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Solid-State Chemistry

Solid-State Chemistry

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Solid-State Chemistry

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  1. Solid-State Chemistry Group U2: Kyle Demel Keaton Hamm Bryan Holekamp Rachael Houk

  2. Overview • Background • Introduction • 3 Articles • Conclusions • Questions

  3. What is Solid-State Chemistry? • Synthesis • Structure • Physical properties • Composition • Atomic arrangement

  4. Examples of Solid State Devices • LED’s • LCD • Transistors • Microprocessor chips

  5. The Holy Grail of Solid-State • The Solid-State Hard Drive • No moving parts • No read/write head • Very fast

  6. Synthesis – Article 1 Floral-like microarchitectures of cobalt iron cyclotetraphosphate obtained by solid state synthesis BanjongBoochonm and NaratipVittayakorn Floral-like microarchitectures of cobalt iron cyclotetraphosphate obtained by solid state synthesis

  7. Potential Applications (Article 1)

  8. Background Information (Article 1) • Transition metal cyclotetraphosphates (CTP) include a P4O12-4 anion and a combination of: • Mn, Ca, Zn, Fe, Ni, Cu, Co • Potentially beneficial properties: • Chemical • Optical • Catalytic • Magnetic

  9. Procedure for Synthesis (Article 1) • Grind 1:1 mol ratio of CoCO3 and Fe • Add H3PO4 solution • Heat at 500°C for 2 hr • Crush product and wash with water until no phosphate leaving • Rinse with MeOH and dry

  10. Product Analysis (Article 1) • Atomic Absorption Spectrophotometry for Co and Fe content • Colorimetric analysis of molybdophosphate complex for P content • X-ray powder diffraction shows homogeneous solid solution, not mixture of 2 single metal CTPs • XRD also gave crystal type and size Floral-like microarchitectures of cobalt iron cyclotetraphosphate obtained by solid state synthesis

  11. Properties of Product (Article 1) • Monoclinic crystal structure • Average crystallite size of 49±20 nm • Uniform particles in floral-like morphology • More superparamagnetic than other morphoplogy Floral-like microarchitectures of cobalt iron cyclotetraphosphate obtained by solid state synthesis

  12. Superparamagnetism(Article 1) Floral-like microarchitectures of cobalt iron cyclotetraphosphate obtained by solid state synthesis; Fundamentals of Materials Science and Engineering: An Integrated Approach

  13. SEM Images of CoFeP4O12(Article 1) B A • A= single-step method • B=acetone 2-step method Floral-like microarchitectures of cobalt iron cyclotetraphosphate obtained by solid state synthesis; A simple route to synthesize new binary cobalt iron cyclotetraphosphate CoFeP4O12 using aqueous and acetone media;

  14. Further Research (Article 1) • Testing with other metals • Application for the new materials, based on desired properties • Other better synthesis methods • Confirm safe for use ? ? ? ?

  15. Article 2 – Structure Kirkendall-effect-based growth of dendrite-shaped CuO hollow micro/nanostructures for lithium-ion battery anodes YingyingHu, Xintang Huang, Kai Wang, Jinping Liu, Jian Jiang, Ruimin Ding, XiaoxuJi, Xin Li

  16. KirkendallEffect (Article 2) • Discovered by Ernest Kirkendoll, 1947 • Proposed that molecular diffusion within solids took place not only by direct exchange or ring mechanism, but also by vacancy exchange. • Rejected at first by his colleagues causing Kirkendall to leave academia Direct exchange Ring Mechanism Vacancy Exchange <>

  17. Experiment Procedure (Article 2) • 1.02 g of CuCl2 dihydrate is dissolved in 200 mL distilled water and stirred with 2 mL of acetic acid. Al foil is placed in reaction beaker for 4 h. • Precursors form on surface of foil that are filtered and vacuum- dried. • Heat is applied at varying Temperature and time duration to induce Kirkendall effect and form hollow dendrites. <>> <>

  18. Experimental Procedure(Article 2) As the samples are heated, exterior Cu particles come into contact with atmospheric oxygen and oxidize into CuO. Remaining interior Cu particles diffuse outward as voids form and merge, hollowing out the structure. Overexposure to heat can cause the hollow to crystallize. Fig. 3. TEM images of the products prepared at 350°C for 5 min (a),15 min (b), and 40 min (c). Fig. 4. Schematic illustration of the growth of typical dendrite-shaped CuO hollow architectures.

  19. Sample Analysis (Article 2) This method produces dendrite shaped CuO structures composed of hollow tubes with a film interior and CuO cube exterior. Precursor dendrites are ~3-10μm long and branch thicknesses range from 160-170 nm. They are composed of FCC Cu metals. Product branch diameter is ~400 nm, and the thickness is ~350 nm Fig. 2. FESEM images of Cu dendrites at (a) low magnification and (b) high magnification and typical CuO hollow structures at (c) low magnification and (d,e) high magnification.

  20. Results (Article 2) The CuO hollow structures as anode materials for lithium-ion batteries exhibit a high initial discharge capacity of 1503.9mAh/g with the average Coulombic efficiency of 97.0% for the next 50 cycles over the potential range 0.02–3.0 V at a current rate of 0.5C at room temperature.

  21. Technological Implications (Article 2) The small primary particles that compose dendrite-shaped CuO and large space in the hollow structure are expected to improve the performance of the Li-ion cells. This Kirkendall-effect-based approach is proven to be an effective method to prepare excellent hollow electrode materials for Li-ion batteries.

  22. Article 3 – Physical Properties Indentation induced solid state ordering of electrospun polyethylene oxide fibres Wei Wang, Ton Peijs, and Asa H Barber

  23. Introduction (Article 3) • Electrospinning can manufacture thin polymer fibers • Fiber diameters range between 100 nm and 10 µm • Fibers have improved mechanical properties over bulk isotropic polymer • Improved mechanical performance due to polymer chain alignment • Sufficient heating degrades mechanical properties • Solid-state deformation processing improves mechanical properties • Stresses induce structural orientation of polymer chains • Can restore properties in polymers that were heated

  24. Experimental Procedure (Article 3) • Polyethylene oxide is a semi-crystalline polymer soluble in water • Fibers were created using electrospinning • Fiber diameter was 500 ± 30 nm • Fiber Tm was 64°C • Isotropic PEO Tm is 69°C • Explanations for Tm difference: • Fibers had a large surface area to volume ratio • Less polymer crystals in electrospun fibres

  25. Experimental Procedure (Article 3) • Thermo-mechanical testing was performed using an atomic force microscope integrated with a heating chamber • Measured the force required to indent the polymer surface • Took data before and after heating polymer to 50ºC • AFM applied large indentations at heated temperature • Took data around and away from indentations

  26. Results and Discussion (Article 3) • Similar forces were applied throughout the experiment • Force vs. indentation depth curve was generated • (a) before any heating • (b) after heating, near indentation stress points • (c) after heating, away from indentation stress points

  27. Results and Discussion (Article 3) • The indentation depth (δ) and force (F(δ))are used to calculate the elastic modulus (Ef) of the electrospun fiber • The values for the elastic modulus show the effects of heating and indentation on the mechanical properties of the polymer

  28. Experiment Conclusions (Article 3) • Electrospinning improves the mechanical properties of polymers • Bulk PEO has an elastic modulus of 0.20 GPa • Electrospun PEO has an elastic modulus of 1.39 GPa • Indentation helps retain mech. properties in post- heated polymers • Around an applied stress, the elastic modulus was 0.53 GPa • Away from an applied stress, the elastic modulus was 0.22 GPa • Changes in mechanical properties are based on solid-state rearrangements at the nano-scale level

  29. Research Implications (Article 3) • Heating may limit the function of electrospun fibers • The mechanical properties of heat-treated electrospun polymers approaches the properties of normal bulk polymers • Further research could yield better property retention in nano-fabrics • Stronger and more applicable textiles • More heat-resistant fibers

  30. Further Research (Article 3) • Which electrospun fibers are susceptible to heat-induced strength degradation other than polyethylene oxide? • How are the mechanical properties of the polymer affected by multiple heating or stress cycles? • How can the electrospun fibers be stress-induced at the macroscopic level? • What are the safety considerations involved? • How much will stress treating cost?

  31. Conclusions Three Aspects of Solid State Chemistry: • Synthesis • Creating cobalt iron cyclotetraphosphate microstructures • Structure • Testing new CuO hollow nanostructures for battery anodes • Physical Properties • Improving the durability of electrospun fibers

  32. Questions

  33. Rebuttal Group from U2

  34. Rebuttal from Group U2: Solid-State Chemistry Group U2: -Kyle Demel -Keaton Hamm -Bryan Holekamp -Rachael Houk

  35. We disagree with the following comments: • Repeat Information – One of the critiques stated that we used the same articles as a previous group. The student who wrote this false accusation is either completely clueless or did not check the website to verify that all of our articles are unique and not repeats. We believe this student was referring to the third article that concerned using solid-state chemistry to analyze physical properties. The article discussed using solid-state techniques at the nanoscale level to investigate how the physical properties of electrospun fibers are affected by heat and stress. Our presentation builds off of the introductory material to electrospun fibers that Group U6 presented. Apparently, we did not make this distinction clear enough. • Understanding = Bad – Another student praised us for making a presentation that was easy to understand and follow. That student then decided to dock us points in the respective category with no further rationale to follow. Either the student thinks we’re playing golf (where a low score is good) or was carping over the fact that the presentation did not allow him/her to feel perplexed, confused, flummoxed, or bruised. While a normal human being would have followed up the comment with a good score, this classmate of ours is apparently a disappointed mental masochist.

  36. We agree with the assessments concerning: • Introduction – Many of the critiques mentioned the introduction being insufficient to cover the topic presented. While the group still stands by the statement that a comprehensive discussion of solid-state chemistry would be time-consuming and unnecessary for this class, we agree that the introduction should have included more detail. Initially, the group believed that focusing on the overall topics covered by solid-state chemistry would steal too much time from elaborating on specific applications. After reviewing the critiques, the group now concurs that more time should have been allotted to the introduction. • Slide Lay-out – We were pleased that most of the audience members commented on the great slide lay-out. The group put in the effort to make all the text, headings, and formatting consistent throughout the presentation. The included figures were all large and clear enough for easy interpretation. The figures were also pertinent to the presentation as a whole, and nearly every slide had at least one visual. Equations were manually typed to ensure legibility.

  37. Definition: Study of synthesis, structure and physical properties of the solid materials Characterization: Optical property Mechanical property Electrical property Catalytic property Review: U1 Solid State Chemistry by U2

  38. Important of Solid State Chemistry Very helpful in preparing the material with unique electrical, magnetic, optical and catalytic properties Current Research numerous scientific areas including Materials Science and Engineering, Ceramics, Chemistry, Chemical Engineering, Mineralogy/Geology, and Condensed Matter Physics Further Research Enhancing the properties of materials like polymers to increase their susceptibility to multiple heating and stress New method of developing and testing these solid state chemicals What we learn?

  39. Group #3 Phillip Keller Krista Melish Micheal Jones James Kancewick Review of Group#2Solid State Chemistry

  40. Review • Slides • Nice pictures, not all were explained but gave the report a good picture to text ratio • The pictures and laser pointer use was done well, for the most part one presenter did wave it at the screen which was distracting • Tech Review

  41. Tech Content • Potential applications “was rushed” for the corrosion resistant coatings • The beginning of the presentation started with good solid examples relating macroscopic examples to microscopic instances. • The battery paper and nanofiber paper also were covered in sufficient detail. This lead to even a lack of question for the nanofiber article.

  42. Solid-State Chemistry Review of Group U2 by Group U4

  43. Oral Presentation and Slides • The slides were very simple and easy on the eyes. There was not an overabundance of text on each slide, and that really helped to keep the audience focused on the presenters’ speech as opposed to simply reading the slides the whole time. • Excellent pictures especially in the dendrite formation slides. • Excellent slides overall with a good balance of text/images and large enough text/images to easily read. • Presenters spoke clearly and loudly through the presentation, and were all involved in the Q&A session at the end. • A little too much reading off slides at portions of the presentation. • Thank you for citing all pictures on every page. Credit should be given where it is due. • Thank you group for the food!

  44. Good introduction overall involving types of solid-state devices and uses; however, it was a little dry in the explanation of what solid-state chemistry is. • Even though each of the papers dealt with the synthesis, structure, and properties of solid-state chemistry devices, we would have like to see a little more depth to those in the introduction. • First article gave a good review of the synthesis of a certain solid-state chemistry application, but we would have liked to see more stress on the importance of superparamagnetism since that is the ultimately desired property of the chosen material. • We really enjoyed the 2nd paper. It was presented very clearly and gave us insight to the future of long-life batteries, and the upgrades that are currently being researched to make them last longer and charge more quickly. • Very educational end to this exciting presentation! With this paper the audience finally learns the reason why research and money should be poured into this field. Would have liked to see elaboration on the heat effects of nanospun fibers. • Overall, an excellent presentation with each group member offering an interesting view of the concept of solid-state chemisty applications and properties. Technical Critique

  45. Solid-state chemistry • Review of Team U2 by Team U5 – Jaynesh Shah, Greg Pudewell, Edwin L. Youmsi Pete and John Pack.

  46. Oral and Quality of Slides Review • The speakers did a great job of speaking in a paced, clear manner. • They were confident and knowledgeable on the subject. • There were a few times when filler words were a bit distracting. • Good use of the microphone.

  47. Technical Review • The presentation was technically sound • Spent too much time on the introduction • Introduction was too elementary for the level of student in that class • Researched three different papers • Outstanding!

  48. Solid State Chemistry Presented by: Group U2 Critiqued by: Group U6

  49. Critique: Oral Presentation & Slides • Slides were easy to read • Good background and good size text • Good transition between slides • Slides kept our attention • Very professional looking – good effort put in preparing the presentation • The use of illustrations complimented the text – would have liked to see more use of graphs though to show results of experiments • The illustrations were cited and found on every page – they were relevant to the topic and helped illustrate points • The outline slide in the beginning as well as the conclusion slide at the end of the presentation were very helpful • Excellent flow of topics in the introduction • The speakers did a good job in presenting. There were a few times when too many filler words were used to not enough eye contact was made. One speaker could have practiced a little bit more to make their speech flow better. • Liked that group members dressed up for presentation – looks professional

  50. Critique – Technical Content • Introduction explained really well – very easy to follow • Presenters took audience through a good overview before going in depth into the research papers • Choice of research papers seemed relevant to topic discussed • Three papers discussed which gave a good range of information on current research • The motivation for each paper given at the beginning – something we really liked • The paper on the lithium battery was the most interesting • Potential applications in cell phones and laptops • The paper which discussed the effects of electrospinning showed the additional strength polymers gained through the process • Potential applications include improvements in synthetic fabrics • Further research on this topic was very well described • The presenters went in depth of the topics covered by each of the research papers • Would have liked to see potential long term impact of the research presented