Stacking

Before starting to stack your 2D materials you should think in what type of stack you want to do and what are the more appropriated methods to do so. Here are some examples:

Stacking to a fragile substrate (e.g., TEM grid): For this you migth want to use the membrane transfer. This one consist in exfoliating in a polymer and releasing this as a membrane to later deposit it the target substrate. You can find all the details in this article and its supplementary.

Stamping: This is the so called dry technique and consists in using a 2D material to pick up sucesive 2D materials. One of the first publications to explain the technique is here. The animation below is very self-explanatory of the process.

Illustration of the principle of stacking 2D materials process. Courtesy of Cory Dean (Columbia University).

The process consist in picking up the different 2D materials one at the time using a combination of polymers (e.g., PPC or PC on top of PDMS) or a SiN membrane (see here). After picking up all the different 2D materials the polymer is melted on top and the stack deposited on the substrate of your preference.

The hot pick up technique (under construction):

Bubble squeezing: After picking up all the layers you might realize that some bubbles are formed in your stack. This are formed of tape residues, water and/or air. To clean up your stack you can squeeze the bubbles mechanically at higher temperatures. The techniques to do this (either with PC or PPC) are described in the following article. As you can see in the pictures bellow the technique is very effective to get ride of bubbles

Stack on PPC slide before bubbles squeezing
Squeezing process in progress

PDMS stamping: As you could see all along this post we have mentioned two main polymers PC and PPC that are deposited on top of PDMS, these are the most used ones in for the stacking. However, there are other polymers also used for this, in the following table we summarize them and give you their main use and temeprature range to be used.

PolymerTemperature
pick-up
Temperature releaseCleaning
PPC
Ploy(propylene carbonate)
40 oC80 oC – 120 oCAnnealing in vacuum
at 360 oC
PC
Polycarbonate
90 oC185 oCChloroform
PET
Poly(ethylene terephthalate)
60 oC130 oC
PVC
Poly(vinyl choride)
70 oC130 oC
PCL
Poly(caproalactone)
30 oC60 oC
Table of polymers to transfer 2D materials in a PDMS stamp

Cutting 2D materials

Now that you have the basic notions of stacking you can start preparing twisting heterostructures. For twisted graphene structures the most widely used technique is the tear and stack technique detailed here. However, the tear part of this technique has been proven to give many problems of breaking the layers. A clear improvement in reproducibility has come with the implementation of different techniques to cut graphene before starting the stacking. Here we list few of them:

  • AFM cutting: the anodic oxidation nanolithography consist in applying a high frequency (>10 kHz) AC voltage to a Pt/Ir coated AFM tip (e.g., Arrow-NCPt-50, available here), to design on it a desired pattern, the resolution of the cut can go down to 10 nm, which makes it particularly interesting for polymer-free lithography of graphene. The full explaination can be found in this research article. An example of what can be done in graphene:
Optical image of a graphene sheet cuted with an AFM.
  • AFM tip on PDMS cutting: A cheaper version of this technique can be achieved by sticking an AFM tip to a PDMS stamp. The PDMS stamp is placed in a transfer station, the optical microscope of this allows you to see when the tip enters in contact by a change in its reflectance. Once in contact the stage is moved to cut the graphene or move pieces of 2D materials that you don’t want in the way, as depicted in the picture below.
a, AFM tip on PDMS stamp. b, AFM tip cutting a graphene flake, zoom on the flake after cut can be seen in c. d-f, AFM tip use to remove an undesirable BN flake
  • Laser cutting: by using a laser (filters between 500 nm and 600 nm) we can perform cuts in graphene and graphite layers in a fast and easy way. This technique was developed by Lutz Waldecker at RWTH and we added a joystick to to make it easier to use:
Laser cutting in action. You can see as the laser spot cuts a thick piece of graphite leaving a trench os ~4 um.