In-situ Imaging electrochemistry reaction with atomic force microscope and 3D desktop manufacturing in developing electrochemistry cells Song Xu, Ph.D. Sr. Application Scientist Agilent Technologies
Why this topic? It is about innovation EC AFM experiments always requires instrument modification This presentation will cover a missing part of education in biology, chemistry and material science: bench top manufacturing This talk is edited for students, and It is NOT about 3D printing! Agilent General Audience 2
The Original Question of all: Why
Lithium Battery
SEM Observation of Solid-Electrolyte Interphase: the ex-situ Elsevier, Comparative study of the solid electrolyte interphase on graphite in full Li-ion battery cells using X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and electron microscopy Jung Tae Lee a, Naoki Nitta a, James Benson a, Alexandre Magasinski a, Thomas F. Fuller b, Gleb Yushin a,*
AFM / STM In Liquid Imaging is used to observe the formation of SEI: the in-situ and in real time
EC Bulk Cu Crystal Deposition
The in-situ experiment, we need to: Combining AFM/STM with the potentialstate to form EC-AFM/STM Reference electrode Electrolyte
But there are tons of problems Atmosphere protection of Lithium Handling of electrodes and set up EC cells Noise isolation Customizable in Footer 9
Problem: operating instrument inside glove box
Problem: handling electrodes working electrode (in contact with Au) reference electrode (no connection with other electrodes) counter electrode (no connection with other electrodes) Problems Small parts Leak evaporation Corrosion
Problem: Small parts of Electrical Chemistry Cell Reference electrode: Mostly Ag, Cu ok for Cu deposition experiment Electrodes Counter electrode: Mostly Pt, Cu ok for Cu deposition experiment. The long loop is for the large current in the big AFM cell. STM counter electrode doesn t need the loop.
The problems: corrosion and small nuts
The problems: sample size and shape
The problems: being a chemist some time is helpless Scientist need to learn engineering Customizable in Footer 15
Desktop manufacture and its application in scientific research: its not 3D printing
The trend of civilization is toward the spread of knowledge and technology, which empower individual toward equality Road, highway, aircraft, high speed railway (transportation) Language, literature, printing, phone, computer, internet (information) Workshop, factory,?? (manufacture)
Last revolutions: desktop publishing
For the past 100 years, mass production industry had little change: standardization, scale and efficiency
And the low cost CNC machines $3000 CNC Mill $1000 CNC laser $700 CNC Mill
Desk top manufacture is the an ongoing revolution a product became a piece of information Want to send me a Christmas gift : email to me
3D printing : precision adding of material melting add glue to powder Photo sensitive polymer laser melting
The limitation of 3D printing: lack of control of material property
Problems and inperfections of 3D printing
Other affordable desktop production tools
CNC laser cutting
CNC laser cutting and its advantage
CNC laser cutting and its advantage: pure 2D design easy to learn
The basics to learn desktop manufacturing: start with CAD Group/Presentation Title Agilent Restricted
What is CAM? (computer aided manufacture) CAM turn a designed shape into a machine tool path code (G code) Traditionally this is taught in trade schools to blue color workers
Easy to learn and sometimes free trial amateur CAM
CAM turns a designed shape into reality Step 2: define the depth of each cutting
CAM turns a designed shape into reality Step 3: machine code tool paths generation by computer
CAM turns a designed shape into reality Step 4: actual cutting of a 2.5D part
Back to Chemistry
Solution to the problems of AFM inside a professional glove box: EC cell made for easy to handle
Solution to the problems of AFM inside a professional glove box: EC cell made for easy to handle
In-situ observation of SEI on HOPG electrode surface during charging circle of a Li ion battery cell the first circle
In-situ observation of SEI on HOPG electrode surface during charging circle of a Li ion battery cell the first circle AFM images of HOPG surface scanned at a synchronous discharge voltage range of a) 3.0 e 2.95 V; b) b) 1.7 e 1.65 V; c) c) 1.0 e 0.95 V; d) d) 0.5 e 0.45 V; e) e) 0.1 e 0.05 V. Scan area 25 mm2.
In-situ observation of bottom SEI on HOPG electrode surface during charging circle of a Li ion battery cell the first circle AFM images of bottom SEI layer: a) pristine HOPG; b) b) discharge to 1.7 V; c) c) discharge to 0.5 V; d) d) discharge to 0.02 V. Scan area 25 mm2.
In-situ observation of SEI on HOPG electrode surface during charging circle of a Li ion battery cell the first circle Schematic of SEI evolutions during the first discharge process. a) The solvent decomposition product (purple dots) deposits at the surface of the graphite; b) the solvated lithium ions (gray dots) pass through the particle layer and intercalated into the graphite layer (black lines); c) solvent decomposition products accumulate at the surface when the lithium intercalation takes places; d) the displacement of the graphite layer caused by the lithium intercalation pushes the top particle layer off the HOPG surface;
In-situ observation of SEI on HOPG electrode surface during charging circle of a Li ion battery cell the delamination of the first SEI layer
In-situ observation of SEI on HOPG electrode surface during charging circle of a Li ion battery cell- the bottom SEI
In-situ observation of SEI on HOPG electrode surface during charging circle of a Li ion battery cell- the bottom SEI is a soft layer Center framed area scanned at higher force (10nN)
On going electrochemistry cell development
Future work: EC AFM cell for Litihium Cell with heating and cooling option
Future work: EC AFM cell for Litihium Cell with oxygen feed to a porous sample electrode
Example of dish type EC liquid cell
EC liquid cell for coin single crystals Customizable in Footer 49
EC liquid cell for gold bead single crystal Customizable in Footer 50
My basement factory (total cost $3000)
Please visit: www.afmuniversity.org email: song_xu@keysight.com
A few words about Keysight Techology AFM: Keysight AFM has the space for innovation due to its tip scan design.