• Title/Summary/Keyword: 정량 X-선 회절분석

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Effects of Aging on Properties of MgO-Partially Stabilized Zirconia (마그네시아 부분안정화 지르코니아 소결체의 특성에 미치는 열처리 효과)

  • 정형진;오영제;이홍림
    • Journal of the Korean Ceramic Society
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    • v.24 no.3
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    • pp.243-250
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    • 1987
  • The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.

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Biocompatibility and Surface Characteristics of (Si,Mn)-HA Coated Ti-Alloy by Plasma Electrolytic Oxidation (PEO법으로 (Si,Mn)-HA 코팅된 치과 임플란트용 Ti 합금의 생체적합성 및 표면특성)

  • Gang, Jeong-In;Son, Mi-Gyeong;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.83-83
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    • 2017
  • 생체재료의 표면은 이식과 동시에 생체계면의 역할을 하게 되어, 일련의 생물학적 반응이 시작되고 진행되는 중요한 장소가 된다. 초기에 생체계면에서 일어나는 단백질 흡착이나 염증반응을 비롯한 생물학적 반응들은 궁극적으로 임플란트의 성패를 좌우할 만큼 중요하다. 골융합을 개선하기 위한 다른 방법으로 생체불활성의 타이타늄 (Ti)과 골조직의 능동적인 반응을 이루기 위해 생체활성 표면을 부여함으로서 계면에서의 골형성 반응을 증진시키는 방법이 이용된다. 생체불활성의 Ti과 Ti합금은 골조직과 직접적인 결합을 이루지 못하므로, 골조직과의 반응을 향상하기 위해 여러 종류의 생체활성 재료를 코팅하는 방법이 연구되어 왔고, 이 중 생체의 변화와 가장 유사한 하이드록시아파타이트 코팅이 가장 대중적인 방법으로 사용되었으며 이는 초기 골형성을 촉진하는 것으로 알려졌다. 치과용 임플란트의 표면형상과 화학조성이 골 융합에 영향을 미치는 가장 중요한 인자이므로 최근의 연구동향은 이들 두 가지 표면특성을 결합함으로서 결과적으로 최적의 골세포반응을 유도하고, 골융합 후 골조직과의 micromechanical interlocking에 의해 임플란트의 안정성에 중요한 역할을 하는 마이크론 단위의 표면조도와 표면 구조를 유지하면서, 부가적으로 골 조직 반응을 능동적으로 개선할 수 있는 생체활성 성분을 부여하여 골 융합에 상승효과를 이루기 위한 표면처리법에 관해 많은 연구가 요구되어지고 있다. 따라서 골을 구하는 원소인 망간과 실리콘으로 치환된 하이드록시아파타이트를 플라즈마 전해 산화법으로 코팅하여 세포와 잘 결합할 수 있는 표면을 제공함으로써 골 융합과 치유기간을 단축시킬 수 있을 것으로 사료된다. 실험방법은 시편은 치과 임플란트 제작 합금인 Ti-6Al-4V ELI disk (grade 5, Timet Co., USA; diameter, 10 mm, thickness, 3 mm)이며, calcium acetate monohydrate, calcium glycerophosphate, manganese(II) acetate tetrahydrate, sodium metasilicate을 설계조건에 따라 혼합 제조된 전해질 용액을 이용하여 플라즈마 전해 산화법으로 표면 코팅을 실시하였다. 각 시편의 플라즈마 전해시 전압은 280V로 인가하였고, 전류밀도는 70mA로 정전류를 공급하여 해당 인가전압 도달 후 3분 동안 정전압 방식을 유지하였다. 코팅된 피막 표면을 주사전자현미경과 X-선 회절분석을 통하여 미세구조 및 결정상을 관찰하였다. 또한 코팅된 표면의 생체활성 평가는 정량적으로 평가하기 위해 동전위시험과 AC 임피던스를 통하여 시행하였다. 분극거동을 확인하기 위해 potentiostat (Model PARSTAT 2273, EG&G, USA)을 이용하여 구강 내 환경과 유사한 $36.5{\pm}1^{\circ}C$의 0.9 wt.% NaCl에서 실시하였다. 전기화학적 부식 거동은 potentiodynamic 방법으로 조사하였고 인가전위는 -1500 mV에서 2000 mV까지 분당 1.67 mV/min 의 주사속도로 인가하여 시험을 수행하였다. 임피던스 측정은 potentiostat (Model PARSTAT 2273, EG&G, USA)을 이용하였으며, 측정에 사용한 주파수 영역은 10mHz ~ 100kHz 까지의 범위로 하여 조사하였고 ZSimWin(Princeton applied Research, USA) 소프트웨어를 사용하여 용액의 저항, 분극 저항 값을 산출하였다. 망간의 함량이 증가할수록 불규칙한 기공을 보였으며, 실리콘은 $TiO_2$ 산화막 형성을 저해하는 경향을 확인할 수 있었다. 단독으로 표면을 처리한 경우보다 두 가지 원소를 이용해 복합 표면처리를 시행한 경우가 내식성이 좋아 임플란트과의 골 유착에 긍정적인 영향을 미칠 것으로 사료된다.

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Effect of Styrene and Maleic Anhydride Content on Properties of PP/Pulp Composites and Reactive Extrusion of Random PP (랜덤 PP의 반응압출 및 PP/Pulp 복합체 특성에 대한 스티렌과 무수말레인산 함량의 영향)

  • Lee, Jong Won;Kim, Ji Hyun;Kim, Youn Cheol
    • Applied Chemistry for Engineering
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    • v.25 no.3
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    • pp.318-323
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    • 2014
  • In order to analyze the effect of maleic anhydride (MAH) content and styrene monomer (SM)/MAH mole ratio on reactive extrusion of maleic anhydride grafted random polypropylenes (MAH-g-rPP), MAH-g-rPPs were prepared by using a twin screw extruder. MAH contents were 0.5, 1.0, 3.0, and 5.0 phr and SM/initiator mole ratio was 0.0, 1.0, and 2.0. Dicumyl peroxide (DCP) was used as an initiator. The graft degree of MAH was confirmed by the existence of carbonyl group (C = O) stretching peak at $1700cm^{-1}$ from FT-IR spectrum. The degree of graft reaction increased up to 3.0 phr MAH and showed the optimum value at 1.0 SM/MAH mole ratio from the area ratio of C = O and C-H stretching peak. Thermal and crystallization properties of MAH-g-rPP and PP/MAH-g-rPP/pulp composites were investigated by DSC, TGA, XRD, and POM. There was a decrease in non-isothermal crystallization temperature of PP/MAH-g-PP/pulp composites. Based on tensile properties and SEM pictures for the fractured surface of PP/MAH-g-PP/pulp composites, MAH content of 1.0 wt% and SM/MAH mole ratio of 1.0 were the optimum formulation as the compatibilizer. The rheological properties of the composites were measured by dynamic Rheometer to compare the processability of the composites with and without compatibilizer. The power law index showed slightly low value at the composites with compatibilizer.

Relationship between Physicochemical Properties, Heavy Metal Contents and Magnetic Susceptibility of Soils (토양의 물리화학적 특성, 중금속 함량, 대자율 간의 상호관계 연구)

  • Chon, Chul-Min;Park, Jeong-Sik;Kim, Jae-Gon;Lee, Youn-Soo
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.4
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    • pp.281-295
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    • 2010
  • This paper deals with magnetic susceptibility, mineralogy, soil properties (pH, EC, CEC, loss on ignition), iron and manganese oxides, the content and partitioning of heavy metals (As, Cd, Cr, Cu, Ni, Pb, Zn), and their mutual relationship in the soil samples of an unpolluted, abandoned mine area, and industrial complex area. The various minerals derived from weathered bedrock were identified by X-ray diffraction in the unpolluted soil samples, except for the magnetic minerals. XRD analysis also revealed the existence of hematite and magnetite related to mine tailings and waste rocks in the abandoned mine area samples. The industrial complex area samples had carbonate minerals, such as calcite and dolomite, that might be due to anthropogenic deposition. The sum of the reducible, oxidizable, and residual fractions was over 80% for the abandoned mine area samples and over 50% for the industrial complex area samples using the sequential extraction method. The industrial complex area samples had a relatively high carbonate fraction that was associated with carbonate minerals. The content of aqua regia-extractable Fe, Mn, As, and Zn had a high positive correlation with the content of the dithionite-citrate-bicarbonate (DCB)-extractable method related to Fe/Mn oxide phases. The 54% and 58% of aqua regia-extractable Fe and As content, respectively, acted together with the concentrations of the DCB-extractable phases. Magnetic susceptibility values of total samples ranged from 0.005 to $2.131{\times}10^{-6}m^3kg^{-1}$. The samples including iron oxide minerals, such as hematite and magnetite, had a high magnetic susceptibility. The magnetic susceptibility showed a significant correlation with the heavy metals, Cd (r=0.544, p<0.05), Cr (r=0.714, p<0.01), Ni (r=0.645, p<0.05), Pb (r=0.703, p<0.01), and Zn (r=0.496, p<0.01), as well as Fe (r=0.608, p<0.01) and Mn (r=0.615, p<0.01). The aqua regia-extractable Fe and Mn content had a significant positive correlation with Cd, Cr, Cu, Ni, and Zn. However, the DCB-extractable Fe and Mn content had a significant positive correlation with As and Ni, indicating that the heavy metals were associated with Fe and Mn oxide minerals.

Characterization on the Behavior of Heavy Metals and Arsenic in the Weathered Tailings of Songcheon Mine (송천광산의 풍화광미 내 중금속 및 비소 거동 특성)

  • Lee, Woo-Chun;Kim, Young-Ho;Cho, Hyen-Goo;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.2
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    • pp.125-139
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    • 2010
  • Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

Characteristics of CaCO3 Sorbent Particles for the In-furnace Desulfurization (로 내 탈황을 위한 CaCO3 흡착제 입자의 분위기 기체와 체류 시간의 변화에 따른 특성)

  • Lee, Kang-Soo;Jung, Jae-Hee;Keel, Sang-In;Lee, Hyung-Keun;Kim, Sang-Soo
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.34 no.2
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    • pp.121-127
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    • 2010
  • The in-furnace desulfurization technique is applied to the $O_2/CO_2$ combustion system for the carbon capture and storage (CCS) process because this combustion system does not need an additional chamber for the desulfurization. $CaCO_3$ sorbent particles, which have a wide range in size from a few nanometers to several tens of micrometers, are used for this process. In this study, an experimental system which can simulate the $O_2/CO_2$ combustion system was developed. $CaCO_3$ sorbent particles were exposed to the high temperature reactor at $1200^{\circ}C$ with various residence times (0.33-1.46 s) in air and $CO_2$ atmospheric conditions, respectively. The sorbent particles were then sampled at the inlet and outlet of the reactor and analyzed qualitatively/quantitatively using SMPS, XRD, TGA, and SEM. The results showed that the residence time and atmospheric condition in a high temperature reactor can affect the characteristics of the $CaCO_3$ sorbent particles used in the in-furnace desulfurization technique, such as the calcination rate and reaction mechanism.

Mineralogical, Micro-textural, and Geochemical Characteristics for the Carbonate Rocks of the Lower Makgol Formation in Seokgaejae Section (석개재 지역 하부 막골층 탄산염암의 광물조성, 미세구조 및 지화학적 특성)

  • Park, Chaewon;Kim, Ha;Song, Yungoo
    • Economic and Environmental Geology
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    • v.51 no.4
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    • pp.323-343
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    • 2018
  • This study defines the mineralogical, micro-textural and geochemical characteristics for the carbonate rocks and discusses the fluids that have affected the depositional environment of the Lower Makgol Formation in Seokgaejae section. Based on analysis of X-ray Diffraction (XRD), Scanning Electron Microscope-Energy Dispersive X-ray Spectrometry (SEM-EDS), Electron Probe Micro Analyzer-Wavelength Dispersive X-ray Spectrometry (EPMA-WDS) and Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS), carbonate miorofacies in the basal and the lower members of the Makgol Formation are distinguished and classified into four types. Type 1 dolomite (xenotopic interlocking texture) and Type 2 dolomite (idiotopic interlocking texture) have relatively high Mg/Ca ratio, flat REE pattern, low Fe and Mn. Extensively interlocking textures in these dolomites indicate constant supply of Mg ion from hypersaline brine. Type 3 and Type 4 dolomite (scattered and loosely-aggregated texture) have relatively moderate Mg/Ca ratio, MREE enriched pattern, low to high Fe and Mn. These partial dolomitization indicate limited supply of Mg ion under the influx of meteoric water with seawater. Also, the evidence of Fe-bearing minerals, recrystallization and relatively high Fe and Mn in Type 4 indicates the influence of secondary diagenetic fluids under suboxic conditions. Integrating geochemical data with mineralogical and micro-textural evidence, the discrepancy between the basal and the lower members of the Makgol Formation indicates different sedimentary environment. It suggest that hypersaline brine have an influence on the basal member, while mixing meteoric water with seawater have an effect on the lower member of the Makgol Formation.

About Short-stacking Effect of Illite-smectite Mixed Layers (일라이트-스멕타이트 혼합층광물의 단범위적층효과에 대한 고찰)

  • Kang, Il-Mo
    • Economic and Environmental Geology
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    • v.45 no.2
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    • pp.71-78
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    • 2012
  • Illite-smectite mixed layers (I-S) occurring authigenically in diagenetic and hydrothermal environments reacts toward more illite-rich phases as temperature and potassium ion concentration increase. For that reason, I-S is often used as geothermometry and/or geochronometry at the field of hydrocarbons or ore minerals exploration. Generally, I-S shows X-ray powder diffraction (XRD) patterns of ultra-thin lamellar structures, which consist of restricted numbers of sillicate layers (normally, 5 ~ 15 layers) stacked in parallel to a-b planes. This ultra-thinness is known to decrease I-S expandability (%S) rather than theoretically expected one (short-stacking effect). We attempt here to quantify the short stacking effect of I-S using the difference of two types of expandability: one type is a maximum expandability ($%S_{Max}$) of infinite stacks of fundamental particles (physically inseparable smallest units), and the other type is an expandability of finite particle stacks normally measured using X-ray powder diffraction (XRD) ($%S_{XRD}$). Eleven I-S samples from the Geumseongsan volcanic complex, Uiseong, Gyeongbuk, have been analyzed for measuring $%S_{XRD}$ and average coherent scattering thickness (CST) after size separation under 1 ${\mu}m$. Average fundamental particle thickness ($N_f$) and $%S_{Max}$ have been determined from $%S_{XRD}$ and CST using inter-parameter relationships of I-S layer structures. The discrepancy between $%S_{Max}$ and $%S_{XRD}$ (${\Delta}%S$) suggests that the maximum short-stacking effect happens approximately at 20 $%S_{XRD}$, of which point represents I-S layer structures consisting of ca. average 3-layered fundamental particles ($N_f{\approx}3$). As a result of inferring the $%S_{XRD}$ range of each Reichweite using the $%S_{XRD}$ vs. $N_f$ diagram of Kang et al. (2002), we can confirms that the fundamental particle thickness is a determinant factor for I-S Reichweite, and also that the short-stacking effect shifts the $%S_{XRD}$ range of each Reichweite toward smaller $%S_{XRD}$ values than those that can be theoretically prospected using junction probability.

Engineering Geological Implications of Fault Zone in Deep Drill Cores: Microtextural Characterization of Pseudotachylite and Seismic Activity (시추코어 단층대에서의 지질공학적 의미: 슈도타킬라이트의 미세조직의 특징과 지진활동)

  • Choo, Chang-Oh;Jeong, Gyo-Cheol
    • The Journal of Engineering Geology
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    • v.27 no.4
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    • pp.489-500
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    • 2017
  • It is not rare that pseudotachylite, dark colored rock with glassy texture, is recognizable in deep core samples drilled up to 900 m from the surface. Pseudotachylite with widths varying few to 20 cm is sharply contacted or interlayered with the host rocks composed of Jurassic granite and Precambrian amphibolite gneiss, showing moderately ductile deformation or slight folding. Pseudotachylite occurring at varying depths in the deep drill core are slightly different in texture and thickness. There is evidence of fault gouge at shallower depths, although brittle deformation is pervasive in most drill cores and pseudotachylite is identified at random depth intervals. Under scanning electron microscope (SEM), it is evident that the surface of pseudotachylite is characterized by a smooth, glassy matrix even at micrometer scale and there is little residual fragments in the glass matrix except microcrystals of quartz with embayed shape. Such textural evidence strongly supports the idea that the pseudotachylite was generated through the friction melting related to strong seismic events. Based on X-ray diffraction (XRD) quantitative analysis, it consists of primary minerals such as quartz, feldspars, biotite, amphibole and secondary minerals including clay minerals, calcite and glassy materials. Such mineralogical features of fractured materials including pseudotachylite indicate that the fractured zone might form at low temperatures possibly below $300^{\circ}C$, which implies that the seismic activity related to the formation of pseudotachylite took place at shallow depths, possibly at most 10 km. Identification and characterization of pseudotachylite provide insight into a better understanding of the paleoseismic activity of deep grounds and fundamental information on the stability of candidate disposal sites for high-level radioactive waste.

A Study on the Conservation State and Plans for Stone Cultural Properties in the Unjusa Temple, Korea (운주사 석조문화재의 보존상태와 보존방안에 대한 연구)

  • Sa-Duk, Kim;Chan-Hee, Lee;Seok-Won, Choi;Eun-Jeong, Shin
    • Korean Journal of Heritage: History & Science
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    • v.37
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    • pp.285-307
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    • 2004
  • Synthesize and examine petrological characteristic and geochemical characteristic by weathering formation of rock and progress of weathering laying stress on stone cultural properties of Unjusa temple of Chonnam Hwasun county site in this research. Examine closely weathering element that influence mechanical, chemical, mineralogical and physical weathering of rocks that accomplish stone cultural properties and these do quantification, wish to utilize by a basic knowledge for conservation scientific research of stone cultural properties by these result. Enforced component analysis of rock and mineralogical survey about 18 samples (pyroclastic tuff; 7, ash tuff; 4, granite ; 4, granitic gneiss; 3) all to search petrological characteristic and geochemical characteristic by weathering of Unjusa temple precinct stone cultural properties and recorded deterioration degree about each stone cultural properties observing naked eye. Major rock that constitution Unjusa temple one great geological features has strike of N30-40W and dip of 10-20NE being pyroclastic tuff. This pyroclastic tuff is ranging very extensively laying center on Unjusa temple and stone cultural properties of precinct is modeled by this pyroclastic tuff. Stone cultural propertieses of present Unjusa temple precinct are accomplishing structural imbalance with serious crack, and because weathering of rock with serious biological pollution is gone fairly, rubble break away and weathering and deterioration phenomenon such as fall off of a particle of mineral are appearing extremely. Also, a piece of iron and cement mortar of stone cultural properties everywhere are forming precipitate of reddish brown and light gray being oxidized. About these stone cultural properties, most stone cultural propertieses show SD(severe damage) to MD(moderate damage) as result that record Deterioration degree. X-ray diffraction analysis result samples of each rock are consisted of mineral of quartz, orthoclase,plagioclase, calcite, magnetite etc. Quartz and feldspar alterated extremely in a microscopic analysis, and biotite that show crystalline form of anhedral shows state that become chloritization that is secondary weathering mineral being weathered. Also, see that show iron precipitate of reddish brown to crack zone of tuff everywhere preview rock that weathering is gone deep. Tuffs that accomplish stone cultural properties of study area is illustrated to field of Subalkaline and Peraluminous, $SiO_2$(wt.%) extent of samples pyroclastic tuff 70.08-73.69, ash tuff extent of 70.26-78.42 show. In calculate Chemical Index of Alteration(CIA) and Weathering Potential Index(WPI) about major elements extent of CIA pyroclastic tuff 55.05-60.75, ash tuff 52.10-58.70, granite 49.49-51.06 granitic gneiss shows value of 53.25-67.14 and these have high value gneiss and tuffs. WPI previews that is see as thing which is illustrated being approximated in 0 lines and 0 lines low samples of tuffs and gneiss is receiving esaily weathering process as appear in CIA. As clay mineral of smectite, zeolite that is secondary weathering produce of rock as result that pick powdering of rock and clothing material of stone cultural properties observed by scanning electron micrographs (SEM). And roots of lichen and spore of hyphae that is weathering element are observed together. This rock deep organism being coating to add mechanical weathering process of stone cultural properties do, and is assumed that change the clay mineral is gone fairly in stone cultural properties with these. As the weathering of rocks is under a serious condition, the damage by the natural environment such as rain, wind, trees and the ground is accelerated. As a counter-measure, the first necessary thing is to build the ground environment about protecting water invasion by making the drainage and checking the surrounding environment. The second thing are building hardening and extirpation process that strengthens the rock, dealing biologically by reducing lichens, and sticking crevice part restoration using synthetic resin. Moreover, it is assumed to be desirable to build the protection facility that can block wind, sunlight, and rain which are the cause of the weathering, and that goes well with the surrounding environment.