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At least 199 records · Page 11

Lateral cracks during sliding indentation on various optical materials

A series of static and sliding indentation (ie, scratching) was performed and characterized on a wide range of optical workpiece materials [single crystals of Al 2 O 3 (sapphire), SiC, Y 3 Al 5 O 12 (YAG), CaF 2 , and LiB 3 O 5 (LBO); a SiO 2 –Al 2 O 3 –P 2 O 5 –Li 2 O glass ceramic (Zerodur); and glasses of SiO 2 :TiO 2 (ULE), SiO 2 (fused silica), and P 2 O 5 –Al 2 O 3 –K 2 O–BaO (Phosphate)] at various applied loads using various indenters (Vickers, 10 µm conical, and 200 µm conical). Despite having different load dependencies, the lateral crack depth formed during sliding indentation quantitatively scales with that formed during static indentation, explaining why static indentation has been historically effective in describing various grinding parameters. Depending on the indenter geometry, the amount of residual trench damage (plastic deformation and local fracturing) during sliding indentation was often enhanced by more than an order of magnitude compared with static indentation. A simple ploughing scratch model, which considers both tangential and normal stresses (where the tangential stress is amplified by relatively small tangential contact area), explains this enhancement and other observed trends. Accounting for the high correlation between residual trench depth and volumetric fracturing, the model is extended to estimate the amount of fracture damage as a function of the material properties of the workpiece, indenter geometry, and applied load. Such a model has utility in the design of optimized grinding processes, particularly the abrasive geometry. Finally, at higher loads (>1 N), lateral cracks were often observed to preferentially propagate in the forward scratching direction, as opposed to perpendicular to the scratch as typically observed. High-speed imaging of the scratch process confirms that these cracks propagate ahead of the sliding indenter during the scratching event. Finite element stress analysis suggests the ploughing frictional forces increase the mode I tensile stresses at the leading edge of the sliding indenter explaining the direction of crack propagation of such cracks.

36 MATERIALS SCIENCE↗

Removal characteristics of plasma chemical vaporization machining with a pipe electrode for optical fabrication

Plasma chemical vaporization machining (CVM) is a high-precision chemical shaping method using rf plasma generated in the proximity of an electrode in an atmospheric environment. The purpose of the present study is to clarify the removal characteristics of plasma CVM using a pipe electrode. Polished fused silica plates were processed by plasma CVM, polishing, and precision grinding under various conditions. The removal rate of plasma CVM was about 4 to 1100 times faster than that of polishing, and the maximum removal rate was almost equal to that of precision grinding. The roughness of the resultant surfaces was almost the same as that of the polished surfaces.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Air Classification of Forest Residue for Tissue and Ash Separation Efficiency

The goal of this Case Study was to evaluate the performance of air classification of logging residues toward meeting conversion CMAs for carbon and ash contents, as compared to the static status quo Base Case system in which the residues are first dried and then ground in a hammer mill with a 6 mm screen and fines less than 1.18 mm are removed. Also considered were moisture and ash impacts on throughput and Overall Operating Effectiveness (OOE), as well as delivered feedstock cost and minimum fuel selling price (MFSP). Laboratory data on the impacts of fan speed and moisture content on the separation efficiency of soil ash, needles and bark from white wood were received from FCIC Subtask 5.2: Preprocessing, High Temperature Conversion Preprocessing (Jordan Klinger and Tiasha Bhattacharjee, INL). Average throughput and energy consumption data were obtained from the Bioenergy Feedstock National User Facility (BFNUF) (Neal Yancey, INL) for the same air classifier. These data were utilized to develop the necessary response surface equations to perform throughput analysis using discrete event simulation. Feedstock-Conversion Interface Consortium. Because the Base Case status quo system utilizes drying prior to grinding, we modeled the Case Study with drying prior to air classification and subsequent grinding of the separated white wood to isolate the individual quality and cost impacts of air classification relative to the Base Case system.

CMA↗

Effects of Aging and Decontamination Pressure on the Penetration of Radionuclides into Concrete - 18418

Radionuclide penetration into concrete was investigated as function of time and pressure of an applied water spray. Depth profiles of three radionuclides into a concrete surface over the time periods of 20-24 hours, 9 days, and 90 days were found by grinding the surface. The profiles were starkly different between the radionuclides, as Eu-152 deposited close to the surface and did not penetrate further over time while the depth of Cs-137 increased with time. Such differences suggest that response time during a remediation effort is more important for Cs-137 decontamination compared to Eu-152. The depth profiles were also used to assess the water pressure that was needed to remove contamination. Static tests, where the surface was soaked in 0.5 M KCl, accessed up to 80 μm into the surface, while ablation through high pressure washing removed approximately 10-20 μm of the surface. Similar grind profiles were then collected on decontaminated coupons, displaying that high pressure washing drove Sr-85 into the surface, decreasing the removal of the nuclide. As such, radionuclide specific decontamination may be required because of the varied response times and pressures effects for each radionuclide. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

The Preparation of Luminescent, Mechanochromic Molecular Containers from Non‐Emissive Components: The Box Cations, [Au 6 (Triphos) 4 Br] 5+ and [Au 6 (Triphos) 4 Br 2 ] 4+

Abstract Two new molecular boxes, the mono‐bromo box [Au 6 (Triphos) 4 Br](SbF 6 ) 5 ⋅6(CH 2 Cl 2 ), 4 mB , and the dibromo box, [Au 6 (Triphos) 4 Br 2 ⋅H 2 O](SbF 6 ) 4 ⋅4(CH 2 Cl 2 ), 5 dB , have been prepared in crystalline form. Although constructed from non‐luminescent components, both are strongly luminescent. Like its chloro counterpart, the mono‐bromo box [Au 6 (Triphos) 4 Br](SbF 6 ) 5 ⋅6(CH 2 Cl 2 ), 4 mB , is mechanochromic. Under grinding, it loses its luminescence. The bromo‐bridged helicate, [(μ‐Br){Au 3 (Triphos) 2 } 2 ](CF 3 SO 3 ) 5 ⋅2(CH 2 Cl 2 ), 3μ‐H , with a cation that is isomeric with the box [Au 6 (Triphos) 4 Br] 5+ , has also been prepared and crystallographically characterized. Unlike its chloro analogue, [(μ‐Br){Au 3 (Triphos) 2 } 2 ](CF 3 SO 3 ) 5 ⋅2(CH 2 Cl 2 ) is not luminescent. Thus, the cation produced upon grinding may be the cation present in the bromo‐bridged helicate, [(μ‐Br){Au 3 (Triphos) 2 } 2 ](CF 3 SO 3 ) 5 ⋅2(CH 2 Cl 2 ), 3μ‐H . The dibromo box, [Au 6 (Triphos) 4 Br 2 ⋅H 2 O](SbF 6 ) 4 ⋅4(CH 2 Cl 2 ), 5 dB , is not significantly mechanochromic.

Walters, Daniel T.↗

Surface engineering to enhance heat generation and joint strength in dissimilar materials AZ31 and DP590 ultrasonic welding

A multiscale simulation approach was developed and employed to optimize the sheet surface conditions for higher interfacial temperature and joint strength in ultrasonic welding of magnesium alloy AZ31 and dual-phase steel DP590. First, a mesoscale model was used to study the relationship between friction coefficient and surface roughness, which can be modified by various engineering methods. Then a macroscopic process model was employed to study the effects of surface roughness on heat generation, indicating that a temperature increase can be achieved with rougher surfaces on two sides of both DP590 and AZ31 sheets. Samples prepared by sanding and filing, as well as grinding, were first characterized for surface roughness and then welded under ultrasonic vibration. An infrared camera was used to measure temperatures in situ for model validation. Overall, lap shear test results for the welded joint showed that the joint strength can be improved by 10~25% using filing and round grinding methods as a result of the enhanced heat generation and mechanical interlocking on the interface.

42 ENGINEERING↗

Study on Nanocellulose Properties Processed Using Different Methods and Their Aerogels

In this paper the effects of different mechanical methods including homogenization, ultrasonication and grinding on the properties of the nanocellulose materials and their aerogels, were investigated. The cellulose nanocrystal products, (CNC-H) and (CNC-U), were prepared by homogenization and ultrasonication of the acid hydrolyzed pulps, respectively. The aerogel products were produced by solvent exchanging of nanocellulose hydrogels with tertiary butyl alcohol and followed by freeze drying. The nanocellulose materials were studied using transmission electron microscopy, field emission scanning electron microscopy (FE-SEM), Fourier transformed infrared spectroscopy (TEM), X-ray diffraction (XRD), thermal gravimetric analysis (TGA). Size distribution and surface charges of the nanocellulose suspensions were measured by zetasizer. Also, the morphology, the porosity properties and surface area of the CNCs and CNF aerogels were investigated via FE-SEM and nitrogen adsorption–desorption isotherms. The results showed that CNC-H has higher surface charge, suspension stability (− 41.8 mV), crystallinity index (74.7%) and better size dispersion than CNC-U and CNF with an average particle size of 122 nm. CNC-H microstructures demonstrated homogeneous network structure with smaller nanometer dimensions (15–30 nm width and 60–400 nm length). However, the CNC-H showed lower thermal stability compared to CNC-U and CNF. Larger average pore size (16.32 nm), pore volume (0.42 cc/g) and high specific surface area (> 100 m{sup 2} g{sup −1}) in CNC-H aerogel were obtained. Graphical Abstract: Suspensions of nanocellulose (NC) were prepared by different mechanical methods: Homogenizing, Ultrasonic and grinding. The NC products were investigated and their differences in morphology and other characteristics were studied. The aerogels were prepared from the nanocellulose hydrogels. The nitrogen physisorption was used to study the pore characteristics of the aerogels. .

36 MATERIALS SCIENCE↗

Influence of Oxidation Treatments and Surface Finishing on the Electrochemical Behavior of Ni-20Cr HVOF Coatings

The low-temperature electrochemical behavior of HVOF Ni-20Cr coatings was assessed. The coatings were evaluated in different conditions including as-sprayed, as-ground, and heat-treated in air and argon atmospheres. A detailed analysis of the coatings was carried out by means of XRD, SEM, and EPMA, prior and after the corrosion test. The corrosion rate was analyzed in a NaCl solution saturated with CO{sub 2}. Results demonstrate that the use of a low-oxygen partial pressure favors the formation of a Cr{sub 2}O{sub 3} layer on the surface of the coatings. According to the electrochemical results, the lower corrosion rates were obtained for the heat-treated coatings irrespective of the surface finishing, being the ground and argon heat-treated condition that shows the best corrosion performance. This behavior is due to the synergistic effect of the low-pressure heat treatment and the grinding processes. The grinding promotes a more homogeneous reaction area without surface heterogeneities such as voids, and the pre-oxidation treatment decreases the porosity content of the coating and also allows the growing of a Cr-rich oxide scale which acts as a barrier against the ions of the aqueous solution.

36 MATERIALS SCIENCE↗

Effect of pelleting process variables on physical properties and sugar yields of ammonia fiber expansion pretreated corn stover

Pelletization process variables including grind size (4, 6 mm), die speed (40, 50, 60 Hz), and preheating (none, 70 degrees C) were evaluated to understand their effect on pellet quality attributes and sugar yields of ammonia fiber expansion (AFEX) pretreated biomass. The bulk density of the pelletized AFEX corn stover was three to six times greater compared to untreated and AFEX-treated corn stover. Also the durability of the pelletized AFEX corn stover was >97.5% for all pelletization conditions studied except for preheated pellets. Die speed had no effect on enzymatic hydrolysis sugar yields of pellets. Pellets produced with preheating or a larger grind size (6 mm) had similar or lower sugar yields. Pellets generated with 4 mm AFEX-treated corn stover, a 60 Hz die speed, and no preheating resulted in pellets with similar or greater density, durability, and sugar yields compared to other pelletization conditions.

09 BIOMASS FUELS↗

Mechanically-induced disorder in CaFe 2 As 2 : A 57 Fe Mössbauer study

57 Fe Mössbauer spectroscopy was used to perform a microscopic study on the extremely pressure and strain sensitive compound, CaFe 2 As 2 , with different degrees of strain introduced by grinding and annealing. At the base temperature, in the antiferromagnetic/orthorhombic phase, compared to a sharp sextet Mössbauer spectrum of single crystal CaFe 2 As 2 , which is taken as an un-strained sample, an obviously broadened sextet and an extra doublet were observed for ground CaFe 2 As 2 powders with different degrees of strain. The Mössbauer results suggest that the magnetic phase transition of CaFe 2 As 2 can be inhomogeneously suppressed by the grinding induced strain to such an extent that the antiferromagnetic order in parts of the grains forming the powdered sample remain absent all the way down to 4.6 K. However, strain has almost no effect on the temperature dependent hyperfine magnetic field in the grains with magnetic order. Additional electronic and asymmetry information was obtained from the isomer shift and quadrupole splitting. Similar isomer shift values in the magnetic phase for samples with different degrees of strain, indicate that the stain does not bring any significant variation of the electronic density at 57 Fe nucleus position. As a result, the absolute values of quadrupole shift in the magnetic phase decrease and approach zero with increasing degrees of strain, indicating that the strain reduces the average lattice asymmetry at Fe atom position.

36 MATERIALS SCIENCE↗

Processing of surrogate nuclear fuel pellets for better dimensional control with dry bag isostatic pressing

A study of improved methods of processing fuel pellets was undertaken using ceria and zirconia/yttria/alumina as surrogates. Through proper granulation and vertical vibration (tapping) of the parts bag prior to dry bag isostatic pressing (DBIP), reproducibility of diameter profiles among multiple pellets of ceria was improved by almost an order of magnitude. Reproducibility of sintered pellets was sufficiently good to possibly avoid grinding. Deviation from the mean diameter along the length of multiple pellets, as well as, deviation from roundness, decreased after sintering. This is not generally observed with dry pressed pellets. Thus it is possible to machine to tolerance before sintering if grinding is necessary.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

M(II)-dipyridylamide-based coordination frameworks (M=Mn, Co, Ni): Structural transformation

A series of 1-D double-zigzag (([M(papx){sub 2}(H{sub 2}O){sub 2}](ClO{sub 4}){sub 2}){sub n}; M=Mn, x=s (1), x=o (3); M=Co, x=s (4), x=o (5); M=Ni, x=s (6), x=o (7)) and 2-D polyrotaxane ([Mn(paps){sub 2}(ClO{sub 4}){sub 2}]{sub n} (2)) frameworks were synthesized by reactions of M(ClO{sub 4}){sub 2} (M=Mn, Co, and Ni) with papx (paps, N,N’-bis(pyridylcarbonyl)-4,4’-diaminodiphenylthioether; papo, N,N’-bis(pyridylcarbonyl)-4,4’-diaminodiphenyl ether), which have been isolated and structurally characterized by X-ray diffraction. Based on powder X-ray diffraction (PXRD) experiments, heating the double-zigzag frameworks underwent structural transformation to give the respective polyrotaxane ones. Moreover, grinding the solid samples of the respective polyrotaxanes in the presence of moisture also resulted in the total conversion to the original double-zigzag frameworks. In this study, we have successfully extended studies to Mn{sup II}, Co{sup II}, and Ni{sup II} frameworks from the previous Zn{sup II}, Cd{sup II}, and Cu{sup II} ones, and interestingly such structural transformation is able to be proven experimentally by powder and single-crystal X-ray diffraction studies as well. - Graphical abstract: 1-D double-zigzag and 2-D polyrotaxane frameworks of M(II)-papx (x=s, o; M=Mn, Co, Ni) frameworks can be interconverted by heating and grinding in the presence of moiture, and such structural transformation has be proven experimentally by powder and single-crystal X-ray diffraction studies.

36 MATERIALS SCIENCE↗

Modified Pechini synthesis of tricalcium aluminate powder

Tricalcium aluminate (Ca{sub 3}Al{sub 2}O{sub 6}-C{sub 3}A) was obtained by a modified Pechini synthesis in order to eliminate successive thermal treatments and intermediate grinding usually performed between the two sintering steps and in order to reduce the sintering temperature. Our results indicated that pure C{sub 3}A was obtained, by a single step thermal treatment at 1300 Degree-Sign C for 4 h and 1350 Degree-Sign C for 1 h. The synthesis was confirmed by XRD, FT-IR and free lime analyses. The morphology of synthesised C{sub 3}A was assessed by electron microscopy (SEM and TEM, HRTEM) and it was observed a high tendency of the particles to form aggregates and the individual particles seem to be single crystals. The bioactivity was assessed by specimen soaking in simulated body fluid (SBF) for 7 days; the hydrate (i.e. 3CaO Bullet-Operator Al{sub 2}O{sub 3} Bullet-Operator 6H{sub 2}O formed at the C{sub 3}A surface), can act as nucleation centers for the resulted phosphate phases. - Highlights: Black-Right-Pointing-Pointer A modified Pechini synthesis was used for obtained of tricalcium aluminate. Black-Right-Pointing-Pointer C{sub 3}A was obtained at 1300 Degree-Sign C/4 h and 1350 Degree-Sign C/1 h. Black-Right-Pointing-Pointer Were eliminated successive thermal treatments and intermediate grinding. Black-Right-Pointing-Pointer The morphology of synthesised C{sub 3}A was assessed by electron microscopy (SEM, TEM). Black-Right-Pointing-Pointer Was observed a high tendency of the particles to form aggregates.

36 MATERIALS SCIENCE↗

On the measurement of austenite in supermartensitic stainless steel by X-ray diffraction

Sections of a 13Cr supermartensitic stainless steel were investigated to determine the optimum sample preparation for measurement of the austenite content by X-ray diffraction. The surface of several samples was mechanically ground or polished using media of grit sizes in the range 1–120 μm. The strained surface layer was afterwards removed stepwise by electropolishing, and the austenite content measured at each step. It was found that any level of mechanical grinding or polishing results in a reduction of the measured austenite fraction relative to the true bulk value, and that coarser grinding media impart greater damage and greater reduction in the measured austenite content. The results thus highlight the importance of the electropolishing step in preparation of such samples, but suggest that the American Society for Testing and Materials standard E975-03 substantially overestimates the amount of material which needs to be removed to recover the true “bulk” content. - Highlights: • Quantitative Rietveld analysis of austenite/martensite ratio in supermartensitic stainless steels • Critical evaluation of sample preparation for residual austenite measurements by X-ray diffraction • Highlighting of the importance of electropolishing as a final preparation step.

36 MATERIALS SCIENCE↗

Study of morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled compound

The morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled intermetallic compounds are presented. The polycrystalline HoNi{sub 3} bulk compound crystallizes in the rhombohedral PuNi{sub 3} — type of crystal structure and indicates ferrimagnetic arrangement with the Curie temperature of T{sub C} = 57 ± 2 K, the helimagnetic temperature T{sub h} = 23 ± 2 K with the total saturation magnetic moment of 6.84 μ{sub B}/f.u. at 2 K. The use of the ball-milling method leads to the formation of HoNi{sub 3} nanoflakes with typical thickness of less than 100 nm prone to agglomeration upon milling. The increase of grinding duration leads to the reduction in crystallite size, which was confirmed by various complementary microscopical and diffraction studies. Moreover, the increase in milling duration results in the emergence of the relatively small coercivity (H{sub C}), remanence (M{sub r}) and a variation of the saturation magnetization (M{sub S}). - Graphical abstract: Display Omitted - Highlights: • The ball-milling method exhibits significant potential for producing RT{sub 3} nanopowders. • The AFM method was used for the first time in analysis of R–T nanoflakes morphology. • HoNi{sub 3} compound forms polycrystalline and textured nanoflakes evolving upon milling. • The decrease in crystallite size via grinding is confirmed by XRD, TEM and AFM. • The magnetic parameters were sensitive to the extension of pulverization b.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A simple route for making surfactant free lead sulfide (PbS) quantum dots

Highlights: • Surfactant free PbS NCs were successfully synthesised using CoSP technique. • The technique eliminates the requirements of washing to remove the ligands. • Grinding using mortar and pestle creates well separated PbS QDs. • Surfactant free PbS NCs are stable and do not show any degradation with time. - Abstract: An efficient, cost effective and less time consuming method suitable for mass production of surfactant free quantum dots (QDs) of lead sulfide (PbS) is reported. PbS nanocrystals (NCs) are first synthesised by continuous spray pyrolysis (CoSP) technique and de-agglomeration into PbS quantum dots (QDs) is achieved by vigorous mechanical grinding using mortar and pestle. Lead acetate and thiourea were used as the precursor materials for preparation of surfactant free PbS NCs. The broadening in XRD peaks of ground NCs as compared to as synthesized PbS NCs clearly indicated the reduction in particle size to be QDs of PbS. The TEM images also showed that ground PbS NCs were nearly spherical in shape having an average diameter in the range of 4–6 nm. The shift in optical gap from 0.41 eV to 1.47 eV supported the QD formation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗