20.109(F12): Mod 3 Day 4 Solar cell assembly: Difference between revisions

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==Introduction==
==Introduction==
[[Image:Screen shot 2011-11-16 at 11.02.56 PM.png|thumb|x300px]]
[[Image:Screen shot 2011-11-16 at 11.02.56 PM.png|thumb|x300px]]
The principle of our dye-sensitized solar cells is that light absorption by a dye will provide the energy necessary to transfer its electrons to a mixture of Titania and Titania coated single walled carbon nano-tube(SWNT):phage complexes, which will act as a shuttle to deliver the electrons to an external circuit for extraction of "useful" energy. To complete the cell an Iodide redox mediator is used to recycle electrons back to the dye from a counter-electrode.  During the first two lab sessions of this third module, you worked to coat genetically-modified M13 phage with SWNTs and to mineralize TiO<sub>2</sub> upon them. (These steps are summarized visually in the top of the figure to the right) For today's session, you will use these complexes to construct the anode of the dye-sensitized solar cell.  (The anode can be seen in the bottom left of the image to the right)
As you have already seen in lecture, electrons flow through a dye-sensitized solar cell in the following manner:
#Dye becomes excited by light.
#Dye injects an electron very rapidly to the TiO<sub>2</sub> (the conduction band), dye is oxidized in the process. 
#Electrons are transported through the semi-conducting TiO<sub>2</sub>, move through the load, and eventually reach the counter electrode.
#At counter electrode, normally platinum, the electrons reduce the redox mediator located in the electrolyte of the DSSC.
#Redox mediator diffuses to meet and regenerate oxidized dye molecules.
 
In order for the above process to be completed, five general components must be included in a DSSC.  Below is a list of each of these general components, as well as the specific materials we will be using for each in our DSSC’s.
#Semi-conductor: TiO<sub>2</sub> particles enhanced with either gold or SWNTs via phage bio-templated assembly.
#Sensitizer (dye): N719 dye
#Electrolyte and redox mediator pair: I<sub>3</sub> - / I-
#Counter electrode: Pt
#Mechanical support: TCO (transparent conducting oxide) coated FTO (Fluorine doped tin oxide) glass.  This material will be used as the base of the anode in your DSSC.
 
==Protocols==
==Protocols==
===While You Were Out===
===While You Were Out===
[[Image:Photo050.jpg|thumb]]
[[Image:Photo050.jpg|thumb|Ethyl cellulose/Terpineol mixture(left)Final paste (right)]]
The TiO<sub>2</sub> mineralized SWNT:phage complexes that you left last time were dried in a vacuum oven at room temperature.  The dried substance was then ground, using a mortar and pestle, into a powder on the micrometer scale.  To this ground material, a paste of pure TiO<sub>2</sub>, ethyl cellulose (for viscosity) and terpineol (an organic solvent) was added.  To the right can be seen the image of the paste before the SWNT:Titania powder was added (left) and after (right).
The TiO<sub>2</sub> mineralized SWNT:phage or SWNT:gold complexes from M2D2 were dried in a vacuum oven at room temperature and ground to micron sized particles via mortar and pestle.  After grinding, pure TiO<sub>2</sub>, ethyl cellulose (binder) and terpineol (an organic solvent with a high boiling point) were added to make a paste. 
 
Additionally, FTO glass was coated with a thin layer of TiO<sub>2</sub>.  This glass will be used as the base of your anode. This was achieved by first cleaning the FTO glass, then incubating the glass in a solution of TiCl<sub>4</sub>.


The base of the anode has also been prepared.  It consists of a piece of glass coated on one side with 2mm of Florine-doped Tin Oxide (FTO).  Doping is the controlled introduction of impurities into an extremely pure semiconductor for the purpose of adjusting an electrical property of interest.  In this case, the Tin Oxide has been doped with Florine for the purpose of increasing its conductance.  After several cleaning steps, this base was incubated in a solution of TiCl<sub>4</sub>, a step designed to coat it with TiO<sub>2</sub>; this step is necessary for high efficiency performance of the device.
===Part 1:===
===Part 1:===
[[Image:Photo051.jpg|thumb]][[Image:Photo053.jpg|thumb]][[Image:Photo055.jpg|thumb]][[Image:Photo056.jpg|thumb]]<br>
[[Image:Photo051.jpg|thumb|Testing for resistance]][[Image:Photo053.jpg|thumb|Doctor blading preparation]]<br>
#Use a resistance meter to determine which side of a prepared glass anode base contains the layer of TiO<sub>2</sub> coated FTO.  The coated side of interest should have a measurable level of resistance while the pure glass side should not.
#Use a resistance meter to determine which side of a prepared glass anode base contains the layer of TiO<sub>2</sub> coated FTO.  The coated side of interest should have a measurable level of resistance while the pure glass side should not.
#With the coated side up, align your glass anode base onto a gridded template containing a 4mm x 4mm square so that the square appears in the center of the base.
#With the coated side up, align your glass anode base onto a gridded template containing a 4mm x 4mm square so that the square appears in the center of the base.
#Using scotch tape, create a "well" the size of the 4mm X 4mm square by taping everywhere on the glass except the small square. (One piece on each side and one on the top and bottom should suffice.)  Because the thickness of the tape is consistent (~50 micrometers), this method is a simple way to make uniformly sized solar cells.
#Using scotch tape, create a "well" the size of the 4mm X 4mm square by taping everywhere on the glass except the small square. (One piece on each side and one on the top and bottom should suffice.)  Because the thickness of the tape is consistent (~50 micrometers), this method is a simple way to make uniformly sized solar cells.
#Using a small brush, paint a small amount of the Titania paste that contains SWNT:Titania powder onto the top of the well.  The amount you use should be roughly equivalent to the amount seen on the photo to the right.
#Using a bent pipette tip, paint a small amount of the Titania paste that contains SWNT:Titania powder onto the top of the well.  The amount you use should be roughly equivalent to the amount seen on the photo to the right.
#Spread the paste evenly throughout the well using a glass rod as if you were rolling out dough with a rolling pin.  This process is known as "doctor blading."  Once spread, let the device sit for about 3 minutes; this helps reduce the surface irregularity of the paste.
#Spread the paste evenly throughout the well using the edge of a glass slide.  This process is known as "doctor blading."  Once spread, let the device sit for about 3 minutes; this helps reduce the surface irregularity of the paste.
#Carefully remove the tape from around the well and dry the glass device on a hot plate set to ~120&deg;C for 5 minutes.
#Carefully remove the tape from around the well and heat in air at 120deg for 5 min.
#Safely remove the coated glass from the hot plate and transfer it to an oven in the fume hood that will anneal the sample at 600&deg;C for 30 minutes.  At the end of this annealing step, the thickness of the coating you added should be ~7-8 micrometers.
#Repeat the doctor blading process, and heat again in air at 120deg for 5 min.
#The desired thickness of the photoanode is ~15 micrometers, so repeat steps 3 - 7 in order to achieve this.
#Heat in air for 4 hours at 310deg.  This step removes the virus and cellulose from the device.  <br>
#After letting the device cool from the annealing stage, immerse it in an Ru620 dye solution that contains 1:1 acetonitrile and tert-butyl alcohol.  This will be left at room temperature until the next lab session where the counter electrode along with the completed device will be assembled and tested.<br>
[[Image:Photo056.jpg|thumb|Anode immersed in dye]]
(To be completed by TA)
#Heat in Argon for 30min at 500deg.  This step calcinates the TiO<sub>2</sub> nanoparticles, increasing crystalinity as well as connecting the particles to one another (which is important to electron transport in the device).
# After letting the device cool from the annealing stage, immerse it in Ru620 dye solution that contains 1:1 acetonitrile and tert-butyl alcohol.  This will be left at room temperature until the next lab session where the counter electrode along with the completed device will be assembled and tested.<br>
 
===Part 2:===
===Part 2:===
The groups not visiting the Belcher lab should use the extra time to work on their research proposals. These will be presented/turned in just one week from today! You can review the requirements for the final proposals [[20.109(F12): Oral presentation of research proposal| here (oral presentations)]] and [[20.109(F12): Written research proposal| here (written proposals).]]
The groups not visiting the Belcher lab should use the extra time to work on their research proposals. These will be presented/turned in just one week from today! You can review the requirements for the final proposals [[20.109(F12): Oral presentation of research proposal| here (oral presentations)]] and [[20.109(F12): Written research proposal| here (written proposals).]]

Latest revision as of 23:53, 28 November 2012


20.109(F12): Laboratory Fundamentals of Biological Engineering

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Solar Cell Assembly

Introduction

As you have already seen in lecture, electrons flow through a dye-sensitized solar cell in the following manner:

  1. Dye becomes excited by light.
  2. Dye injects an electron very rapidly to the TiO2 (the conduction band), dye is oxidized in the process.
  3. Electrons are transported through the semi-conducting TiO2, move through the load, and eventually reach the counter electrode.
  4. At counter electrode, normally platinum, the electrons reduce the redox mediator located in the electrolyte of the DSSC.
  5. Redox mediator diffuses to meet and regenerate oxidized dye molecules.

In order for the above process to be completed, five general components must be included in a DSSC. Below is a list of each of these general components, as well as the specific materials we will be using for each in our DSSC’s.

  1. Semi-conductor: TiO2 particles enhanced with either gold or SWNTs via phage bio-templated assembly.
  2. Sensitizer (dye): N719 dye
  3. Electrolyte and redox mediator pair: I3 - / I-
  4. Counter electrode: Pt
  5. Mechanical support: TCO (transparent conducting oxide) coated FTO (Fluorine doped tin oxide) glass. This material will be used as the base of the anode in your DSSC.

Protocols

While You Were Out

Ethyl cellulose/Terpineol mixture(left)Final paste (right)

The TiO2 mineralized SWNT:phage or SWNT:gold complexes from M2D2 were dried in a vacuum oven at room temperature and ground to micron sized particles via mortar and pestle. After grinding, pure TiO2, ethyl cellulose (binder) and terpineol (an organic solvent with a high boiling point) were added to make a paste.

Additionally, FTO glass was coated with a thin layer of TiO2. This glass will be used as the base of your anode. This was achieved by first cleaning the FTO glass, then incubating the glass in a solution of TiCl4.

Part 1:

Testing for resistance
Doctor blading preparation

  1. Use a resistance meter to determine which side of a prepared glass anode base contains the layer of TiO2 coated FTO. The coated side of interest should have a measurable level of resistance while the pure glass side should not.
  2. With the coated side up, align your glass anode base onto a gridded template containing a 4mm x 4mm square so that the square appears in the center of the base.
  3. Using scotch tape, create a "well" the size of the 4mm X 4mm square by taping everywhere on the glass except the small square. (One piece on each side and one on the top and bottom should suffice.) Because the thickness of the tape is consistent (~50 micrometers), this method is a simple way to make uniformly sized solar cells.
  4. Using a bent pipette tip, paint a small amount of the Titania paste that contains SWNT:Titania powder onto the top of the well. The amount you use should be roughly equivalent to the amount seen on the photo to the right.
  5. Spread the paste evenly throughout the well using the edge of a glass slide. This process is known as "doctor blading." Once spread, let the device sit for about 3 minutes; this helps reduce the surface irregularity of the paste.
  6. Carefully remove the tape from around the well and heat in air at 120deg for 5 min.
  7. Repeat the doctor blading process, and heat again in air at 120deg for 5 min.
  8. Heat in air for 4 hours at 310deg. This step removes the virus and cellulose from the device.
Anode immersed in dye

(To be completed by TA)

  1. Heat in Argon for 30min at 500deg. This step calcinates the TiO2 nanoparticles, increasing crystalinity as well as connecting the particles to one another (which is important to electron transport in the device).
  2. After letting the device cool from the annealing stage, immerse it in Ru620 dye solution that contains 1:1 acetonitrile and tert-butyl alcohol. This will be left at room temperature until the next lab session where the counter electrode along with the completed device will be assembled and tested.

Part 2:

The groups not visiting the Belcher lab should use the extra time to work on their research proposals. These will be presented/turned in just one week from today! You can review the requirements for the final proposals here (oral presentations) and here (written proposals).

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