• Title/Summary/Keyword: crystallite orientation

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X-ray Diffraction Studies of Poly(aryl ether ether ketone) Fibers with Different Degrees of Crystallinity and Orientation

  • Karacan Ismail
    • Fibers and Polymers
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    • v.6 no.3
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    • pp.206-218
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    • 2005
  • Structural studies of series of 'as spun' and drawn PEEK fibers have been carried out using X-ray diffraction and optical microscopy techniques. The analysis of results suggest that fibers produced at a constant draw ratio with increasing draw temperatures show enhanced orientation and crystalline behaviour. The resolved equatorial and meridional traces provide additional structural parameters in terms of crystallinity, crystallite size, and crystallite thickness. It is concluded that drawing at a temperature below $T_g(i.e.,\;144^{\circ}C)$ results in poorly oriented non-crystalline materials, whereas drawing above $T_g$ results in highly oriented semi crystalline materials. Additional drawing proved to increase the overall orientation with slight improvements in lateral order of the chain molecules. Quantitative analysis revealed that the crystallite size increases with increasing drawing temperature. The results also revealed the increased crystallite size upon additional drawing. Crystalline orientation parameter, $_c$, suggests almost perfect orientation. In all cases, the amorphous orientation is found to be lower than the overall orientation parameter obtained from the optical birefringence. As a result of additional drawing, crystalline orientation was found to increase slightly but the increase in the orientation of non-crystalline material was found to be substantial. An average crystalline density was determined from the orthorhombic unit cell dimensions. It was found to vary as a result of processing conditions. It was also found that the value of the maximum birefringence shows heavy dependence on the chain conformation.

Variation of Crystalline State in a Stem of Chamaecyparis obtusa E. (편백(Chamaecyparis obtusa E.) 수간내에서의 결정상태의 변이성)

  • Kim, Nam-Hun;Lee, Ki-Yeong
    • Journal of the Korean Wood Science and Technology
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    • v.26 no.4
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    • pp.20-25
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    • 1998
  • Radial variation of crystalline state in a stem of Chamaecyparis obtusa E. was examined by x-ray diffraction analyses. Relative crystallinity and degree of crystallite orientation showed significant differences between juvenile and adult wood. That is, Relative crystallinity increased with increasing the age from pith to about 20th annual ring, after which it reached a more or less constant value. On the other hand, degree of crystallite orientation decreased outward from pith to about 10 years and presented almost a constant value thereafter. Crystal width by Scherrer's equation did not show any significant differences between juvenile and adult wood. Therefore, it was considered that crystallinity index and degree of crystallite orientation by x-ray diffraction method could be used for evaluating wood quality.

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A Study on the Change of fine Structure of Hemp Cellulose (안동포원료 Hemp Cellulose의 미세구조에 관한 연구)

  • Lee UK Ja;Ryu Duck Whan
    • Journal of the Korean Society of Clothing and Textiles
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    • v.8 no.1
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    • pp.29-37
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    • 1984
  • This study was investigation of the change of fine structure of hemp cellulose at different growing stages. The samples collected about every eight day were divided into seven groups based on plants height, then they were numbered from 1 to 7 in the order of their height. For this, the degree of crystallinity, orientation and crystallite size were measured by wide angle X-ray diffraction method. The results of this experiment were summerized as follows ; 1) The degree of crystallinity was increased by growth of hemp celtilose to be maximum in sample 5$\~$6. At this stage, the stability of crystals was showed in good states. In addition to, crystallinity index by Segal, Turley and area method showed same tendency as Ruland's. 2) The change of orientation was gradually increased by growth of hemp cellulose. This result was correlated with the degree of crystallinity. Therefore, the change of orientation depend on the degree of crystallinity. 3) On the other hand, the crystallite size was decreased by growth of hemp cellulose. But, increased after sample 4. By the way, crystallite size was interrelated with growth rate.

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An in Depth Study of Crystallinity, Crystallite Size and Orientation Measurements of a Selection of Poly(Ethylene Terephthalate) Fibers

  • Karacan Ismail
    • Fibers and Polymers
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    • v.6 no.3
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    • pp.186-199
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    • 2005
  • A selection of commercially available poly(ethy1ene terephtha1ate) fibers with different degrees of molecular alignment and crystallinity have been investigated utilizing a wide range of techniques including optical microscopy, infrared spectroscopy together with thermal and wide-angle X-ray diffraction techniques. Annealing experiments showed increased molecular alignment and crystallinity as shown by the increased values of birefringence and melting enthalpies. Crystallinity values determined from thermal analysis, density, unpolarized infrared spectroscopy and X-ray diffraction are compared and discussed in terms of the inherent capabilities and limitations of each measurement technique. The birefringence and refractive index values obtained from optical microscopy are found to decrease with increasing wavelength of light used in the experiments. The wide-angle X-ray diffraction analysis shows that the samples with relatively low orientation possess oriented non-crystalline array of chains whereas those with high molecular orientation possess well defined and oriented crystalline array of chains along the fiber axis direction. X-ray analysis showed increasing crystallite size trend with increasing molecular orientation. SEM images showed micro-cracks on low oriented fiber surfaces becoming smooth on highly oriented fiber surfaces. Excellent bending characteristics were observed with knotted fibers implying relatively easy fabric formation.

The Change of Crystal Structure and Physical Properties of Partially Oriented Polyester Yarn(POY) on the Draw Ratio and Heat Setting Temperature (연신비와 열고정 온도에 따른 Partially Oriented Polyester Yarn(POY)의 구조변화와 물성)

  • 박명수;윤종호
    • Textile Coloration and Finishing
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    • v.12 no.2
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    • pp.103-110
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    • 2000
  • To examine the physical properties of POY through the microstructure control, the crystal structure such as the crystallinity, the crystallite size, the orientation, the shrinkage, the tensile properties, and the thermal stress of POY(80/48, SD) were examined at different draw ratios and annealing temperatures. From the examination following conclusions were obtained : 1. The crystallinity was more effected by the heat setting temperature than by the draw ratio. The increasing rate was greatest at the heat setting temperature range of $170~190^\circ{C}$. 2. The crystallite size perpendicular to the fiber axis was more effected by the annealing temperature at lower draw ratios. On the other hand, the crystal and amorphous orientations were more effected by the heat setting at higher draw ratios. 3. The boiling shrinkage did not change significantly, but the total shrinkage showed 13% at the draw ratio 1.9 and the heat setting temperature $170^\circ{C}$. 4. The maximum thermal stress increased with increasing the draw ratio and decreasing the heat setting temperature in the temperature range of $170~210^\circ{C}$. At the draw ratio 1.9 and the heat setting temperature $170^\circ{C}$, the maximum thermal stress found was 1.1gf/d. 5. In the heat setting temperature above $170^\circ{C}$ after the drawing, the crystallinity, the crystallite size, the orientation, and the strength increased with increasing temperature, but the shrinkage and the maximum thermal stress decreased with increasing temperature.

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Study on Characteristics of Electrodeposited Thin Copper Film by Inorganic Additives in Pyrophosphate Copper Plating Bath (피로인산동욕의 무기첨가제에 의한 전해동박의 특성에 관한 연구)

  • Koo, Seokbon;Hur, Jinyoung;Lee, Hongkee
    • Journal of the Korean institute of surface engineering
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    • v.47 no.1
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    • pp.1-6
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    • 2014
  • The copper deposit on steel plate was prepared by pyrophosphate copper plating solution made with variation of inorganic additive. $NH_4OH$ and $NH_4NO_3$ were used as inorganic additives. The copper layer characteristics - tensile strength, crystallite size and crystal orientation - were evaluated by X-ray diffraction and Universal Test Machine. The presence of ammonium nitrate results in reduction of average roughness value from $0.08{\mu}m$ to $0.03{\mu}m$. In pyrophosphate copper plating solution without Inorganic additive, tensile strength of electrodeposit copper foil was reduced from 600 MPa to 180 MPa after 7 days aging. However, when adding ammonium nitrate, there was almost no change of tensile strength, intensity of crystal orientation - (111), (200) and (220) - and crystallite size (2~30 nm).

A Study On the Structure and Mechanical Properties of Polypropylene filament treated with Dry heat treatment at Different draw ratio (연신비를 달리한 Polypropylene filament의 건열처리에 따른 구조와 물성에 관한 연구)

  • Lee, Eun-Woo;Cho, In-Sul
    • Journal of the Korean Society of Industry Convergence
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    • v.2 no.2
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    • pp.61-68
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    • 1999
  • The variety of crystalline structure and mechanical properties of PP filament treated with dry heat treatment at different draw ratio has been studied. Crystalline structure and mechanical properties of annealed PP filament at different draw ratio has been examined by XRD, UTM, and density method. Heat treatment has been carried out $100^{\circ}C$, $120^{\circ}C$ $140^{\circ}C$ for 30min. in dry oven. From the results of this study, it found the following facts. It was found that the crystallinity and crystallite size of (110) plane of sample were increased with increasing of annealed temperature and draw ratio. The crystalline form of annealed sample which was undrawn showed ${\alpha}$, ${\beta}$ mixing form below $120^{\circ}C$ and showed ${\alpha}$ form at $140^{\circ}C$. But the crystalline form of annealed sample which was drawn showed ${\alpha}$ form at $120^{\circ}C$. Initial modulus and tensile strength were increased with increasing of annealing temperature, and the degree of orientation was decreased with decreasing of annealing temperature.

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Effects of Preferred Orientation and Microstructure on Mechanical Properties of Chemically Vapor Deposited SiC (화학증착 탄화규소막의 방향성과 미세구조가 증착층의 기계적 성질에 미치는 영향)

  • 김동주;김영욱;박상환;최두진;이준근
    • Journal of the Korean Ceramic Society
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    • v.32 no.10
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    • pp.1103-1110
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    • 1995
  • Silicon carbide (SiC) films have been deposited on the isotropic graphite by chemical vapor deposition. Change of deposition parameters affected significantly the microstructure and preferred orientation of SiC films. Preferred orientation of SiC films was (111) or (220), and microstructure showed the startified structure consisting of small crystallite or faceted columnar structure depending on the deposition parameters. For microhardness, (111) oriented film and stratified structure were superior to (220) oriented film and faceted columnar structure, respectively. Surface of (111) oriented films was less rough than that of (220) oriented films. Adhesion force between graphite substrate and SiC films was above 100N for crystalline films and 49N for amorphous film.

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Effect of Additives on the Hardness of Copper Electrodeposits in Acidic Sulfate Electrolyte (황산구리 전착에서의 첨가제가 구리전착층의 경도에 미치는 영향)

  • Min, Sung-Ki;Lee, Jeong-Ja;Hwang, Woon-Suk
    • Corrosion Science and Technology
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    • v.10 no.4
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    • pp.143-150
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    • 2011
  • Copper electroplating has been applied to various fields such as decorative plating and through-hole plating. Technical realization of high strength copper preplating for wear-resistant tools and molds in addition to these applications is the aim of this work. Brighters and levelers, such as MPSA, Gelatin, Thiourea, PEG and JGB, were added in copper sulfate electrolyte, and the effects of these organic additives on the hardness were evaluated. All additives in this work were effective in increasing the hardness of copper electrodeposits. Thiourea increased the hardness up to 350 VHN, and was the most effective accelarator in sulfate electrolyte. It was shown from the X-ray diffraction analysis that preferred orientation changed from (200) to (111) with increasing concentration of organic additives. Crystallite size decreased with increasing concentration of additive. Hardness was increased with decreasing crystallite size, and this result is consistent with Hall-Petch relationship, and it was apparent that the hardening of copper electrodeposits results from the grain refining effect.

Microstructure of Zinc electrodeposit in Cyanide Solution (시안화아연욕을 사랑한 아연 전착층의 조직특성)

  • Ye G.C;Cho E.H.
    • Journal of the Korean institute of surface engineering
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    • v.17 no.2
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    • pp.41-58
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    • 1984
  • Zinc was electrodeposited from cyanide solutions at temperature from 20$^{\circ}C\;to\;40^{\circ}C$ in the range of current density from 0.5 to 8A/$dm^2$. The preferred orientation changed from (10.3)+(11.0) to (11.0) texture with increasing cathode overpotential in the additive free solution, while the (11.0) preferred orientation developed at lower overpotentials (800-1270 mV) and the (11.0)+(10.0) preferred orientation was formed at higher overpotential (1300-1400mV) in the solution with brightner. Mossy type of morphology developed mostly in the additive free deposits and the microstructure of the cross section of the above deposits changed from columar structure to granular structure with increasing overpotential. The surface appearance of the deposits with additive having (11.0) texture was the smooth deposit of very small crystallite, while that of the deposits having (11.0)+(10.0) texture was fine crystalline deposit. The microstructure of the cross section of them was the fine field oriented type of structure.

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