PVK Poly(N-vinylcarbazole) info

Mw about 1.1Mg/mol
Tg: 200.0 C

Calibration of micrograph image's dimension

This refers to micrographs taken with the CoolSNAP Pro CCD camera in our lab.

The CCD used in the CoolSNAP Pro color camera has a 1/2" format, which means the size of the CCD is: 6.4mm x 4.8 mm
So if the 5x objective is used, the micrograph's physical dimension is:
(dimension of CCD) / 5
or
1.28 mm x 0.96 mm

Similarly, with 10x objective, the micrograph's physical dimension is:
0.64 mm x 0.48 mm

These values can be used to calibrate the dimensions of micrographs taken by this camera.

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L-shaped lens in the lab:
magnification: 1.5x, 2.0x, and zoom lens 0.7x - 4.55x

Q-imaging 1394 firewire CCD camera: 1/2" CCD (6.4 mm x 4.8 mm)
Resolution: 1392 x 1040

L-shaped lens with 1/2" CCD:
zoom lens at 4.55x: physical dimension of the image is 468.86 micron in length and 351.65 micron in width
zoom lens at 0.7x: image dimension is 3047.6 micron x 2285.7 micron

For calibration at 4.55x: 468.86 micron/1392 pixel = 0.3368 micron/pixel
For calibration at 0.7 x: 3047.6 micron/1392 pixel = 2.1894 micron/pixel

ITO glass purchase info and specification

ITO coated glass purchase information & specifications

Quotation:
Substrate: Polished soda lime float glass
Dimensions: 14" x 14" x .043"
Coating: SiO2 / ITO per specification S1X0015
Qty/Price: 20 sheets @ $65 EA; 25 sheets @ $60 EA
Minimum Order: 20 sheets

Other specifications:
ITO thickness about 150 nm, Resistance about 9~15 Ohm/square

Contact info:

Shane Vincent
svincent@coloconcept.com
www.coloconcept.com
Colorado Concept Coatings LLC
1110 N. Boise Ave
Loveland, CO 80537
Ph# (970)635-2797 Fax# (970)635-3054

More information on website

Cut ITO glass into small pieces

Use the diamond cutter located in Wagner's group of room J423.

To use the sample holder that can hold 4 pieces together for cathode evaporation, the ITO glass dimension should be between 25~31 mm.
As a rough indicater, align the edge of the glass to the 3rd line counted from the 6" mark toward the 5" mark in the ruler will result in a size of around 28 mm.

For ITO glass pieces used for my design of passive matrix display, the dimension is 35 x 35 mm.

PEDOT layer spin coat recipe

PEDOT solution is Baytron P VP CH 8000, solid content about 2.5%.
The following recipe is used for preparing OLED with F8BT as the active material.

1. First dilute with DI water to about 1.5% by adding 0.6 ml DI water into 1 ml original solution.
2. Use a syringe with a 0.2 micron PVDF membrane syringe filter to filter the prepared solution.
PVDF is hydrophilic and is good for aqueous solution filtering. Do not use hydrophobic membrane filters, such as PTFE.
3. Spin time is 30 sec. For spin speed of about 3,500 - 4,000 rpm, the film thickness before baking is ~ 40 nm.
4. Hotplate bake for 60 minutes at 150C.

alumina coated basket for metal evaporation

Purchase information for alumina boats used for Ca evaporation:
Vendor: CM Furnaces
Part No.: R-123-C
Price: $28.50 each

Catalog of Al2O3 coated evaporation basket from CM Furnaces.

F8BT solution

F8BT (American Dye Sources, ADS133YE, Mw ~16,000 ) in p-Xylene solution.
p-Xylene density: 0.86 g/ml.

F8BT in p-Xylene: 10 mg/ml.

Pluronic L62 block copolymer surfactant

Pluronic L62 block copolymer surfactant from BASF

Photodiode specification used for OLED testing

The photodiode mentioned here is the one used in our lab for measuring OLED emission.
It is model PIN-10DP from UDT Sensors, Inc.

click here for the specification detail

Surface tension of common liquids

Surface tension of common liquids

Spin coat photoresist on fluorinated substrate

It is difficult to spin coat a photoresist on a fluorinated substrate due to its ultra-low surface energy.
In my case the substrate (ITO coated glass, or SiNx layer coated on ITO-glass) is coated by PFOTS first. Photolithography followed by RIE are then applied to pattern the PFOTS/SiNx double layer simultaneously. In this way the PFOTS layer is self-aligned with the SiNx.

The spin recipe for the spin coat of AZ5214 photoresist on PFOTS coated layer used is given as follows.

1. 500 rpm, accelaration 100 rpm/sec, time for 5 sec.
2. 4,000 rpm, accelaration 1,000 rpm/sec, time for 40 sec.

The first step is used to coat the fluorinated substrate with photoresist at a low spin speed. As observed from experiment, a fast spin speed can easily throw away most photoresist due to the non-stick property of the fluorinated substrate.

As usual, spin on a HDMS layer first, followed by a AZ5214 layer.

Photopic Luminous Efficiency Function

1988 CIE Photopic Luminous Efficiency Function

Here is the curve.


Here is the original data.

Manual for 4-source evaporator

Before you go ahead, please check the following points:

• Computer on? Controller software running?
• Compressor on?
• Gate valve open?
• Machine in auto-mode?
• Temperature read-out below 16K?
• “Vent Valve” closed?
• “Source Power Disconnect” off?
• Pressure in chamber below 10^-6 torr?

If any of these checks fail, proceed to trouble shooting section or ask a more knowledgeable person.

Putting your samples into the chamber

• Undo the latch on the chamber door.
• Turn vent valve open. Green lamp above switch should turn on; you should hear the gate valve closing and the nitrogen stream into the chamber. Watch the chamber pressure rising.
• After the chamber door pops, close vent valve.
• Fill materials into the boats as needed. Make sure you put the right material into the right boat.
• Change glass slides.
• Put samples into the sample holder.
• Close door and hold it closed with your right hand.
• Hold door closed while switching on the auto-pump-down. Wait for a while. Don’t be surprised by the noise when the mechanical pump kicks in.
• Watch chamber pressure drop for a while.
• Make sure the “HOLD/PLC START” switch is in the “HOLD” position (i.e., vertical). In that position the evaporator will not begin with the actual evaporation after a certain pressure is reached. In the “PLC START” position, the evaporation will start automatically, which is good if the process is very stable. But considering that you have to consult this manual, it is probably better to leave the switch in the “HOLD” position.
• After about 15-20 minutes, the pressure should be low enough to start with the evaporation.

Programming the Evaporation Controller

• Go to “Edit” > “Process” using the mouse pointer.
• A new window with the header “Process Edit” will appear.
• Choose your process using the list supplied right below the header. A list of standard recipes is provided in the logbook.
• Go to the tab “Layer” and adjust the thickness and the evaporation rate using either the mouse or the dial knob above the mouse pad.
• If you need to edit a new process, go to the next section.
• Close the window by hitting the “CLOSE FORM” key on the left side of the display. If you changed the process, you will be asked to confirm the change.
• Switch on the “SOURCE POWER DISCONNECT”. The green lamp above it should turn on. If not, go to troubleshooting.
• Also, turn on all the needed power supplies. The respective green lamp should turn on.
• Make sure the “SAMPLE SHUTTER” is in the “AUTO” position (vertical).
• The machine is now ready for the evaporation process. Start the process by hitting the “START PROCESS” key.

Take out your sample

• Wait for sample to cool down (30 minutes).
• Undo the latch on the chamber door.
• Turn on “VENT VALVE”.
• After the chamber door pops open, close vent valve.
• Take out your sample.

• Close door and hold it closed with your right hand.
• Hold door closed while switching on the auto-pump-down. Wait for a while. Don’t be surprised by the noise when the mechanical pump kicks in.

• Watch chamber pressure drop for a while.

Remember to switch off “SOURCE POWER DISCONNECT”!

Cryo Pump Regeneration

• Purge for less than a second then close purge switch;
• Rough pump ON, Fore Line valve OPEN to pump down to 5.0x10^-2 torr;
• Close Fore Line valve and stay for 5 min.
• Repeat.
• If vacuum can stay below 7x10^-2 torr for 1 min. Ready to start cryo compressor. Make sure water flow is above 5.

720 shut down and restart

• Shut down procedure: Click “ON” -> File Menu, select exit -> “Start” & select shut down computer -> power off by push 3 Red buttons
• Restart procedure: Start power by push 3 green buttons from left to right -> small room, push “start” button to top position once on the cooler -> computer login as 3333@3333 -> “utilities”: select “turbo pump on” to turn on the turbo pump. -> select a different view diagram to see the turbo pump change from red color to green and done when it’s green.

OLED preparation

• Wash 4 vials using CHCl₃ -> Acetone -> Isoproponal, then blow dry
• Weight 100mg PVK, 40 mg PBD, 6-12 mg C6 (C47, niel red)
• 100 mg PVK + 40 mg PBD + 7.2 ml C.B., bar stir for 1 hour,
  Prepare: 1 mg/ml C6 in chlorobenzene (C.B.); 1 mg/ml C47 in C.B.; 1 mg/ml nile red in C.B.
• Syringe filtering
• Prepare : 100 mg PVK + 40 mg PBD + 0.3 mg C6 in 7.5 ml C.B. for green; 100 mg PVK + 40 mg PBD + 0.2 mg nile red in 7.5 ml C.B. for red; 100 mg PVK + 40 mg PBD + 1 mg C47 in 7.5 ml C.B. for blue emission.
  
• ITO glass: oxygen plasma treatment, plasmatherm 720, 150 mTorr, O2=25 sccm, 25W, 4 minutes;
  
• Spinning coating of PVK+PBD+C6 film, 2000 rpm, 50 sec.
• Bake on hotplate: 80~100 C, 20~30 minutes
  
• Evaporate Mg/Ag cathode. (For Mg evaporation, set I=0 in the automatic control program for stable evaporation)
  

PFOTS SAM growth

PFOTS monolayer self-assembly on SiO2 layer, which is also true for Si wafer when there is a thin oxide layer on the surface.
Use photoresist to pattern the wafer surface since PFOTS will only self-assembly on exposed surface regions.

• No Water! And thus no acetone, isopropanol, methanol. Work in glove box.
• Soap photoresit patterned dry wafer in dodecane for 5 minute
• Add several drops of PFOTS in dodecane and stay for 5 minutes. During summer days when the humidity is high, increase this soap time to 20 minutes in order to achieve a fairly good result.
  
• Rinse in DI water, blow dry
• Use TCE (trichloroethylene) to wash the dish

Hydrophilic treatment

After PFOTS SAM growth, put the wafer in H2O2+H2SO4+H2O (1:1:10) at 40 C for less than 5 minutes can treat the uncovered region more hydrophilic.
--from Anton Darhuber

Remove Photoresist with Oxygen Plasma

in Plasmatherm 790:
Pressure=100 mTorr, O₂=50 sccm, Power=200 W, Time=2 min

Etch SiNx with Plasmatherm 720/790

by Plasmatherm 720

• Pressure=50 mTorr, O­₂=10 sccm, CF₄=70 sccm, Power=100 W
• Rate= 300 nm/ 1.5 min

by Plasmatherm 790

• Pressure=60 mTorr, O­₂=4 sccm, CF4=35 sccm, Power=75 W
• Rate=100 nm/1.5 min; 400 nm/ 5.5 min
  

HF wet-etch of SiNx

1. HF:DI water=1:5, isotropic etch? Rate= very high
2. Suitable for remove all SiN_x and when there is no metal contact

Etch Silicon with Plasmatherm 720

1. Pressure = 100 mTorr (?), SF₆ 100 = 65 sccm, CCl₂F₂ = 15 sccm, Power = 100 W
2. Rate = 2.5 mm/ 10 min; (5 min for about 1 micron)
   

Etch SiNx with Plasmatherm 790

1. Pressure=35 mTorr, O­2=4.0 sccm, CF4=35 sccm, Power=75 W
2. Rate= 300 nm/ 2 min; (for SiNx prepared by FSIN500 in 790 for 10 min 30 min, the etch time is 1 min 30 sec)
3. Optional: dip into HF: DI water=1:5 for 10 seconds

PECVD SiNx on Plasmatherm 790

The whole process takes about 2 hours.

1. Set substrate temperature to 250 °C;
2. Run "jdepprep" recipe that is a 15-minute etch of an empty chamber. Increase the etching time if needed;
3. Load a clean bare Si test wafer, run program "jpredep". The recipe consists of a 3-minute-long etch, followed by a 3-minute-long Ar plasma, and a 3-minute-long SiN deposition;
4. Load your wafer on top of the Si wafer. Run program "jSIN500". Skip the 3-minute-long Ar plasma, if desired. Pump the chamber for 15 minutes before you run the recipe. Growth rate about 1.59 Å/sec. 10 min 30 sec for ~ 100 nm. (etch time : 1 min 30 sec)

AZ5214 as a positive photoresist

Note: 2.0 W is 2 mW/cm^2

1. Spin on HMDS, recipe 1 (4000 rpm, 40 second);
2. Spin on AZ5214, recipe 1;
3. Soft bake for 1 min at 95 °C;
4. Expose with mask on MA6 for 35-45 seconds;
5. AZ 312MIF: DI water=1:1, develop for 1 minute and rinse in DI water;
   
6. Post bake at 110 °C (2-6 mins).

--from Troy Abe

Rebecca’s recipe for AZ5214 (achieve 2.5 micron feature)

1. Clean pieces: acetone 30 sec ultrasonic, 3x; isopropanol 3x; N2 blow dry;
2. 110°C, 15+ min on foil, hotplate dehydrate bake;
3. HMDS 40 sec, 4,000 rpm, spinner recipe 1;
4. AZ5214 40 sec, 4,000 rpm, spinner recipe 1;
5. 95°C, 1 min hotplate softbake on glass slide, slide directly on hotplate;
6. Clean mask acetone 1x isopropanol 1x, N2 dry;
7. Light field mask: Expose 2.0 mW/cm2 for 25 sec using MA6, CL1
   Dark field mask: Expose 2.0mW/cm2 for 40 sec using MA6, CL1
   I use hard contact, WEC=contact;
8. Light field mask: Develop 20-25 sec, 1 : 1 AZMIF 312 : H2O
   Dark field mask: Develop 40 sec in 1 : 1.2 AFMIF 312 : H2O
   I always check the development time on a test sample first--
   sometimes it needs to be shorter. I constantly agitate my sample in the
   developer.
9. DI rinse about 1 min, N2 dry;
10. Inspect under microscope;
11. Hotplate hard bake: for liftoff of metal, no bake; for RIE of SiGe/Si/poly - 110°C, 3 min on foil; for SiO2 etch (HF/BOE or RIE) - 110°C 6 min on foil.

--from Rebecca Peterson

Clean ITO glass

• Add 5~6 drops of Micro-90 solution into DI water;
• Heat to boil;
• Put into ultrasonic cleaner. Add DI water to the line. Ultrasonic clean for 60 minutes;
• Rinse clean by DI water;
• Ultrasonic clean with DI water for another 60 minutes; or repeat from beginning.

--from Ke Long

PDMS stamp preparation

• Weight 15 g A and 1.5 g B (10:1)
• Mix thoroughly for at least 15 minute
• Vacuum degas until all gas bubbles have gone. (25 mmHg for more than 20 minute)
• Template covered by dimethyldichlorosilane SAM
• Pour onto template
• Cure in oven at 100 C (knob reading at ~ 5.1) for 1 hour
• Peal off

--from Troy Abe

MA6 Quick Alignment Tip

• Go to spot #1, press “Set Ref”
• Go to spot #2
• Press “Scan” to go back to Spot #1
• Press “Scan” to go to Spot #2 again

--from Rebecca Peterson

AZ5214 as a negative photoresist

1. Clean sample with acetone, isopropanol and blow dry. Bake
2. Spin on HMDS use recipe 1 (4,000 rpm, 40 sec);
3. Spin on AZ5214 use recipe 1 (4,000 rpm, 40 sec);
4. Soft bake at 95 C for 1 min 15 sec use hotplate;
5. Exposure with mask, 30 sec (MA6);
6. Bake at 110 C for 1 min;
7. Flush exposure without mask for 1 min 30 sec (MA6);
8. Develop use MIF312 : DI = 1 : 1 for 40 sec.

--from I-Chun Cheng

ITO etch recipe

Sample preparation:
ITO glass patterned by photoresist with 110 C hard bake for 5-6 min

Etch solution: 10 DI water : 9 HCl : 1 HNO3
Temperature: 40-60 C, use hotplate

Etch time:
ITO thickness 150 nm, etch time is 3 min at 45 C
ITO thickness 80 nm, etch time is 2 min at 45 C
New ITO glass, etch time is 3 min 45 sec at 45 C

Check:
Use multimeter to check the glass resistance. When etch is done, the measured resistance should be infinite.

--from Ke Long