• Title/Summary/Keyword: Diffraction

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PREPARATION OF AMORPHOUS CARBON NITRIDE FILMS AND DLC FILMS BY SHIELDED ARC ION PLATING AND THEIR TRIBOLOGICAL PROPERTIES

  • Takai, Osamu
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2000.11a
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    • pp.3-4
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    • 2000
  • Many researchers are interested in the synthesis and characterization of carbon nitride and diamond-like carbon (DLq because they show excellent mechanical properties such as low friction and high wear resistance and excellent electrical properties such as controllable electical resistivity and good field electron emission. We have deposited amorphous carbon nitride (a-C:N) thin films and DLC thin films by shielded arc ion plating (SAIP) and evaluated the structural and tribological properties. The application of appropriate negative bias on substrates is effective to increase the film hardness and wear resistance. This paper reports on the deposition and tribological OLC films in relation to the substrate bias voltage (Vs). films are compared with those of the OLC films. A high purity sintered graphite target was mounted on a cathode as a carbon source. Nitrogen or argon was introduced into a deposition chamber through each mass flow controller. After the initiation of an arc plasma at 60 A and 1 Pa, the target surface was heated and evaporated by the plasma. Carbon atoms and clusters evaporated from the target were ionized partially and reacted with activated nitrogen species, and a carbon nitride film was deposited onto a Si (100) substrate when we used nitrogen as a reactant gas. The surface of the growing film also reacted with activated nitrogen species. Carbon macropartic1es (0.1 -100 maicro-m) evaporated from the target at the same time were not ionized and did not react fully with nitrogen species. These macroparticles interfered with the formation of the carbon nitride film. Therefore we set a shielding plate made of stainless steel between the target and the substrate to trap the macropartic1es. This shielding method is very effective to prepare smooth a-CN films. We, therefore, call this method "shielded arc ion plating (SAIP)". For the deposition of DLC films we used argon instead of nitrogen. Films of about 150 nm in thickness were deposited onto Si substrates. Their structures, chemical compositions and chemical bonding states were analyzed by using X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and infrared spectroscopy. Hardness of the films was measured with a nanointender interfaced with an atomic force microscope (AFM). A Berkovich-type diamond tip whose radius was less than 100 nm was used for the measurement. A force-displacement curve of each film was measured at a peak load force of 250 maicro-N. Load, hold and unload times for each indentation were 2.5, 0 and 2.5 s, respectively. Hardness of each film was determined from five force-displacement curves. Wear resistance of the films was analyzed as follows. First, each film surface was scanned with the diamond tip at a constant load force of 20 maicro-N. The tip scanning was repeated 30 times in a 1 urn-square region with 512 lines at a scanning rate of 2 um/ s. After this tip-scanning, the film surface was observed in the AFM mode at a constant force of 5 maicro-N with the same Berkovich-type tip. The hardness of a-CN films was less dependent on Vs. The hardness of the film deposited at Vs=O V in a nitrogen plasma was about 10 GPa and almost similar to that of Si. It slightly increased to 12 - 15 GPa when a bias voltage of -100 - -500 V was applied to the substrate with showing its maximum at Vs=-300 V. The film deposited at Vs=O V was least wear resistant which was consistent with its lowest hardness. The biased films became more wear resistant. Particularly the film deposited at Vs=-300 V showed remarkable wear resistance. Its wear depth was too shallow to be measured with AFM. On the other hand, the DLC film, deposited at Vs=-l00 V in an argon plasma, whose hardness was 35 GPa was obviously worn under the same wear test conditions. The a-C:N films show higher wear resistance than DLC films and are useful for wear resistant coatings on various mechanical and electronic parts.nic parts.

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Growth and Opto-electric Characterization of ZnSe Thin Film by Chemical Bath Deposition (CBD(Chemical Bath Deposition)방법에 의한 ZnSe 박막성장과 광전기적 특성)

  • Hong, K.J.;You, S.H.
    • Journal of Sensor Science and Technology
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    • v.10 no.1
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    • pp.62-70
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    • 2001
  • The ZnSe sample grown by chemical bath deposition (CBD) method were annealed in Ar gas at $45^{\circ}C$. Using extrapolation method of X-ray diffraction pattern, it was found to have zinc blend structure whose lattice parameter $a_o$ was $5.6687\;{\AA}$. From Hall effect, the mobility was likely to be decreased by impurity scattering at temperature range from 10 K to 150 K and by lattice scattering at temperature range from 150 K to 293 K. The band gap given by the transmission edge changed from $2.700{\underline{5}}\;eV$ at 293 K to $2.873{\underline{9}}\;eV$ at 10 K. Comparing photocurrent peak position with transmission edge, we could find that photocurrent peaks due to excition electrons from valence band, ${\Gamma}_8$ and ${\Gamma}_7$ and to conduction band ${\Gamma}_6$ were observed at photocurrent spectrum. From the photocurrent spectra by illumination of polarized light on the ZnSe thin film, we have found that values of spin orbit coupling splitting ${\Delta}so$ is $0.098{\underline{1}}\;eV$. From the PL spectra at 10K, the peaks corresponding to free bound excitons and D-A pair and a broad emission band due to SA is identified. The binding energy of the free excitons are determined to be $0.061{\underline{2}}\;eV$ and the dissipation energy of the donor -bound exciton and acceptor-bound exciton to be $0.017{\underline{2}}\;eV$, $0.031{\underline{0}}\;eV$, respectively.

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Growth of CdSe thin films using Hot Wall Epitaxy method and their photoelectrical characteristics (HWE방법에 의한 CdSe 박막 성장과 광전기적 특성)

  • Hong, K.J.;Lee, K.K.;Lee, S.Y.;You, S.H.;Shin, Y.J.;Suh, S.S.;Jeong, J.W.;Jeong, K.A.;Shin, Y.J.;Jeong, T.S.;Kim, T.S.;Moon, J.D.;Kim, H.S.
    • Journal of Sensor Science and Technology
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    • v.6 no.4
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    • pp.328-336
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    • 1997
  • The CdSe thin films were grown on the Si(100) wafers by a hot wall epitaxy method (HWE). The source and substrate temperature are $600^{\circ}C$ and $430^{\circ}C$ respectively. The crystalline structure of epilayers was investigated by double crystal X-ray diffraction(DCXD). Hall effect on the sample was measured by the van der Pauw method and studied on the carrier density and mobility dependence on temperature. From Hall data, the mobility was increased in the temperature range 30K to 150K by impurity scattering and decreased in the temperature range 150k to 293k by the lattice scattering. In order to explore the applicability as a photoconductive cell, we measured the sensitivity(${\gamma}$), the ratio of photocurrent to darkcurrent(pc/dc), maximum allowable power dissipation(MAPD), spectral response and response time. The results indicated that the photoconductive characteristic were the best for the samples annealed in Cu vapor compare with in Cd, Se, air and vacuum vapour. Then we obtained the sensitivity of 0.99, the value of pc/dc of $1.39{\times}10^{7}$, the MAPD of 335mW, and the rise and decay time of 10ms and 9.5ms, respectively.

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Removal Characteristic of Arsenic by Sand Media Coated with both Iron-oxide and Manganese-oxide (산화철 및 산화망간이 동시에 코팅된 모래 매질을 이용한 비소오염 제거특성 연구)

  • Kim, Byeong-Kwon;Min, Sang-Yoon;Chang, Yoon-Young;Yang, Jae-Kyu
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.7
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    • pp.473-482
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    • 2009
  • In this study, iron and manganese coated sand (IMCS) was prepared by mixing Joomoonjin sand with solutions having different molar ratio of manganese ($Mn^{2+}$) and iron ($Fe^{3+}$). Mineral type of IMCS was analyzed by X-ray diffraction spectroscopy. Removal efficiency of arsenic through As(III) oxidation and As(V) adsorption by IMCS having different ratio of Mn/Fe was evaluated. The coated amount of total Mn and Fe on all IMCS samples was less than that on sand coated with iron-oxide alone (ICS) or manganese-oxide alone (MCS). The mineral type of the manganese oxide on MCS and iron oxides on ICS were identified as ${\gamma}-MnO_2$ and mixture of goethite and magnetite, respectively. The same mineral type was appeared on IMCS. Removed amount As(V) by IMCS was greatly affected by the content of Fe rather than by the content of Mn. Adsorption of As(V) by IMCS was little affected by the presence of monovalent and divalent electrolytes. However a greatly reduced As(V) adsorption as observed in the presence of trivalent electrolyte such as $PO_4\;^{3-}$. As(III) oxidation efficiency by MCS in the presence of NaCl or $NaNO_3$ was two times greater than that in the presence of $PO_4\;^{3-}$. Meanwhile a greater As(III) oxidation efficiency was observed by IMCS in the presence of $PO_4\;^{3-}$. This was explained by the competitive adsorption between phosphate and arsenate on the surface of IMCS.

Alteration Zoning, Mineral Assemblage and Geochemistry of the Hydrothermal Clay Deposits Related to Cretaceous Felsic Magmatism in the Haenam Area, Southwest Korea (한국 서남부, 해남지역에서 백악기 산성마그마티즘에 관련된 열수점토광상의 누대분배, 광물조합의 지구화학적 연구)

  • Kim, In Joon
    • Economic and Environmental Geology
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    • v.25 no.4
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    • pp.397-416
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    • 1992
  • In the present study, three clay deposits, named the Seongsan, Ogmaesan and Haenam deposits, were investigated. The altered zones are recognized in the hydrothermally altered rocks of the clay deposits from the center of the alteration to the margin: Kaolin, Kaolin-Quartz, Quartz, Sericite and Chlorite zones in the Seongsan deposits; Quartz zone, Alunite zone, Kaolin zone, Sericite zone and Chlorite zone in the Ogmaesan deposits; Quartz zone, Pyrophyllite zone, Sericite zone and Chlorite zone in the Haenam deposits. These zones can be grouped into two types of alteration: Acidic alteration such as Pyrophyllite zone, Alunite zone, Quartz zone, Kaolin zone, Kaolin-Quartz zone and a part of Sericite zone; Propylitic alteration such as Chlorite zone and a part of Sericite zone. All clay deposits belong to high-sulfidation (acid-sulfate) system. The rocks of the acidic alterations are composed of pyrophyllite, alunite, kaolin minerals, sericite, quartz and pyrite. On the basis of bulk chemical compositions, it was found that some components such as $SiO_2$, $TiO_2$, $Fe_2O_3$, FeO, MgO, CaO, $K_2O$ and $Na_2O$ were mobilized considerably from the original rocks. The mobility of these major elements is related to, and controls, mineral assemblages in each altered zone. Polytypes of sericite are determined as $2M_1$ and 1M by X-ray diffraction method. The amount of $2M_1$ is nearly equal to that of 1M in the Seongsan deposits whereas $2M_1$ is less and higher than that of 1M in the Ogmaesan and the Haenam deposits. These facts indicate that formation temperature of sericite is relatively high in the Haenam deposits, moderate in the Seongsan deposits, and low in the Ogmaesan deposits. The ratios of Na/(K+Na) for alunite in the Ogmaesan deposits determined by electron microprobe analyzer (EPMA) are higher than those in the Seongsan deposits. Thus, the alunite of the Ogmaesan deposits must have been formed from the solutions with relatively high aqueous Na/(K+Na) ratios and low pH at a high temperature rather than that of the Seongsan deposits. From all data, it is clarified that alunite is hypogene in origin, and has been formed by oxidation of hydrogen sulfide in the steam-heated environment, and that alunite has been produced by the spectacular solfataric alteration observed at the surface of some present-day hydrothermal systems.

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Arsenic Removal Using Iron-impregnated Ganular Activated Carbon (Fe-GAC) of Groundwater (철침착 입상활성탄(Fe-GAC)을 이용한 지하수 내 비소 제거기술)

  • Yoon, Ji-Young;Ko, Kyung-Seok;Yu, Yong-Jae;Chon, Chul-Min;Kim, Gyoo-Bum
    • Economic and Environmental Geology
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    • v.43 no.6
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    • pp.589-601
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    • 2010
  • Recently it has been frequently reported arsenic contamination of geologic origin in groundwater. The iron-impregnated ranular activated carbon (Fe-GAC) was developed for effective removal of arsenic from groundwater n the study. Fe-GACs were prepared by impregnating iron compounds into a supporting medium (GAC) with 0.05 M iron nitrate solution. The materials were used in arsenic adsorption isotherm tests to know the effect of iron impregnation time, batch kinetic tests to understand the influence of pH, and column tests to evaluate for the preliminary operation of water treatment system. The results showed that the minimum twelve hours of impregnation time were required for making the Fe-GAC with sufficient iron content for arsenic removal, confirmed by a high arsenic adsorption capacity evaluated in the isotherm tests. Most of the impregnated iron compounds were iron hydroxynitrate $Fe_4(OH)_{11}NO_3{\cdot}2H_2O$ but a mall quantity of hematite was also identified in X-ray diffraction(XRD) analysis. The batch isotherms of Fe-GAC for arsenic adsorption were well explained by Langmuir than Freundlich model and the iron contents of Fe-GAC have positive linear correlations on logarithmic plots with Freundlich distribution coefficients ($K_F$ and Langmuir maximum adsorption capacities ($Q_m$. The results of kinetic experiments suggested hat Fe-GAC had he excellent arsenic adsorption capacities regardless of all pH conditions except for pH 11 and could be used a promising adsorbents for groundwater arsenic removal considering the general groundwater pH range of 6-8. The pseudo-second order model, based on the assumption that the ate-limiting step might be chemisorption, provided the best correlation of the kinetic experimental data and explained the arsenic adsorption system f Fe-GAC. The column test was conducted to valuate the feasibility of Fe-GAC use and the operation parameters in arsenic groundwater treatment system. The parameters obtained from the column test were the retardation actor of 482.4 and the distribution coefficient of 581.1 L/mg which were similar values of 511.5-592.5 L/mg acquired from Freundlich batch isotherm model. The results of this study suggested that Fe-GAC could be used as promising adsorbent of arsenic removal in a small groundwater supply system with water treatment facility.

Solubility Improvement of Cuttle Bone Powder Using Organic Acids (유기산처리에 의한 갑오징어갑 분말의 가용성 개선)

  • KIM Jin-Soo;CHO Moon-LAE;HEU Min-Soo;CHO Tae-Jong;AN Hwa-Jin;CHA Yong-Jun
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.36 no.1
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    • pp.11-17
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    • 2003
  • As a pan of a study on effective use of seafood processing by-products, such as cuttle bone as a calcium source, we examined on the kind of organic acid (acetic acid and lactic acid), reaction concentration (mole ratio of calcium to mole of organic acid), reaction temperature $(20\~60^{\circ}C)$ and reaction time (6$\~$24 hours) as reaction conditions for the solubility improvement of cuttle bone powder. The high soluble cuttle bone powder was also prepared from the optimal reaction conditions and partially characterized. From the results on examination of reaction conditions, the high soluble cuttle bone powder was prepared with 0.4 in mole ratio of a calcium to mole of a acetic acid at room temperature for 12 hours, Judging from the patterns of IR and X-ray diffraction, the main component of the high soluble cuttle bone powder was presented as a form of calcium acetate, and a scanning electron micrograph showed an irregular form. The soluble calcium content in the high soluble cuttle bone powder was $5.3\%$ and it was improved about 1,380 times compared to a raw cuttle bone powder. For the effective use of the high soluble cuttle bone powder as a material for a functional improvement in processing, it should be used after the calcium treatment at room temperature for about 1 hour in tap water or distilled water. from these results, we concluded that it is possible to use the high soluble cut시e bone powder as a material for a functional improvement in processing.

Mechanical Properties of Granulated Ground Blast Furnace Slag on Blended Activator of Sulfate and Alkali (황산염 및 알칼리계의 혼합 활성화제에 대한 고로슬래그미분말의 역학적 특성)

  • Kim, Tae-Wan;Jun, Yu-Bin;Eom, Jang-Sub
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.19 no.5
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    • pp.104-111
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    • 2015
  • This study shows the mechanical properties of alkali-activated slag cement (AASC) synthesized using sulfate with NaOH solution. The used sulfates were calcium sulfate ($CaSO_4$, denoted CS) and sodium sulfate ($Na_2SO_4$, denoted SS). The replacement ratio of sulfates was 2.5, 5.0, 7.5 and 10.0% by weight of slag. NaOH solution of 2M and 4M concentration was used. A sample was activated with sulfate and activated with blended activator (blending NaOH solution with sulfate) respectively. 24 mix ratios were used and the water-binder weight ratio for the test was set 0.5. This research carried out the compressive strength, flexural strength, ultrasonic pulse velocity (UPV), absorption and X-ray diffraction (XRD). In the case of samples with CS, sample with 7.5% CS, sample with 2M NaOH+5.0% CS and sample with 4M NaOH+5.0% CS showed the good performance in the strength development. In the case of samples with SS, sample with 10.0% SS, sample with 2M NaOH+7.5% SS and sample with 4M NaOH+2.5% SS obtained good performance in strength. The results of UPV and water absorption showed a similar tendency to the strength properties. The XRD analysis of samples indicated that the hydration products formed in samples were ettringite, CSH and silicate phases. In this study, it is indicated that when compared to the use of sulfate only, the use of both sulfate and NaOH solution makes mechanical properties of AASC better.

Crystallographic Studies of $Ag^+$-and $Ca^{2+}$- Exchanged Zeolite A Reacting with Rubidium Vapor (루비듐 증기와 반응한 $Ag^+$ 이온과 $Ca^{2+}$ 이온으로 치환된 제올라이트 A의 결정학적 연구)

  • Han, Young-Wook;Song, Seong-Hwan;Kim, Yang
    • Journal of the Mineralogical Society of Korea
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    • v.4 no.1
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    • pp.22-31
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    • 1991
  • Three crystal structures of dehydrated $Ag^+$-and $Ca^{2+}$- exchanged zeolite $A(Ag_4Ca_4-A,\;Ag_^Ca_3-A,\;and\;Ag_8Ca_2-A)$ treated at 250${\circ}C$ with 0.1 Torr of Rb vapor have been determined by single-crystal x-ray diffraction techniques in the cubic space group Pm3m at 21(1)${\circ}C$ (a=12,271(1)${\AA}$, 12.255(1)${\AA}$, and 12.339(1)${\AA}$, respectively). Their structures were refined to the final error indices. R(weighted) of 0.072 with 130 reflections, 0.050 with 110 reflections, and 0.083 with 86 reflections, respectively, for which $I>3{\rho}(I)$. In each structure, Rb species are found at three different crystallographic sites:3$Rb^+$+ions per unit cell are located at 8-ring centers, ca. 5.6 to 6.4 $Rb^+$ ions are found opposite 6-rings on threefold axes in the large cavity, and ca. 2.5 to 3.0 $Rb^+$ ions are found on threefold axes in the sodalite unit. Also, Ag species are found at two different crystallographic stites: ca. 0.7 to 2.1 $Ag^+$ lie opposite 4-rings and ca. 2.2 to 4.8 Ag atoms are located near the center of the large cavity. In these structures, the numbers of Ag atoms per unit cell are 2.2, 2.4, and 4.8, respectively, and these may form hexasilver clusters at the centers of the large cavities. The $Rb^+$ ions, by blocking 8-rings, may have prevented silver from migrating out of the structure. Each hexasilver cluster is stabilized by coordination to up to 13 $Rb^+$ions. An excess absorption of about 0.8 Rb atom per unit cell indicates that the presence of a triangular symmetric $(Rb_3)2^{+}$ cation in sodalite cavity. At least one large-cavity six-ring $Rb^+$ ion must necessarily approach this cluster and may be viewed as a member of it to give $(Rb)_4^{3+}$, $(Rb)_5^{4+}$ or $(Rb)_6^{5+}$.

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Synthesis and Rietveld Structure Refinement of Mn-Tourmalines (Tsilaisite) (Mn-전기석(Tsilaisite)의 합성 및 리트벨트 구조분석)

  • Grover John;Choi Jin-Beom
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.1 s.47
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    • pp.15-29
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    • 2006
  • Synthetic Mn-tourmalines (tsilaisite) were obtained by hydrothermal synthesis under the condition of 2 Kbar, $375{\sim}700^{\circ}C$, and 50 day-run-time with complete substitution of Mg in dravite by Mn (Mn%=0, 25, 50, 75, and 100%). They are all 6 samples containing Mn-tourmaline with some amounts of albite, spessartine, rhodocrosite, phlogopite etc, showing different synthetic condition of temperature and Mn composition. Synthetic Mn-tourmalines are of site deficiency in X-site ($0.53{\sim}0.68$) more than that of natural ones (approx. $0.2{\sim}0.3$) and show Mn cations occupying Y-site less than expected with initial experiments, leading to failure in synthesis of end-member tsilaisite. Rietveld structural refinements reveal that $R_{wp}$ ($R_{p}/R_{exp}$) is in the range of 13.35 and 18.62%, $R_{B}$ and S (CofF) are $4.85{\sim}6.25%$ (S-18: 8.57%), $1.31{\sim}1.59$ (S-18: 1.81), respectively. Unit cell parameters (space group R3m, z=3) are ${\alpha}=15.8994\;{\AA}$ and $c=7.1846\;{\AA}$ in average (S-18: ${\alpha}=15.9491\;{\AA},\;c=7.1773\;{\AA}$). Average bond lengths of and are $2.67{\sim}2.69\;{\AA}$ (S-18: $2.65\;{\AA}$) and $2.00{\sim}2.02\;{\AA}$ (S-18: $1.96\;{\AA}$), respectively. Ditrigonality (${\delta}$) are in the range of 0.022 and 0.031 (S-18: 0.061), indicating degrading symmetry with increase of Mn content.