• 제목/요약/키워드: powder X-ray diffraction

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Structural and Magnetic Properties of the Brownmillerite $Ca_2Al_xFe_{2-x}O_5$ System

  • 김귀야;로권선;여철현
    • Bulletin of the Korean Chemical Society
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    • 제16권10호
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    • pp.934-938
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    • 1995
  • A series of solid solutions in the Ca2AlxFe2-xO5 (x=0.00, 0.50, 0.66, 1.00 and 1.34) system with brownmillerite structure has been synthesized at 1100 ℃ under an atmospheric air pressure. The solid solutions are analysed by powder x-ray diffraction analysis, Mohr salt titration, thermal analysis, and Mossbauer spectroscopic analysis. The x-ray diffraction analysis assigns the compositions of x=0.00 and 0.50 to the space group Pcmn and those of x=0.66, 1.00, and 1.34 to the Ibm2. Mo&ssbauer spectra have shown the coordination state and disordering of Al3+ and Fe3+ ions. The substituting preference of Al3+ ions for the tetrahedral site decreases with increasing x value. Magnetic susceptibility of the system has been measured in the temperature range of 5 K to 900 K. The solid solutions of the compositions of x=0.00, 0.50 and 0.66 have shown a thermal hysteresis and the thermoremanent magnetization gap decreases with increasing x value in the above systems. However the compositions of x=1.00 and 1.34 do not show the hysteresis. The exchange integral is calculated from Fe3+ ion occupancy ratio. The integral decreases with x value and thus the magnetic transition temperature decreases with the increasing x value.

Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

  • Kim, Tae-Hyun;Heo, Il;Paek, Seung-Min;Park, Chung-Berm;Choi, Ae-Jin;Lee, Sung-Han;Choy, Jin-Ho;Oh, Jae-Min
    • Bulletin of the Korean Chemical Society
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    • 제33권6호
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    • pp.1845-1850
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    • 2012
  • Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.

Fabrication of Fe-TiB2 Composite Powder by High-Energy Milling and Subsequent Reaction Synthesis

  • Khoa, H.X.;Tuan, N.Q.;Lee, Y.H.;Lee, B.H.;Viet, N.H.;Kim, J.S.
    • 한국분말재료학회지
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    • 제20권3호
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    • pp.221-227
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    • 2013
  • $TiB_2$-reinforced iron matrix composite (Fe-$TiB_2$) powder was in-situ fabricated from titanium hydride ($TiH_2$) and iron boride (FeB) powders by the mechanical activation and a subsequent reaction. Phase formation of the composite powder was identified by X-ray diffraction (XRD). The morphology and phase composition were observed and measured by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively. The results showed that $TiB_2$ particles formed in nanoscale were uniformly distributed in Fe matrix. $Fe_2B$ phase existed due to an incomplete reaction of Ti and FeB. Effect of milling process and synthesis temperature on the formation of composite were discussed.

영동 일라이트 분말 제품의 규격에 따른 입도 특성 (Particle Size Characteristics with the Specification of Yeongdong Illite Powder Products)

  • 백은지;이유나;김은정;김영석;김현나
    • 광물과 암석
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    • 제36권4호
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    • pp.345-353
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    • 2023
  • 본 연구는 상업용 영동 일라이트 분말 제품의 판매 규격, 즉 메쉬(mesh)에 따른 구성광물, 입도, 화학조성의 차이를 조사하여, 일라이트 분말 제품의 특성을 이해하고 다양한 활용 분야를 개척하기 위한 광물학적 데이터베이스로 활용하고자 하였다. 충청북도 영동군의 광산을 보유한 두 곳의 회사에서 제공받은 상업용 일라이트 분말 시료를 X-선 회절 분석, 레이저 회절 입도 분석, 주사전자현미경 분석, X-선 형광 분석을 이용해 조사하였다. X-선 회절 분석 결과, 두 광산의 일라이트 분말 제품에는 주로 일라이트 및 백운모, 석영, 사장석이 존재하며, 이는 각 광산의 광석의 구성광물과 일치하는 경향을 보인다. 레이저 회절 입도 분석에서는 제품 규격에 따라 입자 크기의 차이가 나타났으며, 입도의 균일성은 메쉬가 높아질수록 증가하는 경향을 보였다. 주사전자현미경 분석에서는 입자의 형태와 크기가 규격에 따라 다르게 나타났다. 일라이트 입자의 크기는 제품의 규격 메쉬에 따른 차이가 크게 없으며, 주로 장석 및 석영의 입자 크기에 변화가 발생하는 것으로 나타났다. 또한, 시료의 화학 조성은 광산마다 다소의 차이가 있으나, 규격별로 큰 차이는 나타나지 않았다. 이러한 결과를 토대로, 상업용 일라이트 분말의 활용 분야를 고려할 때 규격에 따른 특성 변화를 고려하여 선택하는 것이 중요하다. 본 연구 결과는 상업용 일라이트 분말의 다양한 응용 가능성을 제시하며, 산업적 활용 및 새로운 기술 개발에 기여할 것으로 기대된다.

Softening-hardening Mechanisms in the Direct Hot-extrusion of Aluminium Compacts

  • Zubizarreta, C.;Arribas, I.;Gimenez, S.;Iturriza, I.
    • 한국분말야금학회:학술대회논문집
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    • 한국분말야금학회 2006년도 Extended Abstracts of 2006 POWDER METALLURGY World Congress Part2
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    • pp.718-719
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    • 2006
  • Two different commercial aluminium powder grades have been densified by direct hot extrusion. The extrusion temperature was $425^{\circ}C$, with an extrusion ratio of 1:16. Prior to extrusion, some green compacts were pre-sintered ($500^{\circ}C$). The evolution of the extrusion load during the process and the hardness of the final products have been investigated. Additionally, microstructural characterization by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Backscattered Diffraction (EBSD) was carried out. The obtained results evidence grain refinement. Additionally, inter-metallic precipitation, dynamic recovery and geometric dynamic recrystallization take place depending on some process variables, powder composition, heat treatment, strain $\ldots$

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APPLICATION STUDY OF CHEMOINFOMETRICAL NEAR-INFRARED SPECTROSCOPY IN PHARMACEUTICAL INDUSTRY

  • Otsuka, Makoto;Kato, Fumie;Matsuda, Yoshihisa
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.2111-2111
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    • 2001
  • A chemoinfometrical method for evaluating the quantitative determination of crystallinity one polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the and compared with the conventional powder X-ray diffraction method was performed. [Method] The pPure a and g forms of indomethacin (IMC) were prepared by reportedusing published methods. Six kinds of standard samples obtained by physically mixing of a and g forms. After the powder X-ray diffraction profiles of samples have been measured, the intensity values were normalized to against the intensity of silicon powder as the as an external standard. The calibration curves for quantification of crystal content were based upon the total relative intensity of four diffraction peaks from of the form g crystal. FT-NIR spectra of six calibration sample sets were recorded 5 times with the NIR spectrometer (BRAN+LUEBBE). Chemoinfometric analysis was performed on the NIR spectral data sets by applying the principal component regression (PCR). [Results] The relation between the actual and predicted polymorphic contents of form g IMC measured using by the X-ray diffraction method shows a good straight linen linear relation., and it has slope of 0.023, an intercept of 0.131 and a correlation coefficient of 0.986. PCR analyses wereis was performed based on normalized NIR spectra sets offer standard samples of known content of IMC g form. IMC. A calibration equation was determined to minimize the root mean square error of the predictionthe prediction. Figure 1 shows a plot of the calibration data obtained by NIR method between the actual and predicted contents of form g IMC. The predicted values were reproducible and had a smaller standard deviation. Figure 2 shows that the plot for the predicted transformation rate (%) of form a IMC to form g as measured by X-ray diffractomeoy against to those as measured by NIR method. The plot has a slope of 1.296, an intercept of 1,109, and a correlation coefficient of 0.992. The line represents a satisfactory correlation between the two predicted values of form g IMC content. Thus NIR spectroscopy is an effective method for the evaluation to the pharmaceutical products of quantitative of polymorph.

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초미립 MnxZn1-xFe2O4(x = 0.69~0.74)분말의 제조 및 자기적 성질 (Synthesis of Ultra Eine MnxZn1-xFe2O4(x = 0.69~0.74) Powder and Its Magnetic Properties)

  • 곽재은;이완재
    • 한국분말재료학회지
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    • 제9권6호
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    • pp.449-454
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    • 2002
  • $MnxZn_{1-x}Fe_2O_4$ (x=0.69~0.74) powders synthesized by the thermal decomposition of organic acid salts. The obtained powders were uniform in composition and ultra-fine particle with about 400 nm. The amount of spinel phase of these powders was about 50% in X-ray diffraction patterns. The calcination of powder was carried out at $900^{\circ}C$ for 2 hours in air. After the powders were calcined. the mean size of powder was about 500 nm and the amount of spinel phase was increased over about 65%. The maximum amount of spinel phase was about 75% in the specimen of X=0.72. The magnetic properties of calcined $Mn_{0.72}Zn_{0.28}Fe_2O_4$ powders were the best among the different among the different compositions.

$LiMn_{2-y}M_{y}O_{4}$(M=Mg, Zn) 정극의 충방전 용량 및 AC 임피던스 특성 (Charge-discharge capacity and AC impedance of $LiMn_{2-y}M_{y}O_{4}$(M=Mg, Zn) cathode)

  • 정인성;위성동;이승우;구할본
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2001년도 하계학술대회 논문집
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    • pp.455-458
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    • 2001
  • Spinel $LiMn_{2-y}$$M_{y}$ $O_4$powder was prepared solid-state method by calcining the mixture of LiOH - $H_2O$, Mn $O_2$, ZnO and MgO at 80$0^{\circ}C$ for 36h. To investigate the effect of substitution with Mg, Zn cation, charge-discharge experiments and initial impedance spectroscopy performed. The structure of $LiMn_{2-y}$$M_{y}$ $O_4$crystallites was analyzed from powder X-ray diffraction data as a cubic spinel, space group Fd3m. all cathode material showed spinel phase based on cubic phase in X-ray diffraction. Ununiform which calculated by (111) face and (222) face was constant in spite of the change of y value, except PUf\ulcorner LiM $n_2$ $O_4$. The discharge capacities of the cathode for the cation subbstitUtes $LiMn_{2-y}$$M_{y}$ $O_4$/Li cell at the 1st cycle and at the 40th cycle were about 120~124 and 108~112mAh/g except LiM $n_{1.9}$Z $n_{0.1}$ $O_4$/Li cell, respectively. This cell capacity is retained by 93% after 40th cycle. AC impedance of $LiMn_{2-y}$$M_{y}$ $O_4$/Li cells revealed the similar resistance of about 65~110$\Omega$ before cycling. before cycling.g.g.

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$LiMn_{2-y}M_{y}O_4$ 정극 활물질의 전기화학적 특성 - I. $LiMn_{2-y}Mg_{y}O_4$의 결정 구조 및 AC Impedance 특성 (The Electrochemical Characterization of $LiMn_{2-y}M_{y}O_4$ Cathode Material - I. Crystal Structure and AC Impedance Properties of $LiMn_{2-y}Mg_{y}O_4$)

  • 정인성;김종욱;구할본;김형곤;손명모
    • 한국전기전자재료학회논문지
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    • 제14권4호
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    • pp.309-315
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    • 2001
  • Crystallized $LiMn_{2-y}Mg_{y}O_4$ powder was prepared by calcing the mixture of LiOH.$H_2O$, $MnO_2$ and MgO at $800^{\circ}C$ for 36h in an air atmosphere. The structure of $LiMn_{2-y}Mg_{y}O_4$ crystallites was analyzed from powder X-ray diffraction data as a cubic spinel, space group Fd3m. Though all cathode material showed spinel phase based on cubic phase in X-ray diffraction, other peaks gradually exhibited and became intense with increasing y value in $LiMn_{2-y}Mg_{y}O_4$. However, ununiform which calculated by (111) face and (222) face was constant in spite of the increase of y value, except pure $LiMn_2O_4$. AC impedance of Li/$LiMn_{2-y}Mg_{y}O_4$ cells revealed the similar resistance of about $70\Omega$ before cycling. In addition, The impedance of Li/$LiMn_{1.9}Mg_{0.1}O_4$ cell changed during charge and discharge or after cycling.

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VLS 합성법을 이용한 ZnO 나노구조의 특성 (ZnO Nanostructure Characteristics by VLS Synthesis)

  • 최유리;정일현
    • 공업화학
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    • 제20권6호
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    • pp.617-621
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    • 2009
  • Zinc oxide (ZnO)을 금(Au)과 fluorine-doped tin oxide (FTO) 촉매로 산화실리콘($SiO_2$) 기판에 산화아연입자 20 nm, $20{\mu}m$를 각각 사용하여 기체-액체-고체(VLS) 합성법으로 성장시켰다. 나노로드의 표면특성, 화학조성, 그리고 결정특성을 엑스레이회절(X-ray diffraction (XRD)), 에너지 분산형 X선 분광기(Energy-dispersive X-ray spectroscopy (EDX)), 표면 방출주사현미경(Field-emission scanning electron microscope (FE-SEM))으로 분석하였다. ZnO의 입자 크기 뿐만 아니라 결정형태가 성장에 크게 영향을 미쳤다. ZnO의 모든 나노구조가 6방정계(六方晶系), 단일결정구조를 가지고 있었다. 최적온도는 $1030^{\circ}C$, 입자크기는 20 nm이다. 그러므로 Au 대신 플루오린 첨가 도핑으로 전기음성도가 증가된 FTO 증착에 의해서 생성된 나노로드는 경제성 있는 대체물질로서의 가치가 있을 것으로 사료된다.