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Metals

Metals are a class of elements characterized by their high electrical and thermal conductivity, malleability, and lustrous appearance.
They play a crucial role in a wide range of industries, from construction and transportation to electronics and medicine.
This MeSH term encompasses the study of the chemical, physical, and biological properties of metals, as well as their extraction, purification, and application.
Researchers in this field investigate topics such as metal alloys, corrosion, and the environmental impact of metal production and usage.
The PubCompare.ai platform can help optimize metal research protocols, ensuring reproducibility and accuracy by facilitating the comparison of methodologies from literature, preprints, and patents.

Most cited protocols related to «Metals»

1
Meta-Analysis Techniques in Genetic Studies
Cited 2357 times
The basic principle of meta-analysis is to combine the evidence for association from individual studies, using appropriate weights. METAL implements two approaches. The first approach converts the direction of effect and P-value observed in each study into a signed Z-score such that very negative Z-scores indicate a small P-value and an allele associated with lower disease risk or quantitative trait levels, whereas large positive Z-scores indicate a small P-value and an allele associated with higher disease risk or quantitative trait levels. Z-scores for each allele are combined across samples in a weighted sum, with weights proportional to the square-root of the sample size for each study (Stouffer et al., 1949 ). In a study with unequal numbers of cases and controls, we recommend that the effective sample size be provided in the input file, where Neff = 4/(1/Ncases+1/Nctrls). This approach is very flexible and allows results to be combined even when effect size estimates are not available or the β-coefficients and standard errors from individual studies are in different units. The second approach implemented in METAL weights the effect size estimates, or β-coefficients, by their estimated standard errors. This second approach requires effect size estimates and their standard errors to be in consistent units across studies. Asymptotically, the two approaches are equivalent when the trait distribution is identical across samples (such that standard errors are a predictable function of sample size). Key formulae for both approaches are in Table 1.

Formulae for meta-analysis

Analytical strategy
Sample size basedInverse variance based
InputsNi - sample size for study iβi- effect size estimate for study i
Pi−P-value for study i
Δi - direction of effect for study isei - standard error for study i
Intermediate StatisticsZi = Φ−1(Pi/2) * sign(Δi)wi = 1/SEi2
Overall Z-ScoreZ=β/SE
Overall P-valueP=2Φ(|−Z|)
Willer C.J., Li Y, & Abecasis G.R. (2010). METAL: fast and efficient meta-analysis of genomewide association scans. Bioinformatics, 26(17), 2190-2191.
Publication 2010
Alleles Metals Plant Roots
2
Covalent Docking Methods Evaluation
Cited 494 times
We have developed and tested two methods for docking of covalently-attached complexes: a grid-based approach and a modification of the flexible sidechain method. The grid-based approach calculates a special map for the site of attachment of the covalent ligand. A Gaussian function is constructed with zero energy at the site of attachment and steep energetic penalties at surrounding areas. The docking analysis is then performed by assigning a special atom type in the ligand for the atom that forms the covalent linkage. The docking simulation places this within the Gaussian well. One caveat is that this does not constrain the geometry of the covalent attachment to reasonable bond angles. To overcome this limitation, we tested the method using two Gaussian grids to define the bond that is formed during covalent linkage. Note, however, that the conformational freedom allowed with a single Gaussian grid may be an advantage if the method is used, for instance, to target ligands to metal coordination sites.
We also tested use of the flexible sidechain method for docking of covalent ligands. In this case, a coordinate file is created with the ligand attached to the proper sidechain in the protein, by overlapping ideal coordinates of the ligand onto the proper bond in the protein. This sidechain-ligand structure is then treated as flexible during the docking simulation, searching torsional degrees of freedom to optimize the interaction with the rest of the protein.
Morris G.M., Huey R., Lindstrom W., Sanner M.F., Belew R.K., Goodsell D.S, & Olson A.J. (2009). AutoDock4 and AutoDockTools4: Automated Docking with Selective Receptor Flexibility. Journal of computational chemistry, 30(16), 2785-2791.
Publication 2009
Ligands Metals Proteins STEEP1 protein, human
3
Mapping Annotated Residues from Swiss-Prot to PDB
Cited 263 times
The numbered positions of annotated residues in the Swiss-Prot sequence often do not align to the same numbered positions of the sequence from the PDB structure. Therefore, a mapping of positions between the Swiss-Prot sequence and the PDB sequence must be obtained. We use a variation of the Needleman and Wunsch algorithm to identify if a sequence of a PDB structure can be found to match the sequence containing annotated residues from the Swiss-Prot database.
Specifically, every Swiss-Prot sequence containing one or more annotated residues and a link to a PDB structure was aligned to the corresponding sequence of the PDB structure. Standard annotations of Swiss-Prot used include post-translational modifications (MOD_RES), covalent binding of a lipid moiety (LIPID), glycosylation sites (CARBOHYD), post-translational formed amino acid bonds (CROSSLNK), metal binding sites (METAL), chemical group binding sites (BINDING), calcium binding regions (CA_BIND), DNA binding regions (DNA_BIND), nucleotide phosphate binding regions (NP_BIND), zinc finger regions (ZN_FING), enzyme activity amino acids (ACT_SITE) and any interesting single amino acid site (SITE). To ensure that the mapping is accurate, only alignments of two sequences with a sequence identity greater than ninety five percent were used. The annotated positions from Swiss-Prot are then transferred onto the PDB sequence, as long as the position is not aligned to a gap.
Dundas J., Ouyang Z., Tseng J., Binkowski A., Turpaz Y, & Liang J. (2006). CASTp: computed atlas of surface topography of proteins with structural and topographical mapping of functionally annotated residues. Nucleic Acids Research, 34(Web Server issue), W116-W118.
Publication 2006
Amino Acids Binding Sites Calcium enzyme activity Lipid A Lipids Metals Nucleotides Phosphates Protein Biosynthesis Protein Glycosylation Sequence Alignment Zinc Fingers
4
Nano-CT Visualization of Feather Microstructure
Cited 234 times
For nano-CT, one black contour feather from each species was washed and then soaked in an aqueous solution of Lugol’s solution—1% (wt/v) iodine metal (I2) + 2% potassium iodide (KI) in water—for 2–3 weeks to improve X-ray contrast30 (link). Feathers were scanned at beamline 2-BM at the Advanced Photon Source facility at U.S. Department of Energy’s Argonne National Laboratory, Argonne, Il. Feathers were mounted to a post using modeling clay and surrounded by a Kapton tube to reduce sample motion. Feathers were aligned in the beam to scan a portion of the distal tip that is exposed in the plumage. Scans were made with an exposure time of 30 ms at 24.9 keV to acquire 1500 projections as the sample rotated 180° at 3° s−1. Data sets were reconstructed as TIFF image stacks using the TomoPy Python package (https://tomopy.readthedocs.io) in Linux on a Dell Precision T7610 workstation with two Intel Xeon processors yielding 16 cores, 192-GB RAM, and NVIDIA Quadro K6000 with 12-GB VRAM. The isotropic voxel dimensions of the image stacks were 0.65 µm and the field of view of each data set was ~1.5 mm3.
McCoy D.E., Feo T., Harvey T.A, & Prum R.O. (2018). Structural absorption by barbule microstructures of super black bird of paradise feathers. Nature Communications, 9, 1.
Full text: Click here
Publication 2018
Clay Feathers Lugol's solution Metals Potassium Iodide Python Radiography Radionuclide Imaging
5
Preparation of cDNA for Illumina Sequencing
Cited 159 times
Preparation of cDNA followed the procedure described in Mortazavi et al.2 (link), with minor modifications as described below. Prior to fragmentation, a 7 uL aliquot (∼ 500 pgs total mass) containing known concentrations of 7 “spiked in” control transcripts from A. thaliana and the lambda phage genome were added to a 100 ng aliquot of mRNA from each time point. This mixture was then fragmented to an average length of 200 nts by metal ion/heat catalyzed hydrolysis. The hydrolysis was performed in a 25 uL volume at 94°C for 90 seconds. The 5X hydrolyis buffer components are: 200 mM Tris acetate, pH 8.2, 500 mM potassium acetate and 150 mM magnesium acetate. After removal of hydrolysis ions by G50 Sephadex filtration (USA Scientific catalog # 1415-1602), the fragmented mRNA was random primed with hexamers and reverse-transcribed using the Super Script II cDNA synthesis kit (Invitrogen catalog # 11917010). After second strand synthesis, the cDNA went through end-repair and ligation reactions according to the Illumina ChIP-Seq genomic DNA preparation kit protocol (Illumina catalog # IP102-1001), using the paired end adapters and amplification primers (Illumina Catalog # PE102-1004). Ligation of the adapters adds 94 bases to the length of the cDNA molecules.
Trapnell C., Williams B.A., Pertea G., Mortazavi A., Kwan G., van Baren M.J., Salzberg S.L., Wold B.J, & Pachter L. (2010). Transcript assembly and abundance estimation from RNA-Seq reveals thousands of new transcripts and switching among isoforms. Nature biotechnology, 28(5), 511-515.
Publication 2010
Acetate Anabolism Bacteriophage lambda Buffers Chromatin Immunoprecipitation Sequencing DNA, Complementary DNA Chips Filtration Genome Hydrolysis Ions Ligation magnesium acetate Metals Oligonucleotide Primers Potassium Acetate RNA, Messenger sephadex Tromethamine

Most recents protocols related to «Metals»

1
Enhanced Absorbency of Embossed SAM Sheets
Not available on PMC !

Example 1

A 1 g compressed SAM sheet was formed without embossing. To ensure that Comparative Example 1 had the same compactness as Example 1, meaning that both samples experienced the same compressing pressure, the SAM sheets were each placed between two flat metal plates and compressed twice with a 1000 lb load for 10 minutes using the Carver hydraulic compressor (CE, Model 4350). In this way, the void volumes between and within SAM particles are quite close, if not the same, for Comparative Example 1 and Example 1. The sample was dried in a convection oven at 80° C. for 12 hours before testing.

A 1 g compressed SAM sheet was formed without embossing. The prepared SAM sheet was placed on a flat metal plate, covered with a 1″×1″ metal patterned plate with protruding balls of 250 μm diameter, the balls side facing downward towards the SAM sheet (FIG. 1). The Carver hydraulic compressor (CE, Model 4350) was used to create the embossing pattern by applying a 1000 lb load to a plasticized SAM sheet for 5 minutes. After that, the SAM sheet was flipped over and compressed one more time with the metal balls under same pressure and same dwell time. The resultant SAM sheet has a clear pattern on the surface (FIG. 2). The scale bar shows the diameter of dent of 243 μm. The size of the dent is consistent with the size of metal balls of the embossing plate.

The final 1 g compressed SAM sheet had two-sided embossing. The sample was dried in a convection oven at 80° C. for 12 hours before testing.

The protrusions of this example were ball-shaped, but the protrusion of the pins could be any shape. Shapes without sharper corners, such as spheres, could be less damaging to the SAM particles. The depth of the indentations from the shapes could be in the range of from about 10 μm to 200

Absorbency Evaluation.

Equal masses of embossed and non-embossed SAM sheet samples were each individually dropped in a 100 mL beaker containing 30 mL NaCl solution, which contained blue dye to improve visualization during testing. The time and process of the SAM sheet completely absorbing the saline solution was monitored and compared.

The testing process for both samples to compare their absorbency properties is shown in FIGS. 3a-3e. FIG. 3a shows the testing beakers with 30 mL NaCl solution and blue dye. FIG. 3b shows at the start of the testing (0 min) by adding SAM sheets into the respective NaCl solutions. FIG. 3c shows the completion of absorption of liquid for Example 1 at 27 minutes. After completion, the swollen SAM particles were cast off onto white paper to verify the complete absorption of the fluid (FIG. 3d). At 40 min, Comparative Example 1 completed absorbing all fluid and was cast off onto white paper to verify completion (FIG. 3e). By the time Comparative Example 1 was cast off onto white paper, Example 1 had already turned white because it had finished the absorbing process 13 minutes earlier and the absorbed fluid already diffused into the center of each SAM particle. Absorbency times are summarized in Table 1.

TABLE 1
Absorbency times for SAM sheets.
SampleIntake time (min)
Comparative Example 140
Example 127

Compressing SAM particles into sheets generally leads to lower intake rates and higher intake times compared with SAM particles that are not compressed into sheets due to the loss of free volume within SAM molecular structure and surface area. However, the results demonstrated herein prove that SAM with surface embossing could lead to increase of surface area, thereby increasing the absorbency intake rate compared to the compressed SAM without embossing.

Flexible Absorbent Binder Film.

FAB is a proprietary crosslinked acrylic acid copolymer that develops absorbency properties after it is applied to a substrate and dried, FAB itself can also be casted into film and dried, yet the resultant 100% FAB film is quite rigid and stiff. The chemistry of FAB is similar to standard SAPs except that the latent crosslinking component allows it to be applied onto the substrate of choice as an aqueous solution and then converted into a superabsorbent coating upon drying. When the water is removed, the crosslinker molecules in the polymeric chain come into contact with each other and covalently bond to form a crosslinked absorbent.

In the examples of this disclosure, FAB was coated on a nonwoven substrate to provide a single layer with both intake and retention functions, as well as flexibility. FAB solution with 32% (wt/wt) solids was coated on a nonwoven substrate through a slot die with two rolls. After coating, the coated film was cured by drying in a convection oven at 55° C. for 20-30 minutes, or until the film was dry, to remove the water.

Compression embossing was applied on FAB films. Two-sided embossing was applied on a FAB film. The absorbent properties were characterized and compared through saline absorption testing. The FAB film with an embossed pattern showed 91.67% faster intake rate compared with the FAB film without an embossed pattern.

US11864985B2. Absorbent composites containing embossed superabsorbent materials (2024-01-09). Kimberly-Clark Worldwide, Inc. [US]. Inventors: Feng Chen [US], Wing-Chak Ng [US], Mark M. Mleziva [US].
Full text: Click here
Patent 2024
acrylate Convection Electroplating Metals Molecular Structure Muscle Rigidity Polymers Pressure Retention (Psychology) Saline Solution SKAP2 protein, human Sodium Chloride Urination
2
Synthesis of High-Conductivity Entropy-Stabilized Nanometal Oxide
Not available on PMC !

Example 1

Provided is a preparation method for an A-site high-entropy nanometer metal oxide (Gd0.4Er0.3La0.4Nd0.5Y0.4)(Zr0.7, Sn0.8, V0.5)O7 with high conductivity, the method including the following steps.

    • (1) Gd(NO3)3, Er(NO3)3, La(NO3)3, Nd(NO3)3, Y(NO3)3, ZrOSO4, SnC14 and NH4VO3 were taken at a molar ratio of 0.4:0.3:0.4:0.5:0.4:0.7:0.8:0.5, added to a mixed solution of deionized water/absolute ethyl alcohol/tetrahydrofuran at a mass ratio of 0.3:3:0.5, and stirred for five minutes to obtain a mixed liquid I. The ratio of the total mass of Gd(NO3)3, Er(NO3)3, La(NO3)3, Nd(NO3)3, Y(NO3)3, ZrOSO4, SnC14 and NH4VO3 to that of the mixed solution of deionized water/absolute ethyl alcohol/tetrahydrofuran (0.3:3:0.5) is 12.6%.
    • (2) Para-phenylene diamine, hydrogenated tallowamine, sorbitol and carbamyl ethyl acetate at a mass ratio of 1:0.2:7:0.01 were taken, added to propyl alcohol, and stirred for one hour to obtain a mixed liquid II. The ratio of the total mass of the para-phenylene diamine, the hydrogenated tallowamine, the sorbitol and the carbamyl ethyl acetate to that of the propyl alcohol is 7.5%;
    • (3) The mixed liquid I obtained in step (1) was heated to 50° C., and the mixed liquid II obtained in step (2) was dripped at the speed of one drop per second, into the mixed liquid I obtained in step (1) with stirring and ultrasound, and heated to the temperature of 85° C. after the dripping is completed and the temperature was maintained for three hours while stopping stirring, and the temperature was decreased to the room temperature, so as to obtain a mixed liquid III. The mass ratio of the mixed liquid I to the mixed liquid II is 10:4.
    • (4) The mixed liquid III was added to an electrolytic cell with using a platinum electrode as an electrode and applying a voltage of 3 V to two ends of the electrode, and reacting for 13 minutes, to obtain a mixed liquid IV.
    • (5) The mixed liquid IV obtained in step (4) was heated with stirring, another mixed liquid II was taken and dripped into the mixed liquid IV obtained in step (4) at the speed of one drop per second. The mass ratio of the mixed liquid II to the mixed liquid IV is 1.05:1.25; and after the dripping is completed, the temperature was decreased to the room temperature under stirring, so as to obtain a mixed liquid V.
    • (6) A high-speed shearing treatment was performed on the mixed liquid V obtained in step (5) by using a high-speed shear mulser at the speed of 20000 revolutions per minute for one hour, so as to obtain a mixed liquid VI.
    • (7) Lyophilization treatment was performed on the mixed liquid VI to obtain a mixture I;
    • (8) The mixture I obtained in step (7) and absolute ethyl alcohol were mixed at a mass ratio of 1:2 and uniformly stirred, and were sealed at a temperature of 210° C. for performing solvent thermal treatment for 18 hours. The reaction was cooled to the room temperature, the obtained powder was collected by centrifugation, washed with deionized water and absolute ethyl alcohol eight times respectively, and dried to obtain a powder I.
    • (9) The powder I obtained in step (8) and ammonium persulfate was uniformly mixed at a mass ratio of 10:1, and sealed and heated to 165° C. The temperature was maintained for 13 hours. The reaction was cooled to the room temperature, the obtained mixed powder was washed with deionized water ten times, and dried to obtain a powder II.
    • (10) The powder II obtained in step (4) was placed into a crucible, heated to a temperature of 1500° C. at a speed of 3° C. per minute. The temperature was maintained for 7 hours. The reaction was cooled to the room temperature, to obtain an A-site high-entropy nanometer metal oxide (Gd0.4Er0.3La0.4Nd0.5Y0.4)(Zr0.7, Sn0.8, V0.5)O7 with high conductivity.

As observed via an electron microscope, the obtained A-site high-entropy nanometer metal oxide with high conductivity is a powder, and has microstructure of a square namometer sheet with a side length of about 4 nm and a thickness of about 1 nm.

The product powder was taken and compressed by using a powder sheeter at a pressure of 550 MPa into a sheet. Conductivity of the sheet is measured by using the four-probe method, and the conductivity of the product is 2.1×108 S/m.

A commercially available ITO (indium tin oxide) powder is taken and compressed by using a powder sheeter at a pressure of 550 MPa into a sheet, and the conductivity of the sheet is measured by using the four-probe method.

As measured, the conductivity of the commercially available ITO (indium tin oxide) is 1.6×106 S/m.

US11866343B2. A-site high-entropy nanometer metal oxide with high conductivity, and preparation method thereof (2024-01-09). Zhejiang University [CN]. Inventors: Lingjie Zhang [CN], Weiwei Cai [CN], Ningzhong Bao [CN].
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Patent 2024
1-Propanol 4-phenylenediamine Absolute Alcohol ammonium peroxydisulfate Cells Centrifugation Electric Conductivity Electrolytes Electron Microscopy Entropy Ethanol ethyl acetate Freeze Drying indium tin oxide Metals Molar Oxides Platinum Powder Pressure propyl acetate Solvents Sorbitol tetrahydrofuran Ultrasonography
3
Antibacterial Dental Implant Surface Modification
Not available on PMC !

Example 2

As discussed herein above, the disclosed methods improve the antiseptic properties of a dental implant without using charged metallic ions via conversion of the nitrogen moieties in titanium nitride surface to a positively charged quaternary ammonium via a Menschutkin reaction.

To prepare the antibacterial quaternized TiN surface, an implant which has been coated with TiN was used. The implant was cleaned to improve yield. The implant was washed with two solvents in sequence, acetone and isopropanol, to remove any dust particulate and other residue. The native oxide layer was removed by sonicating in 1:10 HCl:deionized water for 1 minute. This treatment additionally removes any residue that may not have been removed by the solvents. Acetonitrile was used as the solvent; however, any solvent may be used with preference for polar solvents giving improved reaction times (Stanger K., et al. J Org Chem. 2007 72(25):9663-8; Harfenist M., et al. J Am Chem Soc 1957 79(16):4356-4358). An excess of allyl bromide was added to the solvent and continuously stirred. The sample was then submerged in the solution, and full reaction of the surface occurred within about 60 minutes, as confirmed by contact angle measurement. A reference was also measured by submerging in solvent for the duration with no reactant to ensure any changes in surface properties was due to the quaternization.

TABLE 2
SampleContact Angle (°)
As-deposited TiN<6
In solvent 2 hrs (no reaction)16 ± 2
Allyl bromide 30 minutes67 ± 1
Allyl bromide 60 minutes72 ± 3
Allyl bromide 120 minutes71 ± 2

Without wishing to be bound by a particular theory, the increased hydrophobicity of the treated surfaces can be due to the presence of the allyl groups on the surface which will impart some hydrophobicity. The contact angle measurements provide information on whether or not a reaction has occurred and whether it has saturated.

The biocidal activity was tested using live bacteria cultures from a patient's mouth, which provides the full flora to act against rather than targeting an individual strain of bacteria. The bacteria was incubated on the sample surface using several bacteria film thicknesses. The thickness is defined by keeping the same interaction surface area while varying the volume of bacteria solution added. Across two separate patients and several separate growths, within 4 hours 40-50% reduction in bacteria unit counts were observed for quaternized TiN as compared to traditional Titanium implants, outperforming traditional TiN coatings. FIG. 4 shows for two separate patients a set of typical bacteria growth result of the quaternized samples. The exact efficiency varies, as each patient has different flora which varies depending on environmental factors such as hygiene, diet, and familial history.

Unless defined otherwise, all technical and scientific terms used herein have the same meanings as commonly understood by one of skill in the art to which the disclosed invention belongs. Publications cited herein and the materials for which they are cited are specifically incorporated by reference.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present disclosure without departing from the scope or spirit of the disclosure. Other aspects of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.

US11864964B2. Quarternized titanium-nitride anti-bacterial coating for dental implants (2024-01-09). University of Florida Research Foundation, Inc. [US]. Inventors: Josephine F. Esquivel-Upshaw [US], Fan Ren [US], Patrick Carey [US], Arthur E. Clark, Jr. [US], Christopher D. Batich [US].
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Patent 2024
Acetone acetonitrile allyl bromide Ammonium Anti-Bacterial Agents Anti-Infective Agents, Local Bacteria Diet Implant, Dental Ions Isopropyl Alcohol Metals Nitrogen Oral Cavity Oxides Patients Solvents Strains Surface Properties Titanium titanium nitride
4
Optimizing Secondary Battery Pouch Film Production
Not available on PMC !

Example 1

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 100° C.

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 100° C.

Example 2

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 120° C.

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 120° C.

Example 3

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 135° C.

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 135° C.

Example 4

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 150° C.

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 150° C.

Example 5

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 165° C.

Example 6

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 180° C.

Example 7

A secondary battery pouch film is produced, after the drying process temperature of the two-component type solvent-based emulsion having a start temperature of 175° C. to 190° C. is set to 200° C.

Example 8

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 165° C.

Example 9

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 180° C.

Example 10

A secondary battery pouch film is produced, after the process temperature of the two-component type solvent-based emulsion having a start temperature lowered to 135° C. to 150° C. is set to 200° C.

TABLE 1
Start Drying process
No.temperature (° C.)temperature (° C.)
Comparative Example 1175~190100
Comparative Example 2120
Comparative Example 3135
Comparative Example 4150
Comparative Example 5165
Comparative Example 6180
Comparative Example 7200
Example 1135~150100
Example 2120
Example 3135
Example 4150
Comparative Example 8165
Comparative Example 9180
Comparative Example 10200

Evaluation of Properties

Evaluation of Initial Peel Strength

    • (1) An experimental sample is prepared by cutting the secondary battery pouch film to have a size of 1.5 cm by 15 cm in width and length, respectively.
    • (2) The metal layer and the sealant layer are peeled off, and the peel strength is measured.

Evaluation of Hydrofluoric Acid Resistance

    • (1) After the secondary battery pouch film is cut to have a size of 10 cm by 20 cm, two surfaces on both sides thermally adhered to each other.
    • (2) A manufacturing solution (electrolyte+water (10,000 ppm (about 1%) of concentration of water in the solution)) is put inside the secondary battery pouch having the two surfaces adhering to each other, thermal adhering is performed, and a pack is manufactured.
    • (3) The pack is stored at a high-temperature condition (85° C.) for 24 hours.
    • (4) The electrolyte inside the pack is removed, and the sample is prepared (width 1.5 cm and length 15 cm) in the same manner as in the evaluation of initial peel strength.
    • (5) The peel strength between the metal layer and the sealant layer is measured.

Evaluation of Electrolyte Resistance

    • (1) An experimental sample is prepared by cutting the secondary battery pouch film to have a size of 1.5 cm by 15 cm in width and length, respectively.
    • (2) The prepared sample is impregnated with a standard electrolyte (1.0 M LiPF6(EC/DEC/EMC: 1/1/1)) and is stored at a high temperature condition (85° C.) for 24 hours.
    • (3) After the electrolyte is washed off, the metal layer and the sealant layer are peeled off, and the peel strength is measured.

Evaluation of Formability

    • (1) A sample is prepared by cutting the produced secondary battery pouch film to have a size of 15 cm by 15 cm.
    • (2) The prepared samples are formed by using a test die (size of 3 cm×4 cm) manufactured by Youlchon Chemical, Co., Ltd.
    • (3) Evaluation of formability is repeatedly performed by changing the setting of the forming depth and is performed until ten or more samples are not broken.
    • (4) A forming depth, in ten or more samples are not broken, is measured.

Evaluation of Penetration Strength

    • (1) A sample having a width of 35 mm and a length of 600 mm is produced from the secondary battery pouch film.
    • (2) The penetration strength is measured at intervals of about 40 mm in a direction from the outer layer toward the inner layer.
    • (3) After the strength is measured ten times, an average value thereof is recorded.

In this case, the higher the formability, a forming process range may be wider during manufacturing of a battery. It is appropriate that the electrolyte resistance strength is equal to or higher than 90% of the initial peel strength, and the hydrofluoric acid resistance strength should be equal to or higher than 5 N/15 mm. Since the electrolyte resistance strength and the hydrofluoric acid resistance strength are much affected by the initial peel strength, it is appropriate that the initial peel strength is equal to or higher than 14 N/15 mm.

Table 2 shows evaluation of physical properties based on the curing start temperature and the drying process temperature.

TABLE 2
Hydrofluoric
DryingInitialElectrolyteacid
StartprocesspeelresistanceresistancePenetration
temperaturetemperaturestrengthstrengthstrengthstrengthFormability
No.(° C.)(° C.)(N/15 mm)(N/15 mm)(N/15 mm)(N)(mm)
Comparative1751002PeelingPeeling18.46.5
Example 1~190
Comparative1202.3PeelingPeeling19.26.6
Example 2
Comparative1352.2PeelingPeeling19.36.6
Example 3
Comparative1506.4PeelingPeeling19.36.5
Example 4
Comparative16514.514.15.824.26.3
Example 5
Comparative18014.814.35.724.66.1
Example 6
Comparative20015.614.85.824.56.1
Example 7
Example 11351009.2 8.13.919.46.8
Example 2~15012012.411.64.320.26.7
Example 313514.614.26.221.86.7
Example 415015.014.36.422.36.8
Comparative16515.114.86.423.86.3
Example 8
Comparative18015.715.16.224.26.1
Example 9
Comparative20016.115.46.524.76.0
Example 10

As known from the above, when an emulsion having a start temperature of 175° C. to 190° C. (Comparative Examples 1, 2, 3, and 4) is applied, the initial peel strength is relatively very low to be 10 N or lower when the drying process temperature is 150° C. or lower. The low initial peel strength resulted in a phenomenon where the sealant layer and the metal layer are completely separated from each other during evaluation of the electrolyte resistance strength and the hydrofluoric acid resistance strength.

When the drying process temperature is 165° C. to 200° C. (Comparative Examples 5, 6, and 7), the initial peel strength, the electrolyte resistance strength, and the hydrofluoric acid resistance strength are all good. However, the penetration strength increased to 24 N or higher. As well, a result that the formability does not reach 6.5 mm is obtained.

When the emulsion having a start temperature lowered to 135° C. to 150° C. is applied, the initial peel strength is 10 N/15 mm or lower only when the drying process temperature is 100° C. (Example 1), and the initial peel strength is 12 N/15 mm or higher in a drying process condition of 120° C. or higher (Examples and Comparative Examples 8 to 10). It is confirmed that a decrease in start temperature improves the adhesiveness even at a low drying process temperature.

However, the hydrofluoric acid resistance strength does not reach 5 N/15 mm in the 120° C. condition (Example 2), and the initial peel strength, the electrolyte resistance strength, and the hydrofluoric acid resistance strength are all good in conditions of 135° C. or higher (Examples 3 and 4 and Comparative Examples 8 to 10).

Similar to Comparative Examples 1 to 7, results of an increase in penetration strength in a condition of 165° C. to 200° C. (Comparative Examples 8, 9, 10) and the result of formability smaller than 6.5 mm is obtained.

The penetration strength increased to 20 N or higher at a condition of 135° C. to 150° C. (Examples 3 and 4), but has the best of the formability of 6.5 mm or more.

Therefore, only in a drying process temperature condition corresponding to the start temperature, all the properties of the initial peel strength, the electrolyte resistance strength, the hydrofluoric acid resistance strength are appropriate. When the drying process temperature is above 150° C., and particularly 165° C. or higher as found in an experiment, the penetration strength of the secondary battery pouch film significantly increases, and thus the formability decreases.

Therefore, in order to appropriately obtain all the physical properties, it is preferable to lower the drying process temperature to 150° C. or below, and to this end, it is preferable to lower the start temperature of the solvent-based emulsion to 150° C. or below.

According to the exemplary embodiments of the invention, when the secondary battery pouch film is manufactured, the primer layer composition that is interposed between the metal layer and the melt-extrusion resin layer or the sealant layer is made of a two-component curing-type organic solvent-based emulsion composition containing acid-modified polypropylene and a curing agent, wherein the curing start temperature and the drying process temperature are adjusted, and thermal lamination is not performed. Thereby, good formability, as well as good initial peel strength, hydrofluoric acid resistance, electrolyte resistance, etc. may be achieved.

The present invention was made under Project ID 20007148 from the Ministry of Trade, Industry and Energy, Korea Evaluation Institute of Industrial Technology under research project “Development of Technology of Materials and Components—Materials and Components Packaging Type”, research title “Performance Evaluation of Medium and Large Size Secondary Battery Pouch and Empirical Research for Application to Demand Companies” granted to Youl Chon Chemical Co., Ltd. For the period 2019 Sep. 1-2021 Feb. 28.

While the present invention has been described with respect to the specific embodiments, it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the following claims.

US11876235B2. Primer layer composition, secondary battery pouch film using the same, and method of manufacturing the same (2024-01-16). Youlchon Chemical Co., Ltd. [KR]. Inventors: Nok Jung Song [KR], Han Chul Park [KR], Hee Sik Han [KR], Ji Min Lee [KR].
Full text: Click here
Patent 2024
Acids Adhesiveness Cold Temperature Electrolytes Emulsions Fever Hydrofluoric acid Metals Oligonucleotide Primers Physical Processes Polypropylenes Resins, Plant Solvents Technology Assessment
5
Polyamide-Imide Films for Flexible Displays
Not available on PMC !

Example 8

An adhesive layer (product name: OCA #8146 from 3M company) was interposed between the prepared film and a PET substrate to obtain a multilayer film. It was folded to have a radius of curvature of 3 mm, which was left at a low temperature of −20° C. for 72 hours, and then unfolded. The extent of wrinkles was visually observed. In such event, if no wrinkles were visually observed, it was evaluated as o. If wrinkles were visually observed slightly, it was evaluated as Δ. If wrinkles were visually observed readily, it was evaluated as x.

TABLE 1
Ex. 1aEx. 2aEx. 3aEx. 4aC. Ex. 1aC. Ex. 2aC. Ex. 3a
CompositionDiamineTFMBTFMBTFMBTFMBTFMBTFMBTFMB
100100100100100100100
Dianhydride6FDA 36FDA 36FDA 106FDA 156FDA 246FDA 06FDA 0
DicarbonylTPC 75TPC 75TPC 75TPC 75TPC 29TPC 75TPC 75
compoundIPC 22IPC 22IPC 15IPC 10BPDC 47IPC 25IPC 25
Imide:amide3:973:9710:9015:8524:760:1000:100
Type of metal saltLiClLi2CO3Li2CO3Li2CO3—LiBrLiBr
Content of metal salt (based on10.50.50.5011
100 parts by weight of polymer
solids content)
Tensile strength (TS1a)kgf/mm232.131.630.427.726.329.221.3
Tensile strength at highkgf/mm226.425.924.62318.721.617.1
temperatures (TS2a)
TSR%82.2481.9680.9283.0371.1073.9780.28
Elongation at break%23.722.721.4218.817.317.618.3
(EL1a)
Elongation at break at%20.718.218.915.114.714.414.3
high temperatures
(EL2a)
ELR%87.3480.1888.2480.3284.9781.8278.14
Modulus (MO1a)GPa7.437.256.86.55.867.47.6
Modulus at highGPa5.85.85.45.14.25.35
temperatures (MO2a)
MOR%78.0680.0079.4178.4671.6771.6265.79
Film thicknessμm50505050505050
Light transmittance%88.888.989.589.688.988.587.9
Haze%0.50.50.40.40.50.82.4
YI—2.82.52.52.52.93.66.12
Flexural resistance (1 R, 20K)passpasspasspassfailfailpass
ProcessDrying step125/15 125/15 115/15 115/15 150/20 150/20 115/15 
(temp./min.)
First thermal125/1 125/1 115/1 115/1 150/1 150/1 115/1 
treatment step
(temp./min.)
Second thermal225/10 225/10 225/10 225/10 225/10 225/10 225/10 
treatment step
(temp./min.)

As can be seen from Table 1 above, the polyamide-imide films of Examples 1a to 4a had an MOR value of 75% or more. Thus, they maintained the modulus at least at a certain level even under the harsh conditions of high temperatures.

Since the display device is an electronic device, it generates heat during its use and it is to be used in a hot place as well, it is essential to secure mechanical properties at least at a certain level at high temperatures. Specifically, when a film is applied to a cover window for a display device, if the MOR value is 75% or more, no problem arises when a display device is fabricated.

In addition, the polyamide-imide films of Examples 1a to 4a were all excellent in the TSR value, ELR value, MO1a value, TS1a value, EL1a value, MO2a value, TS2a value, and EL2a value, in addition to the MOR value. That is, the polymer films of Examples 1a to 4a had high mechanical properties such as tensile strength, elongation at break, and modulus at room temperature and maintained the excellent mechanical properties even after the treatment under the severe conditions of high temperatures for a certain period of time.

Further, the polyamide-imide films of Examples 1a to 4a were all excellent in the evaluation of flexural resistance.

In contrast, since the films of Comparative Examples 1a to 3a had a low MOR value of 72% or less, when the film is applied to cover window for display device, it would have defects in appearance stability. In addition, the films of Comparative Examples 1a and 2a failed in the evaluation of flexural resistance. Thus, they are unsuitable for application to foldable display device or flexible display device.

TABLE 2
Ex. 1bEx. 2bEx. 3bEx. 4bEx. 5bEx. 6bEx. 7bEx. 8bC. Ex. 1bC. Ex. 2b
CompositionDiamineTFMBTFMBTFMBTFMBTFMBTFMBTFMBTFMBTFMBTFMB
100100100100100100100100100100
Dianhydride6FDA6FDA6FDA6FDA6FDA6FDA6FDA6FDA—6FDA
33791215242550
BPDA
10
DicarbonylTPC 70TPC 70TPC 65TPC 69TPC 66TPC 75TPC 29TPC 65TPC 75TPC 25
compoundIPC 27IPC 27IPC 28IPC 22IPC 22IPC 10BPDC 47IPC 25IPC 25
Imide:amide3:973:977:939:9112:8815:8524:7635:650:10050:50
Type/content metal saltLiCl/1LiCl/0.5——————LiBr/1—
Tensile strengthkgf/mm228.4532.1329.630.730.127.529.6128.3124.6122.62
(TS1b)
Tensile strengthkgf/mm227.7828.2430.128.62826.127.4122.9523.222.71
at low
temperatures
(TS2b)
dTS%2.3612.111.696.846.985.097.4318.935.730.40
Elongation at%19.8923.6719.223.12319.427.827.81178.9
break (EL1b)
Elongation at%23.0617.6821.51919.517.121.220.616.211.71
break at low
temperatures
(EL2b)
dEL%115.9425.3111.9817.7515.2211.8623.7425.934.7131.57
Modulus (MO1b)GPa7.427.436.025.925.546.156.446.657.454.83
Modulus at lowGPa7.577.646.216.035.716.326.556.767.464.87
temperatures
(MO2b)
dMO%2.022.833.161.863.072.761.7111.650.130.83
LMO1GPa1.4761.7591.1561.3681.2741.1931.7901.8491.2670.430
LMO2GPa1.7461.3511.3351.1461.1131.0811.3891.3931.2090.570
Thicknessμm50505050505050505050
Transmittance%89898989.189.3898988.588.490.8
Haze%0.470.480.660.520.670.560.460.542.410.41
YI—2.622.653.42.963.122.442.872.74.59141
Folding evaluation○Δ○○○○○Δxx
at low temperatures
(3 R, −20° C., 72 hours)
ProcessDrying125/15 125/15 125/15 125/15 115/15 115/15 115/15 115/15 150/20 115/15 
(temp/min.)First thermal125/1 125/1 125/1 125/1 115/1 115/1 115/1 115/1 150/1 150/1 
treatment
Second thermal225/10 225/10 225/10 225/10 225/10 225/10 225/10 225/10 225/10 225/10 
treatment

As can be seen from Table 2 above, the polyamide-imide films of Examples 1b to 8b had a dMO value of 1% to 8%. Thus, they maintained the modulus at least at a certain level even under the harsh conditions of low temperatures.

In the case where the polyamide-imide film is applied to a cover window for a display device and to a display device, it may be used in an extremely cold environment. Thus, it is essential to secure mechanical properties at least at a certain level even in such an extremely cold environment. Specifically, when the polyamide-imide film is applied to a cover window for a display device and to a display device, if the dMO value is within 1% to 8%, no problem arises.

In addition, the polyamide-imide films of Examples 1b to 8b were all excellent in the dTS value, dEL value, MO1b value, TS1b value, EL1b value, MO2b value, TS2b value, and EL2b value, in addition to the dMO value. That is, the polymer films of Examples 1b to 8b had high mechanical properties such as tensile strength, elongation at break, and modulus at room temperature and maintained the excellent mechanical properties even after the treatment under the severe conditions of low temperatures for a certain period of time.

Further, the polyamide-imide films of Examples 1b to 8b were all excellent in the folding characteristics at low temperatures.

In contrast, since the films of Comparative Examples 1b and 2b had a low dMO value of 1% or less, when it is applied to a cover window for a display device, it would not be balanced with other layers, resulting in cracks, which is defective in terms of the appearance stability. In addition, the films of Comparative Examples 1b and 2b failed in the evaluation of flexural resistance at low temperatures. Thus, they are unsuitable for application to a foldable display device or a flexible display device.

US11873372B2. Polyamide-imide film, preparation method thereof, and cover window comprising same (2024-01-16). SK microworks Co., Ltd. [KR]. Inventors: Han Jun Kim [KR], Sunhwan Kim [KR], Dae Seong Oh [KR], Jin Woo Lee [KR], Sang Hun Choi [KR], Jung Hee Ki [KR], Dong Jin Lim [KR].
Full text: Click here
Patent 2024
1-(decanoylthio)-2-decanoyl-3-phosphatidylcholine 2,2'-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride Amides Cold Temperature Diamines Fever GPA 7 Imides Light LMO1 protein, human Medical Devices Metals Nylons Polymers Radius Sodium Chloride Vision

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More about "Metals"

Metals are a fascinating class of elements that play a crucial role in countless industries, from construction and transportation to electronics and medicine.
These versatile materials are characterized by their high electrical and thermal conductivity, malleability, and lustrous appearance.
Researchers in the field of metallurgy delve into the chemical, physical, and biological properties of metals, exploring topics such as metal alloys, corrosion, and the environmental impact of metal production and usage.
One key aspect of metal research is the extraction and purification of these elements.
Techniques like ion exchange, using products like TALON metal affinity resin, and treatments with chemicals such as sodium hydroxide, hydrochloric acid, and nitric acid, are often employed to refine and concentrate metal samples.
Analytical tools like the S-4800 scanning electron microscope and the D8 Advance X-ray diffractometer provide valuable insights into the structure and composition of metals.
Beyond extraction and analysis, metal research also encompasses the study of metal compounds and derivatives, including the use of solvents like ethanol, DMSO, and methanol.
Researchers may also investigate the reactivity and stability of metals, as well as the impact of additives like oleic acid on metal properties.
By leveraging the power of AI-driven platforms like PubCompare.ai, metal researchers can optimize their protocols, ensuring reproducibility and accuracy.
The platform's intelligent comparisons of methodologies from literature, preprints, and patents help identify the most effective and reliable approaches, streamlining the research process and leading to more efficient and reliable metal-related studies.
OtherTerms: Metallurgy, metal alloys, metal extraction, metal purification, metal analysis, metal compounds, metal reactivity, metal research protocols, PubCompare.ai, TALON resin, sodium hydroxide, hydrochloric acid, S-4800, ethanol, DMSO, methanol, nitric acid, D8 Advance, oleic acid.