반도체 공정에서 발생하는 실리콘 슬러지의 재활용을 위한 상압 저온가열법의 제안

윤창민 한국도시환경학회 2023 한국도시환경학회지 Vol.23 No.3

본 연구에서는 실리콘 슬러지로부터 실라놀 전구체를 추출하지 않고 상압 저온가열법을 통해 실리카 나노입자를 제조하였으며, 기존의 수열합성법과 졸-겔법의 차이를 비교 분석하였다. 실리콘 슬러지의 산세처리를 통해 유기물과 금속 불순물을 제거한 실리콘 분말을 상압에서 가열하여 콜로이달 상태의 실리카 나노입자를 제조하였다. 상압가열법을 통해 제조한 실리카 나노입자는 수열합성법 및 졸겔법과 비교를 위해 형상 및 화학적 특성 분석을 진행하였다. 그 결과, 상압 저온가열법은 수열합성법 대비 균일하고 고순도의 실리카 나노입자가 제조됨을 확인할 수 있었다. 또한, 실리콘 슬러지 자체를 활용하기에 졸-겔법에 비해 높은 수득률의 실리카 나노입자가 합성되었다. 본 연구를 통해 반도체 공정에서 발생한실리콘 슬러지를 효과적으로 재활용하는 새로운 제조법에 대해 제시하였으며, 기존의 제조법에 비해 우수한 특성을 지니고 있어 환경적 측면에서 지속 가능한 방향성을 제공하는데 기여할 것으로 기대된다. In this study, silica nanoparticles are synthesized from silicon sludge using atmospheric heating method without extracting silanol precursor, in which the method is analyzed and compared with existing hydrothermal and sol-gel methods. Organic and metallic impurities in silicon sludge are removed by acid-washing process to obtain silicon powder, followed by heating the powder under atmospheric pressure to prepare silica nanoparticles. The morphological and chemical properties of as-synthesized silica nanoparticles are examined and compared with those obtained using conventional hydrothermal and sol-gel methods. As a result, silica nanoparticles fabricated by atmospheric heating method showed enhanced uniformity and higher purity compared to the nanoparticles synthesized by hydrothermal method. In addition, a higher yield of silica nanoparticles is synthesized compared to sol-gel method owing to the direct utilization of silicon sludge using atmospheric heating method. Accordingly, this study presents a novel approach for effectively recycling silicon sludge generated from semiconductor manufacturing process, which may contribute to providing continuous directions for protecting environment.

은나노를 이용한 비팽윤성 운모의 수열적인 표면개질 및 특성평가

석정원,박라영,김판채,Seok, Jeong-Won,Park, Ra-Young,Kim, Pan-Chae 한국결정성장학회 2007 한국결정성장학회지 Vol.17 No.4

수평회전식 수열법에 의해 운모 분말을 합성하였다. 수열조건은 출발원료로 $K_2O,\;Al(OH)_3$ 그리고 $SiO_2$의 비는 1 : 3 : 3mol%로 하고 수열용매로 8mol%의 KOH를 함께 추가하여 $260^{\circ}C$에서 72시간 동안 반응시켰다. 합성한 분말은 수직형 수열처리법에 의한 은나노 코팅 운모 제조를 위해 사용하였다. 은나노 코팅의 처리를 위한 수열조건은 출발원료로 합성한 분말로 하고, 수열용매로 $0.5{\ell}$ 3차 증류수, 그리고 1,000ppm의 은나노 졸을 코팅원료로 사용하여 $160{\sim}260^{\circ}C$ 범위에서 72시간 동안 반응시켰다. 처리 후 결정구조, 은나노 코팅 여부 및 코팅된 운모의 특성은 XRD, SEM, TEH-EDX 및 shake plask법을 통해 분석하였다. Mica (muscovite) powders were synthesized by hydrothermal method (horizontal turning method). The hydrothermal conditions for the synthesis of mica were prepared by the ratio of $K_2O : Al(OH)_3 : SiO_2$ = 1 : 3 : 3 mol% as the starting materials with KOH (8 mol%) solution as the hydrothermal solvent and reaction temperature at $260^{\circ}C$ for 72hrs. The synthetic powder used for preparation of nano silver coated mica by vertical hydrothermal treatment. The hydrothermal conditions for the treated as nano silver coating were prepared by the synthetic powder as raw materials, triple distilled water ($0.5{\ell}$) solution as the hydrothermal solvent with nano silver sol (1,000 ppm) as the material of nano silver coating and reaction temperature at $160{\sim}260^{\circ}C$ for 72 hrs. After hydrothermal treatment, structural, judgment of nano silver coating and character of nano silver coated mica were examined by XRD, SEM, TEM-EDX and shake plask method.

수열합성법으로 제조된 Zn-TiO₂ 나노입자와 TiO₂ 나노입자가 zebrafish 배발생에 미치는 영향

여민경(Min-Kyeong Yeo),김효은(Hyo-Eun Kim) 환경독성보건학회 2009 환경독성보건학회지 Vol.24 No.4

In this study, we investigated the biological toxicity of nano-scale Zn (0.1, 0.5, and 1 ㏖%)-doped TiO₂ and pure TiO₂ nanoparticles using zebrafish embryogenesis as our model organism. Zn-doped TiO2 nanoparticles were prepared using a conventional hydrothermal method for the insertion of zinc into the TiO₂ framework. The characters of Zn-doped TiO₂ (0.1%, 0.5%, 1%Zn) and pure TiO₂ were about 7~8 ㎚. These sizes were smaller than 100~200 ㎚ of TiO₂ was prepared using the sol-gel method. Particularly, in this study, we found no significant biological toxicity in the hatching rate and abnormal rate under expose pureTiO₂ and Zn-doped TiO₂ nanoparticles were prepared using a conventional hydrothermal method of zebrafish. It was different from the biological damage under TiO₂ nanoparticles were prepared using sol-gel method. We assessed that the damage was not linked to the particle’s nanometer size, but rather due to the prepare method. Moreover, TiO₂ nanoparticles were prepared using a hydrothermal method were not shown to cause cytotoxic effects, like apoptosis and necrosis, that are the major markers of toxicity in organisms exposed to nanomaterials. Therefore, there is some relationship with biological toxicity of nanoparticles and the prepare method of nanometer size particles.

Ferroelectric Property of a Hydrothermally-grown PbTiO3 Film with an Aerosol-deposited Seed Layer

이종필,임연수,노임준,공영민,이정근,이수환,정대용 한국물리학회 2013 THE JOURNAL OF THE KOREAN PHYSICAL SOCIETY Vol.63 No.12

The hydrothermal method is a unique method for the growth of ferroelectric materials becausetheir materials can be grown at a relatively low reaction temperature below 250 C. To grow aPbTiO3 (PT) film on a metal Ni substrate, we first deposited a PT seed layer on the Ni substrateby using the aerosol deposition (AD) method; then we grew PT film on top of the PT seed layer byusing the hydrothermal process. X-ray diffraction (XRD) and scanning electron microscopy (SEM)revealed that the AD PT film acted well as a seed layer and that a highly-dense PT film had beensuccessfully grown following the crystal structure of the seed layer. Both the PT seed layer andthe hydrothermally-grown PT film had distorted crystal structures with decreased tetragonality. The output voltage due to impact on the film confirmed that the hydrothermally-grown PT filmhad a spontaneous polarization along the ‘c’ axis. The hydrothermally-grown PT film exhibitedferroelectric hysteresis loops without mechanical breakage during several cyclic measurements.

수열법에 의한 호주산 천연 사파이어의 색상 개선

김희승,Kim, Hee-Seung 한국결정성장학회 2006 한국결정성장학회지 Vol.16 No.6

The significant color enhancement in low quality Australian natural sapphire has been achieved by a hydrothermal method. The optimal conditions for the color enhancement of Australian natural sapphire were as follows; hydrothermal reaction temperature: $320{\sim}350^{\circ}C$, duration : 3 days, hydrothermal solvent: 2 M NaOH solution. After the hydrothermal treatment, Australian natural sapphires of transparent colors were obtained, and their grades were found to be improved from commercial to middle/top grade by value chart analysis. 본 연구에서는 수열법을 이용하여 저품질의 호주산 천연 사파이어에 대한 색상개선을 행하였다. 호주산 천연 사파이어의 색상 개선에 대한 최적의 수열처리 조건은 다음과 같다. 즉, 수열반응온도 $320{\sim}350^{\circ}C$, 반응시간: 3일, 수열용매: 2 M NaOH 수용액이다. 이와 같은 조건하에서 수열 처리한 후에 투명한 색상의 호주산 천연 사파이어가 얻어졌으며 천연 사파이어 가치 차트로 비교한 결과, commercial 등급이 $middle{\sim}top$ 등급으로 색상이 개선되었음을 확인하였다.

Hydrothermal conversion of <i>Magnolia liliiflora</i> into nitrogen-doped carbon dots as an effective turn-off fluorescence sensing, multi-colour cell imaging and fluorescent ink

Atchudan, Raji,Edison, Thomas Nesakumar Jebakumar Immanuel,Aseer, Kanikkai Raja,Perumal, Suguna,Lee, Yong Rok Elsevier 2018 Colloids and Surfaces B Vol.169 No.-

<P><B>Abstract</B></P> <P>The present work illustrates the potential uses of nitrogen-doped multi-fluorescent carbon dots (N-CDs) for Fe<SUP>3+</SUP> sensing, cellular multi-colour imaging, and fluorescent ink. N-CDs were synthesized using <I>Magnolia liliiflora</I> flower by the simple hydrothermal method. The resulted N-CDs was found to be nearly spherical in shape with the size of about 4 ± 1 nm and showed competitive quantum yield around 11%. The synthesized N-CDs with uniform size distribution and high content of nitrogen and oxygen-bearing functional groups exhibit excellent dispersibility in aqueous media. The N-CDs were able to detect a high concentration of Fe<SUP>3+</SUP> ions (1–1000 μM) with a limit of detection is about 1.2 μM by forming N-CDs-Fe<SUP>3+</SUP> complex due to the functional groups such as nitrogen, carbonyl and carboxyl on the surface of N-CDs. Thus they could be used to remove pollutants from industrial wastewater. The electronic charge on the surface of the N-CDs and N-CDs-Fe<SUP>3+</SUP> complex (zeta potential) is around −36 and 18 mV, respectively. In addition, these N-CDs show excitation-dependent fluorescence that was utilized for multi-colour in vitro cellular imaging in rat liver cells (<I>Clone 9 hepatocytes</I>). The N-CDs are rapidly uptake in the cell cytoplasm and showed high cytocompatibility on cellular morphology. Moreover, as the N-CDs possess strong fluorescence and anti-coagulation they could be utilized in fluorescent ink pens.</P> <P><B>Highlights</B></P> <P> <UL> <LI> Hydrothermal conversion of <I>M. liliiflora</I> into N-CDs by one-pot hydrothermal method. </LI> <LI> N-CDs was applied as a fluorescent probe for the effective detection of Fe<SUP>3+</SUP> ions. </LI> <LI> N-CDs could offer a multi-colour cell imaging without any chemical modification. </LI> <LI> N-CDs was used as a fluorescent ink without any pretreatment of the sample. </LI> </UL> </P> <P><B>Graphical abstract</B></P> <P>N-CDs were synthesized using <I>M. liliiflora</I> flower and were potentially utilized for the detection of Fe<SUP>3+</SUP> ions, multi-colour cellular imaging and fluorescent ink.</P> <P>[DISPLAY OMISSION]</P>

Efficiently photocatalytic CO₂ reduction with H₂O vapors to CH₄ using Sb1.5Sn8.5-xTixO₂ synthesized by hydrothermal method

김현수,임영환,김강민,박민규,박덕영,강미숙 한국공업화학회 2014 한국공업화학회 연구논문 초록집 Vol.2014 No.1

To enhance the photoreduction of CO₂ into CH₄, this study focused on a new typed photocatalyst, Sb1.5Sn8.5-xTixOy, which partially Tiincorporated to the framework of ATO (antimony-doped tin oxide) with high conducting property and low band-gap, synthesized using a controlled hydrothermal method. The structures and properties of the Sb_1.5Sn_8.5-xTixOy (x=0, 0.5, 1.0, 1.5) photocatalysts were characterized by XRD, TEM, EDAX, XPS, BET, CV, UV-vis and PL spectroscopy. On the XRD and TEM analysis results, it was confirmed that the Sb_1.5Sn_8.5-xTixOy nanoparticles exhibited a tetragonal crystal structure with about 20 nm. The band-gap increased depends on Ti-addition. In the result of photoreduction of CO₂ with H₂O, the generated CH₄ remarkable increased in Sb_1.5Sn_8.5-xTixOy catalysts, in particular, it was the best on the Sb_1.5Sn_8.5Ti_1.0Oy, and it reached 3-fold higher than an anatase TiO₂ presented for comparison.

Microwave sintering of lead-free barium titanate piezoelectric ceramics from barium titanate powders synthesized by a hydrothermal method

Kongjun Zhu,Jinhao Qiu,Hongli Ji,Yuansheng Chen 한양대학교 세라믹연구소 2010 Journal of Ceramic Processing Research Vol.11 No.3

In this study, three types of BaTiO3 powder with different particle sizes synthesized by a hydrothermal method were used to fabricate the lead-free barium titanate piezoelectric ceramics. The BaTiO3 ceramics from these three types of BaTiO3 powders were sintered at different temperatures (1100 and 1150 oC) using a microwave sintering method, and their piezoelectric properties were investigated and compared. The results indicate that all The BaTiO3 piezoelectric ceramics exhibit higher d33value (above 330 pC/N, the highest is about 370 pC/N). The reasons were also investigated by comparing the properties of the three types of BaTiO3 powders, sintering temperature and method.

수열흡착법을 이용한 은 점코팅된 구리 나노분말의 합성과 미세조직

김형철,한재길,Kim, Hyeong-Chul,Han, Jae-Kil 한국분말야금학회 2011 한국분말재료학회지 (KPMI) Vol.18 No.6

Ag spot-coated Cu nanopowders were synthesized by a hydrothermal-attachment method (HA) using oleic acid capped Ag hydrosol. Cu nano powders were synthesized by pulsed wire exploding method using 0.4 mm in diameter of Cu wire (purity 99.9%). Synthesized Cu nano powders are seen with comparatively spherical shape having range in 50 nm to 150 nm in diameter. The oleic acid capped Ag hydrosol was synthesized by the precipitation-redispersion method. Oleic acid capped Ag nano particles showed the narrow size distribution and their particle size were less than 20 nm in diameter. In the case of nano Ag-spot coated Cu powders, nanosized Ag particles were adhered in the copper surface by HAA method. The components of C, O and Ag were distributed on the surface of copper powder.

Structural and magnetic properties of Ni doped titanate nanotubes synthesized by hydrothermal method

여준한,Wolfgang M. Sigmund 한양대학교 세라믹연구소 2015 Journal of Ceramic Processing Research Vol.16 No.1

A new method, hydrothermal method, to synthesize Ni doped rutile TiO2 nanotube (TNT) powders is introduced. This method is more scalable than ones used before. Interestingly, our Ni doped TNTs’ structures show different characteristics and properties than ones fabricated by other methods. We report these resulting structural and magnetic properties here. Ni doped nanotubes contained H2Ti2O5H2O doped with trivalent Ni. The layered structures had six nm inner and ten nm outer diameters, aspect ratios of seven, and exhibited ferromagnetism at room temperature (undoped nanotubes were diamagnetic). Contrary to earlier versions of Ni doped TNTs, we found that trivalent Ni atoms substituted H+ in the nanotubes and thus interacted with titanate’s 3d electrons to produce ferromagnetic activity. This opens the possibility to achieve ferromagnetic activity in TNTs in a new way.