantities need to be minimized: uncertainty* in photon energy, uncertainty in kinetic energy of photoelectrons and temperature of the sample.
In our approach we combine three recent achievements in the field of synchrotron radiation, surface science and cryogenics. We use synchrotron radiation with tunable photon energy contributing an uncertainty of the order of 1 meV, an electron energy analyzer which detects the kinetic energies with a precision of the order of 1 meV and a He3 cryostat which allows us to keep the temperature of the sample below 1 K. We discuss the exemplary results obtained on single crystals of Sr2RuO4 and some other materials. The electronic structure of this material can be determined with an unprecedented clarity.

The overall goal of this method is to determine the low-energy electronic structure of solids at ultra-low temperatures using Angle-Resolved Photoemission Spectroscopy with synchrotron radiation.

Ângulo resolvido espectroscopia de fotoelétrons em ultra-baixas temperaturas

The physical properties of a material are defined by its  electronic structure. Electrons in solids are characterized by energy (&omega;)  and momentum ...

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Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

Síntese e microdiffraction a pressões e temperaturas extremas

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

Convergent Polishing: A Simple, Rapid, Full Aperture Polishing Process of High Quality Optical Flats &amp; Spheres

Convergent Polishing is a novel polishing system and method for finishing flat and spherical glass optics in which a workpiece, independent of its initial shape (i.e., surface figure), will converge to final surface figure with excellent surface quality under a fixed, unchanging set of polishing parameters in a single polishing iteration. In contrast, conventional full aperture polishing methods require multiple, often long, iterative cycles involving polishing, metrology and process changes to achieve the desired surface figure. The Convergent Polishing process is based on the concept of workpiece-lap height mismatch resulting in pressure differential that decreases with removal and results in the workpiece converging to the shape of the lap. The successful implementation of the Convergent Polishing process is a result of the combination of a number of technologies to remove all sources of non-uniform spatial material removal (except for workpiece-lap mismatch) for surface figure convergence and to reduce the number of rogue particles in the system for low scratch densities and low roughness. The Convergent Polishing process has been demonstrated for the fabrication of both flats and spheres of various shapes, sizes, and aspect ratios on various glass materials. The practical impact is that high quality optical components can be fabricated more rapidly, more repeatedly, with less metrology, and with less labor, resulting in lower unit costs. In this study, the Convergent Polishing protocol is specifically described for fabricating 26.5 cm square fused silica flats from a fine ground surface to a polished ~&#955;/2 surface figure after polishing 4 hr per surface on a 81 cm diameter polisher.

A novel optical polishing process, called &#8220;Convergent Polishing&#8221;, which enables faster, lower cost polishing, is described. Unlike conventional polishing processes, Convergent Polishing allows a glass workpiece to be polished in a single iteration and with high surface quality to its final surface figure without requiring changes to polishing parameters.

Convergente Polimento: Um simples, rápido, de abertura total Polimento Processo de alta qualidade ótica Flats &amp; Spheres

Convergent Polishing is a novel polishing system and method for finishing flat and spherical glass optics in which a workpiece, independent of its initial ...

Fabrication of High Contrast Gratings for the Spectrum Splitting Dispersive Element in a Concentrated Photovoltaic System

High contrast gratings are designed and fabricated and its application is proposed in a parallel spectrum splitting dispersive element that can improve the solar conversion efficiency of a concentrated photovoltaic system. The proposed system will also lower the solar cell cost in the concentrated photovoltaic system by replacing the expensive tandem solar cells with the cost-effective single junction solar cells. The structures and the parameters of high contrast gratings for the dispersive elements were numerically optimized. The large-area fabrication of high contrast gratings was experimentally demonstrated using nanoimprint lithography and dry etching. The quality of grating material and the performance of the fabricated device were both experimentally characterized. By analyzing the measurement results, the possible side effects from the fabrication processes are discussed and several methods that have the potential to improve the fabrication processes are proposed, which can help to increase the optical efficiency of the fabricated devices.

The fabrication of high contrast gratings as the parallel spectrum splitting dispersive element in a concentrated photovoltaic system is demonstrated. Fabrication processes including nanoimprint lithography, TiO2 sputtering and reactive ion etching are described. Reflectance measurement results are used to characterize the optical performance.

Fabricação de grades de alto contraste para o Splitting Spectrum dispersivo Elemento em um sistema fotovoltaico concentrado

High contrast gratings are designed and fabricated and its application is proposed in a parallel spectrum splitting dispersive element that can improve ...

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, building and food industries, amongst others. Polyester and coatings containing both polyester and silica nanoparticles (SiO2NPs) have been widely used to protect steel substrata from corrosion. In this study, we utilized X-ray photoelectron spectroscopy, attenuated total reflection infrared micro-spectroscopy, water contact angle measurements, optical profiling and atomic force microscopy to provide an insight into how exposure to sunlight can cause changes in the micro- and nanoscale integrity of the coatings. No significant change in surface micro-topography was detected using optical profilometry, however, statistically significant nanoscale changes to the surface were detected using atomic force microscopy. Analysis of the X-ray photoelectron spectroscopy and attenuated total reflection infrared micro-spectroscopy data revealed that degradation of the ester groups had occurred through exposure to ultraviolet light to form COO&#903;, -H2C&#903;, -O&#903;, -CO&#903; radicals. During the degradation process, CO and CO2 were also produced.

Two types of surfaces, polyester-coated steel and polyester coated with a layer of silica nanoparticles, were studied. Both surfaces were exposed to sunlight, which was found to cause substantial changes in the chemistry and nanoscale topography of the surface.

A evolução de sílica Coatings nanopartículas-poliéster em superfícies expostas à luz solar

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

Fabricação de alta temperatura de nanoestruturado ria-Stabilized Zirconia-Scaffolds (ZEI) pela<em&gt; In Situ</em&gt; Carbono Templating xerogéis

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.

Caracterização de Ultra-grão fino e nanocristalinos Materiais Usando Transmissão Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and ...

Scalable Solution-processed Fabrication Strategy for High-performance, Flexible, Transparent Electrodes with Embedded Metal Mesh

Here, the authors report the embedded metal-mesh transparent electrode (EMTE), a new transparent electrode (TE) with a metal mesh completely embedded in a polymer film. This paper also presents a low-cost, vacuum-free fabrication method for this novel TE; the approach combines lithography, electroplating, and imprint transfer (LEIT) processing. The embedded nature of the EMTEs offers many advantages, such as high surface smoothness, which is essential for organic electronic device production; superior mechanical stability during bending; favorable resistance to chemicals and moisture; and strong adhesion with plastic film. LEIT fabrication features an electroplating process for vacuum-free metal deposition and is favorable for industrial mass production. Furthermore, LEIT allows for the fabrication of metal mesh with a high aspect ratio (i.e., thickness to linewidth), significantly enhancing its electrical conductance without adversely losing optical transmittance. We demonstrate several prototypes of flexible EMTEs, with sheet resistances lower than 1 &#937;/sq and transmittances greater than 90%, resulting in very high figures of merit (FoM) &#8211; up to 1.5 x 104 &#8211; which are amongst the best values in the published literature.

This protocol describes a solution-based fabrication strategy for high-performance, flexible, transparent electrodes with fully-embedded, thick metal mesh. Flexible transparent electrodes fabricated by this process demonstrate among the highest reported performances, including ultra-low sheet resistance, high optical transmittance, mechanical stability under bending, strong substrate adhesion, surface smoothness, and environmental stability.

Estratégia de fabricação processada e escalável para eletrodos flexíveis e transparentes de alto desempenho com malha metálica embutida

Here, the authors report the embedded metal-mesh transparent electrode (EMTE), a new transparent electrode (TE) with a metal mesh completely embedded in a ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present an advanced method for fabricating ultra-thin color films with improved characteristics. The proposed process addresses several fabrication issues, including large area processing. Specifically, the protocol describes a process for fabricating ultra-thin color films using an electron beam evaporator for oblique angle deposition of germanium (Ge) and gold (Au) on silicon (Si) substrates.&#160; Film porosity produced by the oblique angle deposition induces color changes in the ultra-thin film. The degree of color change depends on factors such as deposition angle and film thickness. Fabricated samples of the ultra-thin color films showed improved color tunability and color purity. In addition, the measured reflectance of the fabricated samples was converted into chromatic values and analyzed in terms of color. Our ultra-thin film fabricating method is expected to be used for various ultra-thin film applications such as flexible color electrodes, thin film solar cells, and optical filters. Also, the process developed here for analyzing the color of the fabricated samples is broadly useful for studying various color structures.

We present a detailed method for fabricating ultra-thin color films with improved characteristics for optical coatings. The oblique angle deposition technique using an electron beam evaporator allows improved color tunability and purity. Fabricated films of Ge and Au on Si substrates were analyzed by reflectance measurements and color information conversion.

Fabricação de filmes de cor ultra-fino com altamente absorvente Media usando ângulo oblíquo deposição

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...

Flow-assisted Dielectrophoresis: A Low Cost Method for the Fabrication of High Performance Solution-processable Nanowire Devices

Flow-assisted dielectrophoresis (DEP) is an efficient self-assembly method for the controllable and reproducible positioning, alignment, and selection of nanowires. DEP is used for nanowire analysis, characterization, and for solution-based fabrication of semiconducting devices. The method works by applying an alternating electric field between metallic electrodes. The nanowire formulation is then dropped onto the electrodes which are on an inclined surface to create a flow of the formulation using gravity. The nanowires then align along the gradient of the electric field and in the direction of the liquid flow. The frequency of the field can be adjusted to select nanowires with superior conductivity and lower trap density. 
In this work, flow-assisted DEP is used to create nanowire field effect transistors. Flow-assisted DEP has several advantages: it allows selection of nanowire electrical properties; control of nanowire length; placement of nanowires in specific areas; control of orientation of nanowires; and control of nanowire density in the device. 
The technique can be expanded to many other applications such as gas sensors and microwave switches. The technique is efficient, quick, reproducible, and it uses a minimal amount of dilute solution making it ideal for the testing of novel nanomaterials. Wafer scale assembly of nanowire devices can also be achieved using this technique, allowing large numbers of samples for testing and large-area electronic applications.

In this paper, flow assisted dielectrophoresis is demonstrated for the self-assembly of nanowire devices. The fabrication of a silicon nanowire field effect transistor is shown as an example.

Dieletroforese assistida por fluxo: Um método de baixo custo para a fabricação de dispositivos de solução-processable nanofio de alto desempenho

Flow-assisted dielectrophoresis (DEP) is an efficient self-assembly method for the controllable and reproducible positioning, alignment, and selection of ...