in-situ imaging electrochemistry reaction with atomic … · · 2017-06-09in-situ imaging...
TRANSCRIPT
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Song Xu, Ph.D.
Sr. Application Scientist
Agilent Technologies
In-situ Imaging electrochemistry reaction with atomic
force microscope and 3D desktop manufacturing in
developing electrochemistry cells
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Why this topic?
Agilent General
Audience
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2
• 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 about 3D printing
!NOT
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The Original Question of all: Why
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Lithium Battery
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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,*
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AFM / STM In Liquid Imaging is used to observe the formation of SEI:
the in-situ and in real time
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EC Bulk Cu Crystal Deposition
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Reference electrode
Electrolyte
The in-situ experiment, we need to: Combining AFM/STM with the
potentialstate to form EC-AFM/STM
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Customizable in
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But there are tons of problems
• Atmosphere protection of Lithium
• Handling of electrodes and set up EC cells
• Noise isolation
•
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Problem: operating instrument inside glove box
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reference electrode
(no connection with
other electrodes)
counter electrode
(no connection with
other electrodes)
working electrode (in contact with Au)
Problem: handling electrodes
Problems
•Small parts
•Leak
•evaporation
•Corrosion
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Electrodes
Reference electrode: Mostly Ag, Cu ok for Cu deposition
experiment
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.
Problem: Small parts of Electrical Chemistry Cell
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The problems: corrosion and small nuts
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The problems: sample size and shape
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Customizable in
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The problems: being a chemist some time is helpless
Scientist need to learn engineering
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Desktop manufacture and its application in scientific research: its not 3D
printing
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• Road, highway, aircraft, high speed
railway (transportation)
• Language, literature, printing, phone,
computer, internet (information)
• Workshop, factory, ?? (manufacture)
The trend of civilization is toward the spread of knowledge and
technology, which empower individual toward equality
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Last revolutions: desktop publishing
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For the past 100 years, mass production industry had little change: standardization, scale and efficiency
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And the low cost CNC machines
$700 CNC Mill
$1000 CNC laser
$3000 CNC Mill
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Want to send me a Christmas gift : email to me。
Desk top manufacture is the an ongoing revolution—a product became a piece of information
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melting add glue to powder
Photo sensitive polymer laser melting
3D printing : precision adding of material
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The limitation of 3D printing: lack of control of material property
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Problems and inperfections of 3D printing
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Other affordable desktop production tools
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CNC laser cutting
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CNC laser cutting and its advantage
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CNC laser cutting and its advantage: pure 2D design easy to learn
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The basics to learn desktop manufacturing: start with CAD
Group/Presentation
Title
Agilent Restricted
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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
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Easy to learn and sometimes free trial amateur CAM
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Step 2: define the depth of each cutting
CAM turns a designed shape into reality
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Step 3: machine code tool paths generation by computer
CAM turns a designed shape into reality
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Step 4: actual cutting of a 2.5D part
CAM turns a designed shape into reality
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Back to Chemistry
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Solution to the problems of AFM inside a professional glove box: EC
cell made for easy to handle
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Solution to the problems of AFM inside a professional glove box: EC
cell made for easy to handle
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In-situ observation of SEI on HOPG electrode surface during charging
circle of a Li ion battery cell—the first circle
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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.
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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.
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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;
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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
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In-situ observation of SEI on HOPG electrode surface during charging
circle of a Li ion battery cell- the bottom SEI
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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)
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On going electrochemistry cell development
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Future work: EC AFM cell for Litihium Cell with heating and cooling
option
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Future work: EC AFM cell for Litihium Cell with oxygen feed to a porous
sample electrode
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Example of dish type EC liquid cell
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EC liquid cell for coin single crystals
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Customizable in
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EC liquid cell for gold bead single crystal
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My basement factory (total cost $3000)
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A few words about Keysight Techology AFM: Keysight AFM has the
space for innovation due to its tip scan design.