Electrochemistry

23 Mar 2016

Nanomaterials Chemistry

Submitted by Anne Bentley, Lewis & Clark College

This list includes a number of LOs to help in teaching nanomaterials subjects; however, it is not exhaustive.

Updated June 2018.

Prerequisites: 
Corequisites: 
6 Jul 2015

Kinesthetic Learning: Cyclic Voltammetry Mechanisms

Submitted by Chip Nataro, Lafayette College
Evaluation Methods: 

I have only used this at the workshop. I do not anticipate teaching this material in class, so I doubt I will get any evaluation data. Perhaps the participants will comment on the effectiveness of this LO.

Description: 

This activity was created as part of a primer on cyclic voltammetry for the 2015 TUES workshop. The activity is designed to have one person represent the potential and several other people represent the molecules in solution. By simply scanning (walking through the line of people) and shaking hands, several simple mechanisms can be illustrated. The use of a joy buzzer with the first hand shake is highly encouraged, but not at all necessary. It adds a bit of levity to a serious topic and the author highly encourages using the joy buzzer on a "volunteer" that promised muffins years ago and has yet to deliver on said promise.

Learning Goals: 
  • A student will visualize simple cyclic voltammetry mechanisms with a kinesthetic experience.
  • A student will explain possible outcomes for single molecules upon oxidation or reduction. 

 

Prerequisites: 
Course Level: 
Corequisites: 
Equipment needs: 

Students

A joy buzzer (picture included in case you are unfamiliar with this object) is optional, but certainly fun.

Subdiscipline: 
Related activities: 
Implementation Notes: 

The idea behind this LO is for students to be able to visualize some of the possible outcomes of a species upon oxidation or reduction. It requires the instructor to select several students (4-6) to participate. The instructor and the students huddle before each demonstration so the students know how to behave. The slides that accompany this LO are used to show what the actual CVs look like after performing the visualization with student volunteers. The following instructions are also summarized in the notes on the slides.

In the case of a reversible system, the instructor (potential) walks past a line of students shaking their hands. The students turn 180 degrees upon shaking hands. When the instructor reaches the end of the line, they turn around and repeat the process in the opposite direction. In an irreversible system, after shaking hands, the students can do any number of thing to represent a chemical reaction taking place, the products of which are electrochemically silent. This could be putting their hands behind their backs, linking hands with another student, or anything else. Upon sweeping back through the line, the instructor discovers no hands to shake. In the third example, the instructor goes through the line very slowly the first time. This gives some of the students time to do something (grasp each other's hands for example) after having getting a hand shake. Not all of the students should undergo this reaction, so some of the students are available to shake hands upon reversing the scan. The second time, the instructor should sweep through fairly quickly so that the students don't have time to form another product. I encouraged my participants to make dramatic movements when I did the slow scan. In the final mechanism, upon shaking hands students were instructed to turn around and lift their hands up for a high five. This showed that an electroactive species was present, but it was somehow different from the starting material.

The joy buzzer is completely optional, but it was great fun. The person I did it to was not at all expecting it. It is electrochemistry after all, there should be a little shock.

Time Required: 
5-10 minutes
2 Jul 2015

Interpreting XPS and CV data from an Electrocatalysis Publication

Submitted by Karen McFarlane Holman, Willamette University
Evaluation Methods: 

Student completion of learning objectives will be assessed through the provided handout that would be turned in after discussions as well as student participation in discussion.  Alternatively, the questions could be used in a problem set or exam question, in which case the answers would be graded.

Evaluation Results: 

This LO was developed at the VIPER workshop on Heterogeneous Catalysis in 2015 and has not been tested.

Description: 

This is a learning object focused on analyzing a specific figure from a research article that show XPS and CV data on Ni(OH)2/NiOOH thin films that have incorporated Fe. The paper is one for which we created a “bigger picture” Literature Discussion LO during the 2015 VIPEr TUES workshop at UW, based on  Shannon Boettcher’s group’s “Nickel-Iron Oxyhydroxide Oxygen-Evolution Electrocatalysts: The Role of Intentional and Incidental Iron Incorporation”.  This LO could be used in conjunction with our more general Lit Discussion LO on the scientific method, or could be used as follow-up exercise as either a set of homework questions or exam questions.

Corequisites: 
Course Level: 
Prerequisites: 
Learning Goals: 

Working through these problems, a student will gain experience...

  • interpreting XPS spectra and identifying control experiments.

  • interpreting cyclic voltammograms.

  • tying together results from these two different types of experiments to gain insight into sample composition.
Implementation Notes: 

We envision at least three possible ways to implement this LO:  (1) students are provided with the student handout and the paper to complete before a class discussion; (2) students are given the handout after a class discussion on the related scientific method LO; or (3) these questions (or a subset thereof) are asked in an exam after the article has been read and discussed in class.

Time Required: 
15-30 minutes if used in class, highly dependent on students' previous knowledge of XPS and CV.
2 Jul 2015
Evaluation Methods: 

Students can hand in tthe first set of questions as homework which may be evaluated.  Class participation and group work may also be graded appropriately.

Evaluation Results: 

This is an untested LO.

Description: 

This learning object is based on discussion of the literature, but it follows a paper through the peer review process.  Students first read the original submitted draft of a paper to ChemComm that looks at photochemical reduction of methyl viologen using CdSe quantum dots.  There are several important themes relating to solar energy storage and the techniques discussed, UV/vis, SEM, TEM, electrochemistry, and catalysis, can be used for students in inorganic chemistry.

Unlike a typical literature LO where students discuss only the current science, this LO contains the actual reviewer comments to the original submitted manuscript as well as a link to the final version that was published in Journal of Materials Chemistry A.

DOI: 10.1039/C5TA03910J

Prerequisites: 
Learning Goals: 

Students will be able to...

·  Communicate the main ideas of a scientific research paper to classmates.

·  Identify the research area, importance of the research, and background information provided in a scientific paper.

·  Discuss areas of a paper that may be improved through revision.

·  Compare their views of necessary revisions with actual anonymous reviewers on a scientific paper and the eventual publication.

·  Understand the importance and shortcomings of the peer review process using an actual publication from the literature.

Implementation Notes: 

The LO has multiple sections which may be discarded or edited depending on the particular learning goals desired.  While the chemistry may be difficult for lower level students, the discussion of the peer review process may be valuable to students across multiple levels and even in writing courses.  Also provided are the authors' actual responses to the reviewers comments.  It should also be noted that the original article was submitted to ChemComm, but the subsequent revised article was submitted and accepted to Journal of Materials Chemistry A.

Time Required: 
Homework Assignment + 1 h in class
2 Jul 2015
Evaluation Methods: 

The assignment can be graded at the conclusion of the class period and then revisited at points later on an exam or at the final.  

Description: 

This question set has students examine the kinetics of the electrocatalytic reduction of CO2 to CO described in Sampson, D.L.; Nguygen, D., Grice, K.A.; Moore, C.E.; Rheingold, A.L.; Kubiak, C.P. Manganese Catalysts with Bulky Bipyridine Ligands for the Electrocatalytic Reduction of Carbon Dioxide:  Eliminating Dimerization and Altering Catalysis.  J. Am. Chem. Soc. 2014, 136, 5460-5471. 

Learning Goals: 

Students will be able to...

  • Identify the experimental conditions required for the pseudo-first-order kinetics assumption to be valid.
  • Compare and contrast electrochemical and chemical kinetics.
  • Apply given experimental data to deduce the reaction order with respect to all reactants in the electrocatalytic reduction of CO2.
  • Calculate the rate constant (kcat) for a given set of conditions.
Corequisites: 
Equipment needs: 

Students should have access to a computer with Microsoft Excel.  

 

 

Implementation Notes: 

This can be adapted to a general chemistry/introductory class or can be used as in-class discussion with upper level students.  Secondarily this can be given as a homework asssignment and then used in class as a discussion or as an in-class acctivity.  

 

 

Time Required: 
one 50 minute class
2 Jul 2015
Description: 

Upper division literature discussion of a JACS paper on electrocatalysis.  This activity serves as an introductory look at the paper as a homework assignment to prepare the student for a more in depth class discussion.

Course Level: 
Corequisites: 
Learning Goals: 

Learning Objectives

  1. Identify the structure of a research article
  2. Summarize the motivation and major goals of a study.
  3. Recognize the central reaction and catalyst of a paper.
  4. Analyze a catalytic cycle.
  5. Explain how particular conclusions were determined based on experimental data.
  6. Recognize applications of the techniques presented in the paper.
Time Required: 
50 minutes
2 Jul 2015
Evaluation Methods: 

Options for assessment include:

  • Students can complete the questions and submit their responses which are then evaluated for clear understanding of the concepts (For example: Is the student able to describe clearly the purpose behind the paper?)
  • Students can be evaluated for the quality of their contributions to in-class discussion (Is it evident that the student read the paper?)
  • Students can be asked follow up questions on a later exam (Can the student recall the basic principles discussed in the activity?)
Evaluation Results: 

We have no results at this time for this newly created activity.  If you use this object in Fall 2015, please post comments to this LO so we can include yours results!

Description: 

This literature discussion is meant to give students an understanding of both the key concept-driven and more “meta” information of a literature paper.  Students will use Jillian Dempsey’s paper, “Electrochemical hydrogenation of a homogeneous nickel complex to form a surface-adsorbed hydrogen-evolving species,” to investigate paper authorship, how the scientific method is used in research, and how to understand the important findings of a research article.

 

Reference: Chem. Commun., 2015, 51, 5290-5293

DOI:10.1039/C4CC08662G

 

For a general chemistry course, questions 1-4, 7, and 10 could be utilized to expose students to the format of literature articles without diving too deeply into content.

 

For an advanced inorganic course, all questions could be used to include some introductory content to the discussion.

 

This learning object was developed at the 2015 NSF sponsored cCWCS VIPEr workshop at University of Washington where we were fortunate to hear Prof. Jillian Dempsey present this research. It is worth mentioning that the first author of this paper was an undergraduate student at UNC-CH. The Dempsey’s research lab focuses on developing new technology to support a solar energy economy through catalysis.

Corequisites: 
Prerequisites: 
Learning Goals: 

After completing this activity, the student will be able to:

  • access different parts of a paper and its supplementary information for different levels of understanding.
  • use information in a paper to determine the intent behind published research and how it fits into a larger purpose.
  • see that chemical research builds on earlier work and is an iterative process in which direction can change based on new information.
  • understand the difference between homogenous and heterogeneous catalysis
  • identify and define inorganic chemistry related terms
Implementation Notes: 

The first author of this publication, Daniel J. Martin is an undergraduate student!  It may be worth mentioning this fact to the students and to help them understand that in the academic world publications are the “currency” needed for career advancement.  We envision that the students will receive a copy of the article as well as the student handout containing the discussion questions several days prior to the discussion.  The faculty member may also choose to omit one or more questions from the student handout and only ask them during the discussion period.

Time Required: 
0.5-1.5 hours
2 Jul 2015
Evaluation Methods: 
Options for assessment include: 
  • Students can complete the questions and submit their responses, which are then evaluated for clear understanding of the concepts. (Is the student able to describe clearly the chemistry in the paper?) 
  • Students can be evaluated for the quality of their contributions to in-class discussion. (Is it evident that the student has read the paper?)
  • Students can be asked follow up questions on a later exam. (Can the student recall and apply the principles discussed in the activity to a similar problem?) 
Evaluation Results: 

We have no results at this time for this newly created activity.  If you use this object in Fall 2015, please post comments to this LO so we can include your results!

Description: 
The paper entitled “Electrochemical hydrogenation of a homogeneous nickel complex to form a surface adsorbed hydrogen-evolving species” explores the discovery, characterization and catalytic activity of a film that deposited on the electrode while studying a nickel complex under electrocatalytic conditions.
 
This literature discussion includes several sets of questions that address different aspects of the paper, as described in the implementation notes. Discussion questions cover the structure and electron configuration of the compounds used to form catalysts, their synthesis and reactivity, the formation and activity of the catalytic film, electrocatalysis using cyclic voltammetry, and the characterization of the catalytic film.  The list of questions is extensive, but we encourage you to review them and select the ones that will best fit the goals of your lesson. 
 
This learning object was developed at the 2015 NSF sponsored cCWCS VIPEr workshop at University of Washington where we were fortunate to hear Prof. Jillian Dempsey present this research. It is worth mentioning that the first author of this paper was an undergraduate student at UNC-CH. The Dempsey’s research lab focuses on developing new technology to support a solar energy economy through catalysis. 
 
Reference: Chem. Commun., 201551, 5290-5293 DOI: 10.1039/c4cc08662g
 
Several questions of the discussion focus on data found in the supporting information. 
Corequisites: 
Learning Goals: 
By completing this activity, the student will be able to:
  • Identify the difference between facial and meridional geometries.
  • Apply 18 electron counting rules to a transition metal complex.
  • Apply electrochemical concepts to describe qualitative features of a cyclic voltammogram trace.
  • Apply knowledge of redox chemistry to understand electrocatalysis.
  • Demonstrate an understanding of reduction and oxidation reactions as they relate to transition metal complexes.
  • Use retrosynthetic analysis to determine which starting materials are needed for a Schiff base product.
  • Understand what a hydrogenation reaction is and show what happens to a double bond when it is hydrogenated.
  • Understand the use of SEM (Scanning Electron Microscopy) and TEM (Transmission Electron Microscopy) images to characterize a film. 
  • Understand the use of XPS (X-ray Photoelectron Spectroscopy) and EDS (Electron Dispersion Spectroscopy) to elucidate the elemental composition of a film.
Implementation Notes: 
It may help to split this activity and assign portions to groups of students. Or it may be better to spread the questions out over several weeks of the course, as relevant topics present themselves in the course content. For reference, the questions are split into groups below. You may also choose to eliminate certain groups of questions if they do not align with the covered content of your course. Also, a suggested exam question is included separately.
 
Questions 1-3. The structure and electronic configuration of two octahedral nickel(II) complexes. Includes basic concepts on coordination chemistry like isomerism, coordination geometry, oxidation state, and the 18 electron rule.
 
Questions 4-9. Synthesis and reactions of the organic ligands coordinated to nickel. Includes imine chemistry and the concepts of hydrogenation, hybridization, and aromaticity.
 
Questions 10-15. Electrochemical deposition of a film and its catalytic activity to produce hydrogen. Electrocatalysis and hydrogen evolution. Includes topics of cyclic voltammetry, overpotential, reversible and irreversible reductions. 
 
Questions 16-17. Discussion of methods used in the paper: CV, imaging (SEM and TEM) and spectroscopic techniques (XPS and EDS) and how XPS was used to characterize the film . Question 16 is particularly amenable to division among groups of students.
 
Suggestions for exam questions (faculty handout only). The provided exam question would be used to assess students after they have completed the in-class discussion. If very specific details about the mechanism behind the voltammetric response are desired then students may benefit from access to a clean version of the paper during the exam, 
 
This activity has not yet been tested. If the in-class discussion is to fit within 50 minutes, then several questions need to be left out of the discussion, though the students still need to do them to prepare for the discussion. Also, closely related questions can be addressed together. For example, questions 1, 2, and 6 are primarily intended to review concepts that the students need to answer questions 3, 4-5,  and 7-8. Question 9 deals with organic retrosynthetic analysis and is not essential for the questions that follow. Questions 10-13 deal with the heart of the paper, and questions 14-17 deal with controls and characterization of the system. The instructor's priorities should determine whether only the most critical questions (such as 3-5, 7-8, 10-13, and perhaps 14 and 15) are each briefly discussed in one fifty class period, or if at least half of two class periods are used for a more extensive discussion.
 
 
The activity uses some figures from the paper itself. The paper was published under a Creative Commons Attribution-NonCommercial 3.0 Unported (CC BY-NC 3.0) license as described below:
 
Time Required: 
Untested. A selection of key questions could be discussed in one 50 minute session (see implementation notes). Otherwise, the activity could take over 90 minutes.
29 Jun 2015

Copper Oxide Crystal Growth

Submitted by Ellen Steinmiller, University of Dallas
Evaluation Methods: 

Student answers to the reading comprehension questions were collected at the beginning of class and graded out of 10 points.  An additional 15 points was based on on class participation during the discussion and answers to the in class questions. 

Evaluation Results: 

Overall, students did well on this paper.  During the group problems, students struggled the most with Miller indexes and drawing the layer diagrams of the Cu atoms.  In the future I would incorporate ICE models in the class discussion so that students can more clearly see the different crystal planes.  Students are often quite confused as to why copper oxide is a primitive cubic cell and I think see the models would help with the visualization that not all Cu atoms are created equally.

Description: 

Students in a 2nd year inorganic class read an article describing the effect of additives on the final morphology of copper oxide. (Siegfried, M.J., and Choi, K-S, “Elucidating the Effect of Additives on the Growth and Stability of Cu2O Surfaces via Shape Transformation of Pre-Grown Crystals”J. Am. Chem. Soc., 2006, 128 (32), pp 10356–10357.  dx.doi.org/10.1021/ja063574y). The authors describe a systematic method that exploits the preferential adsorption phenomenon to regulate crystals shapes by observing the shape transformation of pre-grown crystals over time (e.g cubic to rhobooctahedral to octahdral and back).  The authors start with seed crystals of specific morphology and then immerse the pre-grown crystals in a second solutions with additives to direct the crystal growth.    This strategy allowed them to develop a general scheme to determine the relative order of surface energies and form new crystal shapes containing planes that cannot be directly stabilized by preferential adsorption alone.  

Prerequisites: 
Corequisites: 
Learning Goals: 

After reading and discussing this paper, students will be able to:

-          Differentiate between notations describing planes, directions, and families of planes

-          Describe atomic surface terminations of different crystal faces of the same unit cell

-          Describe the effect of common additives on synthesis of crystals

-          Determine d-spacings of planes from XRD data

-          Determine lattice parameters from XRD data 

Implementation Notes: 

I used this article in the Spring of 2014 in a class of 9 (1 freshmen, 1 sophomore, 5 juniors, 2 seniors) as our conclusion of our discussion of solid state chemistry.   Students had a background in electrochemistry, crystal structures and x-ray diffraction before reading this paper.  Students were required to submit the first set of questions when they came to class and then they worked on the second set of questions in small groups.  During the class discussion, we reviewed electrochemistry, in particular the reaction of electrodeposition of Cu2+ to Cu2O and revisited Pourbaix diagrams briefly to discuss stability of different metal oxide species.  We also discussed preferential adsorption and how this impacts crystal growth.  For a good paper on preferential absorption, see Matthew J. Siegfried and Kyoung-Shin Choi, “Electrochemical Crystallization of Cuprous Oxide with Systematic Shape Evolution,” Adv. Mater. 2004, 16, 1743-1746. (dx.doi.org/ 10.1002/adma.200400177). Schematic 1 is particularly helpful and I used it to develop the concept preferential adsorption and the relative enrgies of planes. 

Time Required: 
50 minutes
12 Jun 2015

Materials Project

Submitted by Barbara Reisner, James Madison University
Description: 

The Materials Project is part of the Materials Genome Initiative that uses high-througput computing to uncover the properties of inorganic materials.

It's possible to search for materials and their properties

It employs high-throughput computation approaches and IT to create a system that can be used to predict properties and construct phase diagrams andPourbaix diagrams.

Prerequisites: 
Corequisites: 

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