• 대한화학회지
• /
• 제46권5호
• /
• pp.419-437
• /
• 2002

산성조건에서 $H_2O_2$에 의한 $Fe^{2+}$ 이온의 산화($Fe^{2+}{\to}Fe^{3+}$)반응과 $Fe^{3+}$이온과 $SCN^-$이온이 결합하여 붉은색 Fe$(SCN)^{3-x}_x$ 이온을 형성하는 착화반응을 도입한 흐름주입분석기법을 사용하여 $Fe^{2+}$이온과 $Fe^{2+}$이온이 공존하는 시료용액 중 각 이온들의 동시정량을 위한 분석법을 개발하였다. 이 분석법은 개별 이온들에 대한 정량단계에 앞서 혼합시료의 전처리($Fe^{2+}$이온의 예비산화 혹은 $Fe^{2+}$이온의 예비환원)단계를 거쳐야 하는 기존의 분석법들과는 달리 두가지 단계들을 동시에 수행할 수있다는 장점을 가진다. 이 분석법의 측정한계는 [$Fe^{2+}$]=6.00${\times}10^{-7}$M 이었다.

• 한국전기전자재료학회논문지
• /
• 제30권4호
• /
• pp.246-252
• /
• 2017

Pulverized $FeS_2$ (pyrite) gives different discharge test results with as-received $FeS_2$ electrodes. The as-received $FeS_2$ electrode shows three voltage plateaus during the discharge test. However, the ball-milled $FeS_2$ electrode shows two voltage plateaus. To interpret this result, the effect of $FeS_2$ particle size on electrochemical reactions is investigated by unit cell discharge tests, SEM and XRD. As a result, it is found that the transition reaction product ($Li_2+xFe+xS_2$) of $FeS_2$ explains the difference. The as-received $FeS_2$ reacts according to three reaction steps ($FeS_2{\rightarrow}Li_3Fe_2S_4{\rightarrow}Li_2+xFe_1+xS_2{\rightarrow}LiFe_2S_4$). However, ball-milled $FeS_2$ reacts without the $Li_2+xFe_1+xS_2$ stage. In this study, this result is explained by the difference in electrochemical reaction mechanism. The as-received $FeS_2$ has a larger radius than the ball-milled $FeS_2$. Therefore, the lithium ion has to diffuse into the $FeS_2$ unreacted core, and $Li_2+xFe_1+xS_2$, the transition reaction product of as-received $FeS_2$, is formed during this stage.

• 한국세라믹학회지
• /
• 제36권5호
• /
• pp.471-477
• /
• 1999

Fe and Fe-Mo binder were used to produce TiB2 based cermet by a pressureless sintering. The densification behaviour of TiB2-Fe-Mo cermet during liquid-phase sintering in argon was studied in relation to binder phase charactertics. The effects of Mo addition and sintering condition on the sintering behaviour and mechanical properties were also investigated. TiB2-based cermets with Fe-Mo binder composition showed a better sinterability than the cermets with only Fe binder. In TiB2-Fe-Mo cermet higher densities in the wide temperature range were obtained and also fully densified sintered cermet were obtained at 1873K The enhancement in the densification phenomenon of TiB2-Fe-Mo system can be explained by improved liquid phase wettability associated with the roles of Mo components as solute atoms. When Fe-Mo binders were used cermets with a finer grain size and enhanced mechanical properties wereproduced and new phases such as Fe2B and Mo2FeB2 were observed in the sintered cermet. The highest bending strength was obtained from the 20vol% Fe-Mo cermet and these hardness-fracture toughness combination in the wide binder compositions is better than that of TiB2-Fe cermet. In order to improve mechanical properties microstructure control with high purity powders is desirable because high purity powders prevent the formation of Fe2B and Mo2FeB2 phase which comsume the ductile binder phase.

• 한국세라믹학회지
• /
• 제32권2호
• /
• pp.234-238
• /
• 1995

MgFe2O4 formation, grain growth in Fe2O3, Fe solid-solution limit in MgO for MgO-Fe2O3 mixture were studied by means of investigating the distribution of phases and compositions in reaction area between MgO and Fe2O3. The reaction area at equlibrium was composed with MgO-FexO matrix and MgFe2O4 precipitation, MgFe2O4 was formed by precipitating from MgO-FexO matrix dependent on oxygen partial pressure. Fe contents was exponentially decreased with diffusion distance in MgO single crystal, and thus Fe solid-solution limitation in MgO was about 4mol%. The grain growth rate in Fe2O3 base was increased with Mg contents diffused from MgO single crystal.

• 한국재료학회지
• /
• 제22권11호
• /
• pp.620-625
• /
• 2012

A general synthetic method to make $Fe_3O_{4-{\delta}}$ (activated magnetite) is the reduction of $Fe_3O_4$ by $H_2$ atmosphere. However, this process has an explosion risk. Therefore, we studied the process of synthesis of $Fe_3O_{4-{\delta}}$ depending on heat-treatment conditions using $FeC_2O_4{\cdot}2H_2O$ in Ar atmosphere. The thermal decomposition characteristics of $FeC_2O_4{\cdot}2H_2O$ and the ${\delta}$-value of $Fe_3O_{4-{\delta}}$ were analyzed with TG/DTA in Ar atmosphere. ${\beta}-FeC_2O_4{\cdot}2H_2O$ was synthesized by precipitation method using $FeSO_4{\cdot}7H_2O$ and $(NH_4)_2C_2O_4{\cdot}H_2O$. The concentration of the solution was 0.1 M and the equivalent ratio was 1.0. ${\beta}-FeC_2O_4{\cdot}2H_2O$ was decomposed to $H_2O$ and $FeC_2O$4 from $150^{\circ}C$ to $200^{\circ}C$. $FeC_2O4$ was decomposed to CO, $CO_2$, and $Fe_3O_4$ from $200^{\circ}C$ to $250^{\circ}C$. Single phase $Fe_3O_4$ was formed by the decomposition of ${\beta}-FeC_2O_4{\cdot}2H_2O$ in Ar atmosphere. However, $Fe_3C$, Fe and $Fe_4N$ were formed as minor phases when ${\beta}-FeC_2O_4{\cdot}2H_2O$ was decomposed in $N_2$ atmosphere. Then, $Fe_3O_4$ was reduced to $Fe_3O_{4-{\delta}}$ by decomposion of CO. The reduction of $Fe_3O_4$ to $Fe_3O_{4-{\delta}}$ progressed from $320^{\circ}C$ to $400^{\circ}C$; the reaction was exothermic. The degree of exothermal reaction was varied with heat treatment temperature, heating rate, Ar flow rate, and holding time. The ${\delta}$-value of $Fe_3O_{4-{\delta}}$ was greatly influenced by the heat treatment temperature and the heating rate. However, Ar flow rate and holding time had a minor effect on ${\delta}$-value.

• 한국세라믹학회지
• /
• 제33권3호
• /
• pp.327-331
• /
• 1996

$\delta$-FeOOH was prepared by rapid oxidation method of Fe(OH)2 using H2O2. The effects of reaction temperature and mole ratio ([OH-]/[Fe2+])의 몰비를 제조 변수로 하여 최종 생성된 $\delta$-FeOOH의 입자크기 입자형태, 자기특성을 조사하였다. Fe(OH)2 의 반응온도 및 [OH-]/[Fe2+] 비가 $\delta$-FeOOH의 입자크기 및 형상에 많은 영향을 미침을 알수 있었으며 입자 크기는 이 두인자에 비례하여 증가하였다 Fe(OH)2 의 반응온도가 4$0^{\circ}C$ [OH-]/[Fe2+]=5 Fe(OH)2 숙성 시간 2시간에서 제조된 $\delta$-FeOOH를 TEM, VSM으로 입자의 크기 및 자기특성을 조사한결과 평균 입경이 630$\AA$ 정도이고 입도 분포가 양호하였으며 포화자화 및 보자력은 각각 20.8emu/g 210 Oe였다.

• 한국광물학회지
• /
• 제20권4호
• /
• pp.367-376
• /
• 2007

에이니그마타이트($Na_4(Fe^{2+},Ti,Fe^{3+}){_{12}}(Fe^{3+},Si){_{12}}O_{40}$)는 Na가 풍부한 알칼리 화성암에 흔히 산출되는 광물이며, 분지 개방형 단쇄형 규산염광물로 분류된다. 3개의 산출이 다른 자연산 에이니그마타이트를 대상으로 뫼스바우어 분광분석을 실시하였으며 상세한 결정화학적 연구가 수행되었다. 뫼스바우어 분광분석 결과 9개의 흡수선이 분리되었는데, 3쌍의 흡수선은 팔면체 자리를 점유하는 $Fe^{2+}$의 피크이며, 저속도 구간의 독립적인 2개의 흡수선과 대응하는 한 개의 중첩된 흡수선은 각각 사면체와 팔면체 자리의 $Fe^{3+}$의 피크로 밝혀졌다. $Fe^{2+}$와 $Fe^{3+}$의 정확한 함량비에 의해 화학분석치가 재계산되었으며, Fe 양이온의 사면체 자리와 팔면체 자리에 대한 정확한 자리점유율로 상세한 결정화학적 정보를 제공하였다. 상당한 함량의 $Fe^{3+}/tet$는 사면체 자리점유에 있어 $Fe^{3+}$가 $Al^{3+}$보다 우위를 보여준다. 결정화학적로 규명된 에이니그마타이트(AEN1)의 상세한 화학조성은 $(Na_{3.97}Ca_{0.03})(Ca_{0.11}Mn_{0.59}Fe^{2+}{_{8.07}}Ti_{2.07}Mg_{0.70}Fe^{3+}{_{0.43}}Al_{0.04})(Fe^{3+}{_{0.56}}Al_{0.18}Si_{11.26})O_{40}$으로 밝혀졌다.

• Bulletin of the Korean Chemical Society
• /
• 제19권6호
• /
• pp.654-660
• /
• 1998

$[Fe^{II}Fe^{III}BPLMP(OAc)_2](BPh_4)_2$ (1), a new model for the reduced form of the purple acid phosphatases, has been synthesized by using a dinucleating ligand, 2,6-bis[((2-pyridylmethyl)(6-methyl-2-pyridylmethyl)amino) methyl]-4-methylphenol (HBPLMP). Complex I has been characterized by X-ray diffraction method as having (μ-phenoxo)bis(acetato)diiron core. Complex 1 was crystallized in the monoclinic space group C2/c with the following cell parameters: a=41.620(6) Å, b=14.020(3) Å, c=27.007(4) Å, β=90.60(2)°, and Z=8. The iron centers in the complex 1 are ordered as indicated by the difference in the Fe-O bond lengths which match well with typical $Fe^{III}-O\; and\; Fe^{II}-O$ bond lengths. Complex 1 has been studied by electronic spectral, NMR, EPR, SQUID, and electochemical methods. Complex 1 exhibits strong bands at 592 nm, 1380 nm in $CH_3CN$ (ε = 1.0 × 103 , 3.0 × 102). These are assigned to $phenolate-to-Fe^{III}$ and intervalence charge-transfer transitions, respectively. Its NMR spectrum exhibits sharp isotropically shifted resonances, which number half of those expected for a valence-trapped species, indicating that electron transfer between $Fe^{II}\;and\;Fe^{III}$ centers is faster than NMR time scale. This complex undergoes quasireversible one-electron redox processes. The $Fe^{III}_2/Fe^{II}Fe^{III}\;and\;Fe^{II}Fe^{III}/Fe^{II}_2$ redox couples are at 0.655 and -0.085 V vs SCE, respectively. It has $K_{comp}=3.3{\times}10^{12}$ representing that BPLMP/bis(acetate) ligand combination stabilizes a mixed-valence $Fe^{II}Fe^{III}$ complex in the air. Complex 1 exhibits a broad EPR signal centered near g=1.55 which is a characteristic feature of the antiferromagnetically coupled high-spin $Fe^{II}Fe^{III}$ system $(S_{total}=1/2)$. This is consistent with the magnetic susceptibility study showing the weak antiferromagnetic coupling $(J= - 4.6\;cm^{-1},\; H= - 2JS_1{\cdot}S2)$ between $Fe^{II}\; and \;Fe^{III}$center.

• 한국결정성장학회지
• /
• 제9권2호
• /
• pp.185-190
• /
• 1999

$Al_2O_3/Fe$ 복합재료 제조는 반응소결법에 의한 2단계 공정을 통해서 제조되었으며 이 공정은 장비가 간단하고 near-net-shape이 가능한 장점이 있다.$Al_2O_3/Fe$ 복합재료를 제조하기 위해서 1차로 $650^{\circ}C$에서 5시간동안 산화/환원 처리를 행하고 $1200^{\circ}C$에서 2차로 소결처리를 행하였다. 제조된 복합재료의 상분석결과 $\alpha$-Fe 와 $\alpha$-$Al_2O_3/Fe$가 주된 상이었고 소량의 $FeAl_2O_4$가 검출되었다. 이 소량의 $FeAl_2O_4$상은 Fe가 $Al_2O_4$기공을 채우는 것을 방해함으로써 소결동안 미세구조 내에 약간의 기공을 발생시킨다.

• 한국세라믹학회지
• /
• 제34권7호
• /
• pp.738-746
• /
• 1997

MgO clinker and two kinds of dolomite clinkers with different microstructures and CaO contents were used as starting materials, and the effects of Fe2O3 addition on the properties of MgO and dolomite were investigated in the range of 2 to 8 wt% of Fe2O3 content. Secondary phases contributed to densification of MgO-Fe2O3 and dolomite-Fe2O3 were magnesioferrite and dicalciumferrite, respectively. Sinterabilities of MgO-Fe2O3 and dolomite-Fe2O3 were directly proportional to the amount of secondary phases. Also, sinterability of dolomite itself was dependent on the microstructure of starting material including distribution of CaO and MgO as well as the addition amount of Fe2O3. The flexural strength of MgO-Fe2O3 content was almost constant. The hydration resistance of dolomite with large size of MgO and discontinuous distribution of CaO was higher than that of dolomite with small size of MgO and continuous distribution of CaO. Also, the minimum content of Fe2O3 to prevent they hydration of dolomite was about 4wt%. As increasing Fe2O3 content, the penetration resistance of MgO-Fe2O3 was improved by the increment of magnesioferrite. On the other hand, the penetration resistance of dolomite-Fe2O3 was decreased because of the increment of dicalciumferrite having low melting point.