Substrates

Your substrate literally is the foundation of good results. Here are some things to consider when choosing a substrate.

Substrate Considerations

Substrate choice can be very crucial in microscopy. In some cases, the wrong substrate can make a given microscopy technique impossible. Some things to consider when choosing a substrate:

Conductivity

Some techniques require a pathway for electrons to and from the sample, e.g. SEM and STM. In such a case, mica, an insulator would likely be a poor choice. However conductive coatings, such as a gold film can make the surface usable. Be sure to know if your microscopy has special needs in this regard.

Smoothness/Roughness

The desired technique as well as the desired data can both require varying degrees of flat clean surfaces. How smooth does your substrate need to be?

Sample-Substrate Interaction

Chemical reactivitiy and mobility are common concerns as well as whether or not your sample will even stick to the substrate. If you are using spin coating to deposit your sample, then sticking is even more important of an issue.

Common Substrates

Gold Films

I have worked almost exclusively with gold on mica thus far, but gold films are also commercially available on glass (see below).

    • Pros
      • Atomically flat terraces; per Molecular Imaging, "Atomically flat terraces are typically several hundreds of nanometers across, with this size increasing after hydrogen flame annealing."
    • Cons
      • Mica is not a fun material to cut. It is easy to unintentionally delaminate the mica, deform it, and/or make the gold film unusable. Take a look at cutting mica, below. Because of the gold film, the punch method is not very useful, due to contamination (when you see a punch, you'll understand).

Vendors

    • Arrandee - These folks specialize in gold on glass. Nota bene: Hydrogen flame annealing is too hot for these substrates.
    • Platypus Technologies, LLC - They specialize in gold-coated substrates, providing gold on mica, glass, and silicon wafers.
    • Molecular Imaging - Makers of SPMs and gold films on mica.

HOPG

I found useful info on HOPG use to be quite sparse so I thought I would type up what I have found.

Vendors

You need to buy some before you can use it.  Following are the only vendors I know of thus far:

Pros

  • HOPG can be cleaved to a nice, clean surface.
  • It is conductive
  • It is made of carbon

Cons

  • It is quite expensive, about hundred-fold more expensive than mica
  • Lead times for orders are usually at least a week
  • Very few vendors which leads to a lack of competitive salesmanship that fosters good customer service

Preparation

  • Cutting
    • Life is easier if you can avoid this, but the best method seems to be a clean, sharp razor blade.  I later was told that's how Advanced Ceramics does it.  You will likely introduce clumping at the edges and shear forces that will split the HOPG along the planes, producing multiple, thinner pieces of HOPG.  The less cutting a specific piece undergoes, the better.  I have successfully cut a piece on all four sides and used it, but it required a lot of finesse, patience, and tape (of course, I wanted a double-sided cleaving as well).
  • Cleaning one side
    • HOPG is a layered surface which you can cleave using simple scotch tape.  Unlike mica, some HOPG samples seem to have a distinct preference for which direction will provide the best cleaving.
  • Cleaning both sides
    • This can be irritating.  There are two approaches I have had reasonable success with:
      • use two pieces of tape simultaneously, cleaving one surface and then the other
      • basically cleave each side in succession:
        • secure a glass slide to a surface
        • put a piece of sticky tape on it with a tab hanging over the edge of the glass
        • put the HOPG on the tape
        • use a second piece of normal scotch tape to cleave off the top surface
        • pull up the tape and repeat
        • Note: the second time around, you may want to carefully scrape the the sticky tape up with a razor blade so that you can cleave the underside cleanly again
  • Thickness
    • Once the HOPG get to the order of ~0.1 mm thick, it starts to become to flexible and cracks and defects due to simple bending of the substrate become very problematic.

Mica

A mineral formed in flat layered sheets.

    • Pros
      • Cheap
      • Easy to cut into desired shapes
      • Easy to clean via simple cleaving with scotch tape
    • Cons
      • A fair amount of mica is too poor a quality for some uses
      • Solvent can get trapped in the substrate
      • Brittle, thin material
      • Insulating - inadequate, as is, for some applications, e.g. STM
    • Conductivity: Mica is an insulator, although it is often used as a substrate for a conductive layer, esp. gold films. Even with such films, attention needs to be paid to making sure the conductivitiy needs of your technique, if any, are met.
    • Smoothness: RMS roughness of < 1 nm over one square micron is easily achieved.

Cutting Mica

Cutting mica can be problematic. There are two basic approaches that I have found viable, using a sharp straight blade to make a guillotine-like cut or a precision punch. If you have good advice and/or suggestions, please do not hesitate to contact me.

Guillotine Cut

To make a guillotine-like cut, you simply have to arrange the system so that the blade cuts through at a slight angle away from the surface. I have actually used a simple hobby tool for this, the Chopper. Note: this is still very much an art. You can buy one of these via most Railroad hobby shops, or online hobby sites like micromark.com.

It consists of a standard razor blade affixed to a metal lever. By placing a thin teflon block under the blade, a guillotine-like cut can be approximated reasonably well. A slight curl sometimes results., but with practice the frequency of this problem can be minimized.

Note: some folks have good luck with using a fresh razor blade flat against the surface, but the occurence of delamination seems greater.

Punches

Quality punches are great for making discs of mica for AFM imaging. Incredibly easy and quick without delamination. Surface contamination is certain, but with mica, the ability to cleave off both surfaces to produce a clean surface makes this problem moot. I have found the hand held punches from Ted Pella, Inc. produce a messy disc, but of course, they offer nice clean mica discs for sale. Clearly, this option is not as desirable for gold-coated mica as you may rip the gold surface off or damage/contaminate it beyond utility.

Vendors

    • Ted Pella, Inc. - They sell V1 and V2 (a higher grade); use their site search engine to find it. I have good dealings with these folks.
    • B & M Mica Co., Inc., P.O. Box 525243, Flushing, NY 11352, USA. Tel: 718-461-6233, Fax: 718-461-0414. 0.0001" Thick & Up (need to call and verify)

MoS2 (Molybdenum disulfide)

This material can be a real nuisance to work with, because it is a thin flimsy film. I have worked with it too little to offer up more information right now.

Vendors

Sapphire (Al2O3)

Sapphire is single-crystal Al2O3.

  • Pros
    • flatness - as low as 3 Å roughness (Ra) [Wafer World]
    • transparent - handy if you wish to backside illuminate the system (lasers, etc.)
    • hardness - Moh's hardness of 9 (out of 10); it can cut glass.
    • Melting point - 2320 K (softening point 2070 K)
  • Cons
    • hardness - (see above); it can only be cut by diamond
    • somewhat expensive
    • may require dicing service

Information Links

Cleaning Sapphire - I use a piranha solution to clean the wafers and I had good results; see my cleaning page for details.

Silicon

    • Pros
      • Well characterized
      • History of use, which makes protocols related to it easier to find
      • Robust, not as brittle as mica, for example
    • Cons
      • Difficult to cut into desired shapes, unless your desired shapes are rectangular
      • Good cleaning is time-consuming
    • Conductivity: Silicon is a semiconductor. Doping can have profound effects on conductivity, as can the thickness, if any, of the oxide layer. You should get this number from your manufacturer.
    • Roughness: This will depend on your processing methods, if any. Generally, < 1 nm RMS roughness over one square micron is easily achieved.

     

Surface-Modified Substrates

  • Ssens - ready-made modified surfaces, reagents to modify surfaces, and contracting to create custom solutions.

Dicing Wafers

I will try to assemble companies here as I learn about them.

 

Questions? Comments? Please let me know via my questions/comments form!