How to grow your first sample: (2×4)/(4×2) transition 

Faebian Bastiman

The (2×4)/(4×2) RHEED transition is a very useful flux calibration point, since it tells you when your As and Ga fluxes are equal. I described what a (2×4) and a (4×2) reconstruction are in my What is a reconstruction post. In this post I will explain how to spot the transition with RHEED.

First of all you need to produce a good starting (2×4) surface. In order to do that follow the steps in my Oxide remove post. With the Ga shutter closed and an As overpressure incident on the sample you should see the As-rich (2×4) reconstruction on your RHEED pattern (Figure 1a). How can you be sure this is a (2×4) and not a (4×2) in disguise?

You can be 99% certain that if you are annealing at a temperature around 15 °C below the oxide remove temperature and the As flux that you are supplying is sufficient to grow GaAs that this is a (2×4) reconstruction. You can test very simply by stopping the rotation so you can see the 4x on the [‑110] azimuth and reducing the temperature. Reduce the temperature until a 2x appears. Rotate to 90° to the [110] azimuth. Still 2x?

If yes, then this a c(4×4) and the early reconstruction was a (2×4). Return to the original temperature and retrieve your (2×4). Note if you want to know what a c(4×4) is read my As cap post.

If no, and you are looking at a 4x, then this is now a (2×4). Remain at this temperature.

If no, and you are also not looking at a 4x, then something is very, very wrong with your sample. Are you sure it is GaAs(100)?

Assuming you have found your (2×4) make sure it looks like the one in Figure 1. If not change your temperature by 5 – 10 °C and your As flux by 10-20% and try to get the best (2×4) you can. You will note that in Figure 1a on the [‑110] azimuth the 4x rods are fairly short and bright even if the 2nd order rods are not very clear. The 2x on the [110] azimuth is simply a 2x and cannot give you any quality information at this point.

Try opening the Ga shutter. Does your 4x change to look like Figure 1b? It should. The Ga flux breaks up the static (2×4) and creates some disorder. This disorder results in an elongation of the 4x rods and an overall decrease in the intensity. The 2x on the other hand does not really change. You can consider Figure 1b as the dynamic (2×4), where “dynamic” means “growing”.

RHEED Ga to As

We are about to search for the Ga-rich (4×2) pattern. In your first few attempts do not rotate the sample, but rather keep the RHEED pointing along the [110] azimuth and looking at the 2x pattern. During the search the 2x will change into a 4x on [110] and the 4x will change into a 2x on [-110]. You can see the Ga-rich reconstructions in Figure 1d.

The problem with performing the transition without rotation is that you are only seeing the transition at the point the RHEED beam is hitting with the Ga and As flux pattern present at that point. This As/Ga ratio can be very different from the one created whilst rotating, since when you rotate you create a more even flux across the wafer. On the other hand since both the starting and ending reconstructions have both a 2x and a 4x azimuth it is not so obvious when the transition has happened until you have some experience looking at it.

So with the rotation off, the Ga shutter open and the 2x on the [110] azimuth on the screen close the As shutter (or close your cracker valve if you do not have a shutter).

Am I serious?

Yes.

Close the As shutter for a few seconds and watch the RHEED, it should quite rapidly turn into a 4x like Figure 1d. Once it does open the As shutter again and make sure the 2x returns. When the As flux is greater than the Ga flux, you see the 2x of the (2×4) when the Ga flux is greater than the As flux you see the 4x of the (4×2). In the extreme case we just witnessed the Ga was of course practically infinitely bigger than the As flux.

Ok step 2 is a little less brutal… with the rotation off, the Ga shutter open and the 2x on the [110] azimuth on the screen… half the As flux. Wait 15s. Did the 4x appear? If yes return to the original As flux, if no half the As flux again. What you are doing is performing a binary search. You take the lowest As flux you know gives you a 2x and the highest As flux you know gives you a 4x and you apply the average of the two and see if you get a 2x or a 4x. Always wait the same 15s between flux changes for consistency.  

You may notice on your search that the 2x creates a rather dim 3x rather than the desired 4x (Figure 1c). This is a mixed reconstruction between the (2×4) and (4×2) that many people overlook. It is weak on both [110] and [-110] azimuths and hence probably lacks the long range order of the (2×4) and (4×2) reconstructions. The low intensity makes it difficult to say whether it is a (3×1) or a (3×4) or a (3×6) and indeed the physical surface of the GaAs could be made up of domains of each.

Once you have found the maximum As flux that gives you a 4x on the [110] in 15s, return to the original As flux that gave you the 2x on the [110]. In the third step gradually reduce the As flux from the start value toward the value you found and watch the RHEED pattern evolve. Double check the As flux you believe gives you a 4x on the [110] is reproducible and get familiar with the process.

Finally set the substrate rotation to around 0.2 revolutions per second and perform the third step again. The As flux required to create the 4x on the [110] azimuth may be a little different this time. With the rotation on you will see the 2x on the [-110] azimuth for the first time. Take a closer look at the reconstructions in Figure 1d.

The dynamic 4x you get when you are Ga rich is much sharper than the dynamic 4x you get in Figure 1b. This is because that whilst the Ga breaks up the As-rich (2×4), the Ga only ever improves the Ga-rich (4×2). Hence the dynamic 4x of Figure 1d is similar to the static 4x in Figure 1a. Note too that the 2x in Figure 1d is very different. There exist some extra bright spots at the bottom of the image that are much dimmer in the 2x of Figure 1a and cannot be seen in Figure 1b.

Hopefully you are now familiar with the process and can readily ascertain the maximum As flux required to create a (4×2) reconstruction in 15s. This is called the “1 to 1” point. The point at which the As flux is approximately equal the Ga flux. You could argue that the Ga flux is slightly higher than the As flux, since the surface turns Ga rich; however they are approximately equal. More importantly this transition is very repeatable. You need to make sure you always do the test in the same way. i.e. you must always wait 15s and always do the test at this temperature. Otherwise the flux will vary from check to check. It is worthwhile observing that variation yourself.

Once you have found this point you can calculate your fluxes in the system independent units of atoms/nm2/s (see Flux determination post) and state the atomic fluxes in any journal articles you write.

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4 thoughts on “How to grow your first sample: (2×4)/(4×2) transition 

  1. Pingback: Little known MBE facts: Flux determinationmy (2×4)/(4×2) | Dr. Faebian Bastiman

  2. Pingback: Little known MBE facts: MBE crystal growth optimisation | Dr. Faebian Bastiman

    • Centred (American: Centered), referring to how the reconstruction is “centred” on the underlying lattice. In zinc blende this means rotated 45° with respect to a non-centred reconstruction.

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