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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Combinatorial measurement of critical cooling rates in aluminum-base metallic glass forming alloys

Direct measurement of critical cooling rates has been challenging and only determined for a minute fraction of the reported metallic glass forming alloys. Here, we report a method that directly measures critical cooling rate of thin film metallic glass forming alloys in a combinatorial fashion. Based on a universal heating architecture using indirect laser heating and a microstructure analysis this method offers itself as a rapid screening technique to quantify glass forming ability. We use this method to identify glass forming alloys and study the composition effect on the critical cooling rate in the Al–Ni–Ge system where we identified Al 51 Ge 35 Ni 14 as the best glass forming composition with a critical cooling rate of 10 4 K/s.

36 MATERIALS SCIENCE↗
NASA NTRS1989

'Nose method' of calculating critical cooling rates for glass formation

The use of the so-called 'nose method' for computing critical cooling rates for glass formation is examined and compared with other methods, presenting data for the glass-forming systems SiO2, GeO2, and P2O5. It is shown that, for homogeneous crystallization, the nose-method will give an overestimate of Rc, a conclusion which was drawn after assessing the enfluence of a range of values for the parameters which control crystal growth and nucleation. The paper also proposes an alternative simple procedure (termed the 'cutoff method') for computing critical cooling rates from T-T-T diagrams, which was shown in the SiO2 and GeO2 systems to be superior to the nose method.

Weinberg, Michael C.↗
NASA NTRS1986

Dependence of the critical cooling rate for lithium-silicate glass on nucleating agents

The critical cooling rate, Rc, for glass formation of a glass containing 40 mol pct Li2O and 60 mol pct SiO2, doped with small amounts of Pt, Au, P2O5, and TiO2 nucleating agents, has been measured. Rc increases with increasing Pt and Au additions, but Pt has a larger effect than Au. Additions of P2O5 tend to decrease Rc, whereas TiO2 has practically no effect on Rc. The devitrified glass nucleated with Pt contains only crystalline Li2O-SiO2, but all the other devitrified glasses, including the undoped glass, contain both Li2O-SiO2 and Li2O-2SiO2. Analysis shows that Rc increases as the concentration of the Li2O-SiO2 phase in the devitrified glass increases.

Huang, W.↗
DOE OSTI2021

Critical cooling rates for amorphous-to-ordered complexion transitions in Cu-rich nanocrystalline alloys

Amorphous complexions in nanocrystalline metals have the potential to improve mechanical properties and radiation tolerance, as well as resistance to grain growth. In this study, the stability of amorphous complexions in binary and ternary Cu-based alloys is investigated by observing the effect of cooling rate from high temperature on the occurrence of amorphous-to-ordered complexion transitions. Bulk Cu-Zr and Cu-Zr-Hf alloy samples were annealed to induce boundary premelting and then quenched through a procedure that induces a gradient of local cooling rate through the sample height. Amorphous complexion thickness distributions were found to be invariant to local cooling rate in the Cu-Zr-Hf alloy, demonstrating enhanced stability of the amorphous complexion structure compared to the Cu-Zr alloy, which had thinner amorphous complexions in the regions that were slowly cooled. The experimental results are used to construct time-temperature-transformation diagrams for the amorphous-to-ordered complexion transition in both the binary and ternary alloys, enabling a deeper understanding of the influence of cooling rate and grain boundary chemistry on complexion transitions. In conclusion, the critical cooling rate necessary to avoid complexion transitions in the ternary alloy is found to be at least three orders of magnitude slower than that for the binary alloy.

36 MATERIALS SCIENCE↗
NASA NTRS2004

A New DTA Method for Measuring Critical Cooling Rate for Glass Formation

A new differential thermal analysis (DTA) experimental method has been developed to determine the critical cooling rate for glass formation, R(sub c). The method, which is found especially suitable for melts that, upon cooling, have a small heat of crystallization or a very slow crystallization rate, has been verified using a 38Na2O-62SiO2 (mol%) melt with a known R(sub c) (-approx. 19 C/min), then used to determine R(sub c) for two complex lithium silicate glass forming melts. The new method is rapid, easy to conduct and yields values for R(sub c) that are in excellent agreement with the R(sub c)-values measured by standard DTA techniques.

Ray, Chandra S.↗
DOE OSTI2022

Machine Learning Prediction of the Critical Cooling Rate for Metallic Glasses from Expanded Datasets and Elemental Features

In this study, we use a random forest (RF) model to predict the critical cooling rate (R C ) for glass formation of various alloys from features of their constituent elements. The RF model was trained on a database that integrates multiple sources of direct and indirect R C data for metallic glasses to expand the directly measured R C database of less than 100 values to a training set of over 2000 values. The model error on 5-fold cross-validation (CV) is 0.66 orders of magnitude in K/s. The error on leave-out-one-group CV on alloy system groups is 0.59 log units in K/s when the target alloy constituents appear more than 500 times in training data. Using this model, we make predictions for the set of compositions with melt-spun glasses in the database and for the full set of quaternary alloys that have constituents which appear more than 500 times in training data. These predictions identify a number of potential new bulk metallic glass systems for future study, but the model is most useful for the identification of alloy systems likely to contain good glass formers rather than detailed discovery of bulk glass composition regions within known glassy systems.

36 MATERIALS SCIENCE↗
NASA NTRS1981

Calculation of the critical cooling rate for amorphous Pd/77.5/Si/16.5/Cu/6/

The viscosity of the molten alloy Pd(77.5)Si(16.5)Cu(6) has been determined from 744 to 1000 C using an oscillating cup viscometer. Using these data (together with other pertinent physical data available for this alloy) in existing crystallization theory indicates that it could be made amorphous at cooling rates as low as 5-10 K/sec. This analysis assumes strictly homogeneous nucleation. Containerless solidification will be one good testing ground for the results of this analysis.

Steinberg, J.↗
NASA NTRS1983

Glass formation - A contemporary view

The process of glass formation is discussed from several perspectives. Particular attention is directed to kinetic treatments of glass formation and to the question of how fast a given liquid must be cooled in order to form a glass. Specific consideration is paid to the calculation of critical cooling rates for glass formation, to the effects of nucleating heterogeneities and transients in nucleation on the critical cooling rates, to crystallization on reheating a glass, to the experimental determination of nucleation rates and barriers to crystal nucleation, and to the characteristics of materials which are most conducive to glass formation.

Uhlmann, D. R.↗
NASA NTRS1995

(abstract) Undercooling Studies of the Bulk Metallic Glass Forming Zr(sub 41.2)Ti(sub 13.8)Cu(sub 12.5)Ni(sub 10.0)Be(sub 22.5) Alloy During Containerless Electrostatic Levitation Processing

Bulk glass forming metallic alloys have long been desired for technological applications and for investigation into liquid undercooling, solidification processes, and thermophysical properties. A glass forming alloy Zr(sub 41.2)Ti(sub 13.8)Cu(sub 12.5)Ni(sub 10.0)Be(sub 22.5) was used to investigate the thermal treatments affecting undercooling and vitrification. The experiments were performed using the high temperature high vacuum electrostatic levitator at JPL. A sample approximately 3 mm in diameter was melted, superheated, undercooled, and solidified while levitated in high vacuum. The results show that when the sample was held above its melting temperature for a sufficient period of time to dissolve oxides and then cooled faster than a critical cooling rate, it undercooled to the glass transition temperature, T(sub g), and formed a glassy alloy. The required critical cooling rate for metallic glass formation was obtained to be between 0.9 K per second and 1.2 K per second for the 42.4 mg sample.

levitation vitrification↗
NASA NTRS1982

Simplified model evaluation of cooling rates for glass-containing lunar compositions

The simplified model of glass formation and the development of partial crystallinity in cooled bodies has been applied to lunar compositions 10060, 15028, 15086, 15101, 15286, 15301, 15498, 15499, 60255, 65016, 77017, Apollo 15 green glass and LUNA 24 highland basalt. The critical cooling rates for glass formation predicted by the simplified model are found to be in good agreement (to within an order of magnitude) with those predicted by the exact treatment of crystallization statistics. These predicted critical cooling rates are in even better agreement (a factor of 2) with measured values of the rates required to form glasses of the materials.

Uhlmann, D. R.↗
NASA NTRS2006

Method of Estimating Continuous Cooling Transformation Curves of Glasses

A method is proposed for estimating the critical cooling rate and continuous cooling transformation (CCT) curve from isothermal TTT data of glasses. The critical cooling rates and CCT curves for a group of lithium disilicate glasses containing different amounts of Pt as nucleating agent estimated through this method are compared with the experimentally measured values. By analysis of the experimental and calculated data of the lithium disilicate glasses, a simple relationship between the crystallized amount in the glasses during continuous cooling, X, and the temperature of undercooling, (Delta)T, was found to be X = AR(sup-4)exp(B (Delta)T), where (Delta)T is the temperature difference between the theoretical melting point of the glass composition and the temperature in discussion, R is the cooling rate, and A and B are constants. The relation between the amount of crystallisation during continuous cooling and isothermal hold can be expressed as (X(sub cT)/X(sub iT) = (4/B)(sup 4) (Delta)T(sup -4), where X(sub cT) stands for the crystallised amount in a glass during continuous cooling for a time t when the temperature comes to T, and X(sub iT) is the crystallised amount during isothermal hold at temperature T for a time t.

Zhu, Dongmei↗
NASA NTRS1984

Crystallization of calcia-gallia-silica glasses

A thermal image furance is presently used to study the critical cooling rate for glass formation, and the kinetics of crystallization, of the compositions 18.4CaO-(81.6-X)Ga2O3-XSiO2, where X = 3, 6, 9, and 13.8. Crystallization was studied nonisothermally, and the data were analyzed in light of the Avrami (1939) equation. Critical cooling rate and crystallization activation energy are both found to decrease with increasing silica content, and the results obtained by the present technique are noted to agree with those obtained on the basis of differential thermal analysis measurements.

Ray, C. S.↗
DOE OSTI2021

The effects of Ti content and quenching on phase transformations, microstructures, and mechanical properties in uranium-titanium alloys

In this work, the effect of Ti content on phase transformations, microstructures, and mechanical properties of U-Ti alloys are described for alloys containing 0.3 wt.% to 2.0 wt.%Ti. Rapid cooling is required to overcome diffusional decomposition of γ-phase and facilitate diffusionless transformation to supersaturated variants of α-phase. Critical cooling rate increases with increasing Ti content, opposite to the trend observed in U-Mo and U-Nb alloys. This difference occurs because the martensite transformation temperatures in these relatively dilute U-Ti alloys are above the knee of the C-curve for diffusional decomposition, unlike those in the more concentrated U-Mo and U-Nb alloys. In these U-Ti alloys critical cooling rate depends on the amount of undercooling required to reach M s , which increases with increasing Ti content, and the time for diffusional decomposition to occur just above M s , which decreases with increasing Ti content. The net result is that higher cooling rates are required as Ti content increases. Full quenching results in diffusionless transformation of γ-phase to supersaturated variants of α-phase. Very dilute alloys transform via a γ → β → α m sequence of massive transformations. Martensitic γ → α' a transformation begins at ~0.4%Ti, and 100% α' a microstructures are obtained from ~0.65% to ~1.4% Ti. A transition to banded α'b martensite occurs at ~1.5%Ti. Evidence suggests that the α' a to α' b transition may occur when the cubic γ-phase first transforms to tetragonal γ°, which in turn transforms to orthorhombic α' b via the sequence γ → γ° → α' b . Fully quenched alloys exhibit moderate strengths and ductilities, and their supersaturation with Ti makes them amenable to subsequent age hardening. Subcritical quenching typically results in two-phase microstructures with lower ductilities and near-zero Ti-supersaturation, eliminating the possibility of subsequent age hardening.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Effects of Solidification Cooling Rates on Microstructures and Physical Properties of Fe-6.5%Si Alloys

Compared to the widely used Fe-3.2wt%Si steel, Fe-6.5wt%Si has superior electric and magnetic properties, including higher electrical resistivity, lower iron loss, higher permeability, and near zero magnetostriction. However, Fe-6.5wt%Si sheet is difficult to produce using traditional manufacturing processes as the high silicon content favors the formation of ordered phases that embrittle the material. Fortunately, these ordered phases can be suppressed if the alloy is cooled fast enough from a high temperature kinetically trapping the disordered solid solution or amorphous state. Planar flow casting is known for its rapid solidification rate. In order to consider it as a viable method to manufacture ductile Fe-6.5wt%Si sheets, the effect of cooling rate on physical properties of Fe-6.5wt%Si alloy are systematically investigated. In this work, various cooling rates are achieved by changing melt-spin wheel speeds, which significantly affect the solidification temperature profile and have profound effects on ordering, microstructures, textures, hardness, and magnetic properties. High cooling rates result in refined grains, reduced ordering, enhanced <100> out of the plane texture, decreased hardness, and increased coercivity. This study demonstrates a critical cooling rate at ~1.7 × 10 5 K/s, corresponding to a tangential wheel speed of 5-7 m/s, below which the hardness significantly increases in agreement with the sudden increase of the ordered phases that causes the material embrittlement.

36 MATERIALS SCIENCE↗
NASA NTRS1983

Cooling rates for glass containing lunar compositions

Cooling rates required to form glassy or partly-crystalline bodies of 14 lunar compositions have been estimated using a previously introduced, simplified model. The calculated cooling rates are found to be in good agreement with cooling rates measured for the same compositions. Measurements are also reported of the liquidus temperature and glass transition temperature for each composition. Inferred cooling rates are combined with heat flow analyses to obtain insight into the thermal histories of samples 15422, 14162, 15025, 74220, 74241, 10084, 15425, and 15427. The critical cooling rates required to form glasses of 24 lunar compositions, including the 14 compositions of the present study, are suggested to increase systematically with increasing ratio of total network modifiers/total network formers in the compositions. This reflects the importance of melt viscosity in affecting glass formation.

Fang, C. Y.↗
NASA NTRS1989

Thermal Analysis Of Reluctant Glass Formers

Thermocouple holds sample and monitors temperature during cooling. Ellipsoidal furnace provides controlled cooling rates for studies of thermal properties of reluctant glass formers. Glass tube inserted into furnace and used to blow helium on specimen to cool rapidly. Cooling curve analyzed to determine rate of cooling and such properties of sample as nucleation and recalescence temperatures at cooling rate. Continuous-cooling-crystallization boundaries determined empirically from plots of nucleation time vs. nucleation temperature from runs at large number of different rates of cooling. Apparatus used to examine glass-formation ability of material and critical cooling rate to form glass.

Ethridge, Edwin C.↗
DOE OSTI2023

Phase patterning of metallic glasses through superfast quenching of ion irradiation-induced thermal spikes

Amorphous metallic glasses (MGs) convert to crystalline solids upon annealing at a high temperature. Such a phase change, however, does not occur with the local melting caused by damage cascades introduced by ion irradiation, although the resulting thermal spikes can reach temperatures > 1000 K. This is because the quenching rate of the local melting zone is several orders of magnitude higher than the critical cooling rate for MG formation. Thus the amorphous structure is sustained. This mechanism increases the highest temperature at which irradiated MG sustains amorphous phase. More interestingly, if an irradiated MG is pre-annealed to form a polycrystalline structure, ion irradiation can locally convert this crystalline phase to an amorphous phase if the grains are nanometers in size and comparable to the damage cascade volume size. Combining pre-annealing and site selective ion irradiation, patterned crystalline-amorphous heterogeneous structures have been fabricated. This finding opens new doors for various applications.

36 MATERIALS SCIENCE↗
NASA NTRS1988

Apparatus for rapid thermal analysis studies of reluctant glass formers

An apparatus is described for performing rapid thermal analysis of milligram quantities of reluctant glass formers. Nucleation and crystallization kinetic analysis on samples cooled at very rapid cooling rates of 10 to 2500 C/s is described. The apparatus utilizes focused heating of a sample contained on a fine thermocouple. The measured times and temperatures for nucleation of crystallization at various cooling rates and experimental conditions permit the construction of continuous cooling crystallization boundaries and the determination of critical cooling rates for glass formation.

Ethridge, Edwin C.↗