Week+of+7-23+to++7-27

7-23-12 I mounted a gold sample on the sample holder and waited for Matt to come in to calibrate the scope. I annealed a sample. We will keep it in solution for about 40 minutes while we make sure everything works. I made a solution by taking a pipette and dipping it in some Octanethiol. I used that Octanethiol that was stuck in the end from hydrostatic pressure and rinsed the pipette out with ethanol into a vile. I then filled the vile halfway with Ethanol and placed the gold in the solution. We scanned for a bit then I prepared the new sample holder with the ceramic material and the resistor. I cut two wires about 4 feet each and connected one end to a banana clip. The other end was crimp connected to the resistor. It will go from inside of the scope's box to the power supply to allow for minimal movement. I annealed another sample and placed it in a solution that Matt made. 7-24-12 I came in and began working with an old sample. On my first heating attempt with the new system, I used half the possible resistance and turned the system on for about 20 seconds. Images "AE" and "AF" showed similar regions. 7-24-12AE There is not much to this image. There are several large pits. No surface details are clear here. 7-24-12AF We had tried moving the scanning region to avoid the pits in the lower region and in the left middle. There is not much to this image either. The step edges are fairly well-defined but there is no clear display of surface molecules here. We tried heating the next image, "AG", for 5 seconds at full power. The tip crashed so we retracted it then changed it. 7-24-12AG This image is simply a re-scan of the one from before. The next image, "AH", drifted near the end and seemed to have a double tip for the first half. 7-24-12AH There was a lot of drift in this image near the end and a lot of junk was present in the lower half of this image. The step edges in the upper half of this image are not vey well-defined. There also looks like there is a double tip here. "AI" was slightly better. There no longer appeared to be a double tip. We hit it with the heat at full power for 5 seconds and the tip crashed. We let it sit for a short while. 7-24-12AI This image was much better than the previous. There wasn't a great deal of junk like in the last one and there was no longer a double tip. The step edges also look to be slightly more distinct. We took an image after,"AK", to show what happened. It was only a partial image though. 7-24-12AK

This image has many features under the general haze that covers the whole of the image. There are streaks throughout and noise covers the craters in the surface.

After this, I went to check the temperature of the resistor after 5 seconds and then 10 seconds. I placed the thermocouple directly under the resistor. I ran three trials. Time: 5 Seconds After turning the power supply off, the resistor would often peak at around 50 degrees Celsius for all three tests. Time: 10 Seconds The first test peaked at about 80 degrees Celsius, while the other two peaked at 72 degrees Celsius. After lunch, I got the new sample and began scanning with it and with everything connected. AM-3000 Angstroms Unfortunately, this is one of the BEST images I have ever gotten, comparative with those from June 28, 2011. This is unfortunate because the heating system was not in place for this image.The black streaks are caused by Octanethiol molecules on the surface forming a monolayer. They are very clear here and show their chain-like structure. AN- 3000 Angstroms This image occurred after I took the sample out of the box and mounted it on the sample holder designed for heating. Not much is visible here besides noise and streaks. There was a lot of drift in this image which forced me to stop taking it. AO- 3000 Angstroms This image is not much better than the one before. It is blurry because of the quality of the tip and most likely the A/D gain was probably too low. Unfortunately, I did not take note of that whilst scanning, though I assume it was either 8 or 4 when it should've been 16 or 32. It drifted near the end, which is why I had to stop taking this image. There are some very faint craters underneath the general haze, though not much can be gained from their presence. AP- 1000 Angstorms This image is very blurry, filled with streaks, and small bits of junk across the surface. No surface molecules are clearly present here and there are not any characteristics typical to Gold surfaces here such as smaller craters and mounds. The step edges here are poorly defined. It is unclear where exactly one ends and the next begins.
 * Test || Starting Temperature(Celsius) || Final Temperature(Celsius) ||
 * 1 || 27.5 || 34.2 ||
 * 2 || 26.5 || 40.7 ||
 * 3 || 27.5 || 43.8 ||
 * Test || Starting Temperature(Celsius) || Final Temperature(Celsius) ||
 * 1 || 27.5 || 68.4 ||
 * 2 || 27.5 || 63.5 ||
 * 3 || 27.5 || 62.9 ||

AQ- 3000 Angstroms The gigantic pit in the lower right quadrant shot this image's quality down the tubes. That is why I had to take a derivative plot of it. Otherwise, one would not be able to see barely anything, which would not be much worse than this image's current quality. There are no clear molecules on this surface but some of the step edges here are somewhat discrete, while others are very unclear.

AR- 3000 Angstroms. This image is horrible. The two huge pits on both sides. Nothing in the lower two-thirds is visible. There are some craters in the upper right corner but they are obscured by the noise caused by the two huge pits and most likely the poor tip.

7-25-12 I got the new sample of gold out of the heating block that Matt had placed in Octanethiol solution for about 40 minutes. I then began scanning with the system ready to heat. Matt suggested I scan very large areas then heat it up and scan again to look for changes in the largest areas. I took 4 scans that are 3777.80 Angstroms by 3777.80 Angstroms that fill up the scannable range of the scope. AA- Bottom left quadrant

There are several mounds in the upper right quadrant and the lower third of this image. This image is very blurry and has a lot of noise. Streaks go throughout the image. This was probably either caused by a scanning speed that was too fast. The step edges can be faintly seen under the haze of this image. AB- Upper left quadrant This image is much worse than the previous. The streaks are much more obvious here and the entire image is horribly blurry. There are a few very faint mounds on this surface but not much can be gained from them. AC- Upper right quadrant This image is much better than the previous one, but it is still pretty bad. There are more mounds in this image than the previous two images and they are somewhat clearer. However, the steps in this image are still fairly undefined and there are a great deal of streaks. AD- Lower right quadrant The streaks in this image are much more profound than in the previous one. This image also has more mounds than the previous few. The boundaries in this image are also not well-defined.

After taking all 4 images, I turned on the heating system at lowest resistance for 2 seconds. Before doing so, I also had retracted the tip six steps. I let it cool for about a minute then reapproached. AE-Bottom left after This image most nearly resembles the region in AD and AC. Craters are evident in this image, suggesting that a monolayer has indeed formed. There are still very profound streaks given by the large discontinuities in the scan. There are also many mounds on this surface. The step edges still had the same low quality definition. AF- Upper left after heating This image does not resemble any of the regions from the first four images, suggesting that the scanning region moved up and to the right in accordance with the previous scan. There are only a few craters here in the upper third of the image and quite a few mounds present. The image is mostly blurry and has a lot of streaks, indicative of a bad tip.

AG- Upper right after heating Most of this image is blurred nonsense. There are a few mounds but there are not any molecules to be seen. There are a lot of streaks and the step edges are horribly undefined. AH- Bottom right after heating. This image seems to be less defined than the one before. It looks more noisy and hazy than the previous image. There are quite a few streaks and the boundary edges are not very discrete. I changed the tip following this set. On my next set, I only managed to get through half a scan because of all the streaks. I went to change the tip and noticed that it was very loose in the tip holder and probably cause the shakiness. AI- 3939.31 Angstroms-Bottom left quadrant I am fairly confident that this image would have looked a great deal better had it not been taken with the huge crater in the bottom part. There are craters, mostly in the upper third. Streaks caused by noise cover the majority of them and they are only faintly seen. The step boundaries are much more distinct in this image than in the previous two sets. AJ- 3939.31 Angstroms- Upper left quadrant There are some fairly clear craters in the middle portion of this image. The step edges seem pretty well-defined in this derivative plot of the surface. The quality of the images decreased drastically. I finished one more image then checked the tip. AK-3939.31 Angstroms- Upper right quadrant. This image is horribly blurry. This is most likely caused by the gigantic pit running down the right side of the image. Little can be said of this image. There are many streaks and no clearly defined features or surface molecules. There are only some faint mounds that offer no real insight into the surface.

The tip was not loose, just a bad tip and a bad sample. I ended the day by annealing a new sample and preparing a solution. 7-26-12 I rinsed the sample with Ethanol then put it on the sample holder. I cut the tip and began scanning. The tip got stuck in the sample holder again so I waited for Matt to return to do anything. Matt came and checked and there was not a tip in the holder which is very good. I cut a new one and began scanning again, but now with the sample from yesterday and without the resistor. AA-1969.65 Angstroms- Lower right region of upper right quadrant This was an image of the surface when the gold sample was not on the sample holder designed to do the heating experiment. It was a fairly wonderful image. There are many clear features on this surface. despite the drift at the beginning. It would've been very interesting to see how this region would have reacted to the heat. I placed the sample on the other sample holder and began scanning. I think that the tip is fairly decent so I will attempt the heating now and change to the resistor system. AB- 1969.65 Å- Upper left of upper left quadrant. This image was very blurry. I changed the tip following it. Compared to the first image, this was a huge disappointment. Most of the problems in this image were most likely caused by the two huge pits that ran diagonally through the middle and on the left side. Also, the tip drifted near the end, further decreasing the quality of this image. There are many craters that can be seen fairly clearly both in the upper third and the lower right. However, there is noise that covers these features, rendering them inconsequential. AC- 1969.70 Å- Bottom right of bottom right quadrant. The large pit that runs diagonally through the center of this image obscures a lot of this image. There are only a couple of mounds and they are ill-defined, just like the step edges in this image. This was an incredibly blurry image and I decided I would change the tip after it. When I attempted this though, I thought I got the tip stuck inside the tip holder and so I had to wait until Matt got back from a conference to do anything to prevent another fracture of the piezoelectric stack. There was not really much to the image. It was an old sample and not a very good tip. I annealed a new piece of gold for the next day. 7-27-12 I took the sample off the heating block and let it cool for 7 minutes. I rinsed it with ethanol 5 times, back and front. Then, I began scanning. I took the largest regions possible at 7853.50 Å and at 400 ms/line. AA- First before image. I fixed the offset and scanned the same region again. This image was very strange. It was blurry and appeared to have a double tip. There are not any clear features here and there are a lot of streaks. The step edges are poorly defined. This image provides no insight into the surface of the gold and the molecules. AB-Second before image. My next attempt was a different area so I once more adjusted the offset. This image does not look much different from the previous image. It looks mostly just like the previous image moved down. AC- This turned out to be the same region as AB. This image is just another scan of the previous region. After, there was weird noise. I placed another washer on top of the scope and changed the tip because it was not very tightly placed. The noise was fairly reduced afterwards. AD- 7852,58 Ā- Before image This image has many features that can be faintly seen under the general haze caused by the poor quality of the tip. The step edges in this image are not very well-defined. I tried heating this image up for 5 seconds. AE- 7852.58 Å. It was a new area. I zoomed in to a region in the upper left. There ended up being too much noise. I had to tie the wires leading from the resistor around one of the poles inside the scope to reduce noise. My next scan was even worse. This image is filled with streaks and it is hard to see any features underneath all of the streaks. The boundaries here are not very distinct either. The next scan that IK attempted was even worse and by time I had tried that, it had been time for me to leave that day.