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Making High-Temperature Superconductors

What follows are the instructions for making ceramic superconductors in a high school science laboratory. These
were originally the instructions that were included in a Colorado Futurescience kit for superconductor fabrication.
We have not sold the fabrication kit for many years, so we decided to put these instructions on the web site.

Since we're making this information available without charge, we can assume no liability for the safety or
reliability of the procedure.

This procedure was originally written in 1988 for high school science labs; but, of course, it can also be used at
colleges and in other settings. Individuals unaffiliated with any research laboratory or educational institution have
also used this procedure successfully. Unaffiliated individuals, however, may have difficulty obtaining the
required chemicals. None of the major suppliers of research chemicals will sell chemicals to individuals.
Colorado Futurescience no longer exists. Futurescience, LLC also no longer regularly sells these chemicals,
although we are willing to discuss making some of the necessary materials available on a custom-made basis to
universities and to qualified high school science teachers. We have put together custom kits with some of the
harder-to-obtain materials for schools. For the unaffiliated individual with a scientific background, one option for
making these superconductors is to volunteer to assist a High School Science Department with this project. Many
schools are in need of qualified volunteers to assist with science projects.

Making yttrium-barium-copper-oxide superconductors requires the following items:

Yttrium Oxide
Barium Carbonate
Cupric Oxide
A Laboratory Furnace such as a Thermolyne Muffle Furnace or a converted pottery kiln.
Labware made of alumina. The recommended labware is the 20 ml. CD-20 alumina dish made by Coors
Ceramics.
An Oxygen Source
Liquid Nitrogen and a rare-earth magnet for testing and demonstrating the superconductors

(See the listing of sources of equipment and supplies for making superconductors.)

Important Safety Note: Barium Carbonate is a toxic substance. It can be safely handled with ordinary
laboratory procedures. It is imperative, however, that (especially during the grinding and mixing of the
chemicals) a good-quality dust mask is worn during the procedure. It is also important to wear laboratory
gloves, such as disposable latex surgical gloves, while working with these chemicals.

The process described here may appear rather formidable at first, but it is actually straightforward and typical of
ceramic processes often used in scientific research. The most time-consuming part of the process is gathering the
necessary materials and equipment, since the materials and equipment are uncommon in a high school laboratory
where experiments with ceramic materials are rare.

There are a number of methods of preparing yttrium-barium-copper-oxide superconductors. The simplest is the
one that has become known as the "shake-and-bake" method. This involves a four step process.

1. MIXING THE CHEMICALS

2. CALCINATION (the initial firing)

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3. THE INTERMEDIATE FIRING(S) (oxygen annealings)

4. THE FINAL OXYGEN ANNEALING

Some of the details of the procedures are very flexible. The number of intermediate firings and the length of the
firings are largely up to the user. In general, the more intermediate firings, and the longer the duration of the
firings under oxygen flow, the better the superconductor. But definite signs of superconductivity can usually be
obtained without any intermediate firing at all. In fact, if the initial mixing of the chemicals is sufficiently
thorough, the intermediate firing is not necessary at all.

It is recommended that no more than half of your chemicals fired at a time so that all of your chemicals will not be
ruined if there is a problem during a firing. The most common problem encountered is overheating due to errors in
the pyrometer on the furnace. It is strongly recommended that the calibration of your temperature indicator be
checked before the first firing. If there are any doubts about the accuracy of your temperature indicator, an
inexpensive pyrometric cone can be obtained from a pottery shop for a reasonably good calibration check. See the
section of the instructions on pyrometric cones.

See Using a Pottery Kiln as a Laboratory Furnace and Using Pyrometric Cones to Calibrate Furnace Temperature
Indicators.

1. MIXING THE CHEMICALS. The starting mix is a gray powder formed by thoroughly mixing yttrium oxide,
barium carbonate, and cupric oxide. There are a number of workable methods of mixing the powders. The
recommended procedure for modestly equipped laboratories is to first use a mortar and pestle to grind down any
lumps or large particles in the chemical powders, then to shake the mix vigorously in a capped jar or stoppered
flask for several minutes. The ultimate purpose of this entire process is to combine the starting compounds at the
molecular level. A really thorough dry mixing of chemicals is a difficult process, but taking extra time and work
during the initial dry mixing process will pay off later. (Mixing in a sealed plastic bag is also a workable mixing
method, especially if your starting chemical are lumpy, but it is best to shake them thoroughly in a jar at the end of
your mixing process.) Use a dust mask and avoid breathing any of the chemical powders. The chemicals
must be mixed in the proper proportions so that the atomic ratios of yttrium, barium, and copper are 1:2:3. (For an
explanation of how this is done, see the section on molecular weights.) The proper weight ratios are:

Yttrium Oxide, Y 2O3 11.29 grams

An important note about temperatures: The furnace temperatures stated here are temperatures as they are
usually measured on the temperature indicator of the furnace. In most cases, the temperature sensor is located
slightly higher in the furnace chamber than the sample you are firing. Therefore, the indicated temperature will
often be a few degrees higher than the actual temperature of the material. If the temperature sensor in your furnace
is at the same level as the material being fired, the maximum indicated temperature should never be allowed to
exceed 980 degrees Celsius.

2. CALCINATION. For the initial heat treatment, called calcination, the mix is heated at 925-950 degrees
Celsius for about 18-24 hours. (The 950 degree temperature works much better if this is within the rating of your
furnace for continuous use.) This first treatment may be done a crucible or evaporating dish made of alumina or of
a good grade of laboratory porcelain. It is best to use alumina unless you have a particular reason for using
ordinary porcelain labware. This first heat treatment forms the basic crystal structure of YBa 2Cu3O6.5, and gets
rid of the carbon dioxide from the barium carbonate. (Barium carbonate is used instead of barium oxide because
barium oxide of any reasonable purity is difficult to obtain. Also, exposing barium oxide to air tends to quickly
convert much of it to barium carbonate and barium hydroxide.)

The result of this first firing is a porous black or very dark gray clump. The coloration should be fairly even. An
uneven green coloration is an indication that the powders are not as thoroughly mixed as they should have been,

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and that extra time and care should be taken to insure thorough grinding and mixing on subsequent steps. The
material will seem to shrink rather dramatically during the initial firing as it loses its carbon dioxide and becomes
much denser than the original powder mix.

3. INTERMEDIATE FIRING(S). The porous black clump is ground into a fine powder and placed in the
furnace in an alumina dish. A final furnace temperature of 925 to 975 degrees Celsius is recommended for the
intermediate firings. A temperature much higher than this will result in a material that is much harder to re-grind.
Temperatures above 1000 degrees Celsius may destroy the crystal structure.

After the mix has heated in the furnace for at least 18 hours at 925-975 degrees Celsius, begin a slow flow of
oxygen into the furnace, and reduce the temperature slowly. If you plan to test the sample for superconductivity
after this firing, the cooling rate must be no more than 100 degrees per hour until 400 degrees Celsius is reached.
The rate of cooling from 400 degrees down to room temperature can be increased to about 200 degrees per hour.
If you do not plan to test for superconductivity after this firing, a cooling rate in excess of 100 degrees per hour
may be used; however a cooling rate in excess of 250 degrees per hour is not recommended. Do not remove the
oxygen flow until the indicated furnace temperature has fallen below 400 degrees Celsius.

The material should be thoroughly re-ground in a mortar and pestle (or similar device) between each firing. (If,
after an intermediate firing, there is some green coloration in the resultant disk, it is important to take extra time
and care in re-grinding and mixing the material before the next firing.)

Problems that occur in the mixing and grinding process in any of these steps are often due to hard, coarse particles
being mixed in with the finely powder material. An ordinary kitchen tea strainer can come in handy at this point to
separate the coarser particles or lumps so they may be ground separately. IMPORTANT: If you an ordinary tea
strainer, make sure it is made of a non-magnetic material, or make sure you are satisfied that none of the material
in the sifter or strainer will contaminate the chemicals. Even very small quantities of magnetic materials in the
chemical mix can diminish or destroy the potential superconductivity. (It is also for this reason that "ceramic
grade" chemicals, which tend to have iron impurities, are not often usable for making superconductors.) Shortcuts
in grinding the materials, such as using an electric coffee grinder, often contaminate the compound with elements
that destroy the superconducting properties. Some contaminates will destroy superconductivity in very tiny
amounts. To keep your chances of success high, grinding with a good-quality mortar and pestle is the best method.
This manual grinding can be an arduous process, but the results are worth the trouble.

4. THE FINAL OXYGEN ANNEALING. The sample should be thoroughly reground, and the resultant black
powder placed back in the alumina dish. The thickness of the layer of loose powder in the dish should match the
desired thickness of the final superconducting disk. For this final firing, the powder should be as finely-ground
and as densely-packed as possible. Do NOT pack the powder into the dish by pressing on it from the top (as this
can makes the superconductor tend to stick to the alumina dish). Better results can usually be obtained by tapping
the alumina dish with a pestle or a similar object so that the particles of the mix settle together in an evenly packed
disk.

For this final heat treatment, heat the sample to between 950 degrees and 1000 degrees Celsius for about 18 hours.
The higher temperature is better, but be sure of the accuracy of your temperature indicator before getting too
close to 1000 degrees. Temperatures much above 1000 degrees risk decomposition of the crystal structure and the
possibility of the material sticking to the alumina dish. On the other hand, a final oxygen annealing at an indicated
temperature of 950 degrees Celsius may yield a superconductor that will crack easily, but will otherwise be
satisfactory.

Very Important: It is absolutely necessary that the cool-down take place very slowly and under adequate oxygen
flow. The rate of cooling must be no more than 100 degrees Celsius per hour, especially during the critical
temperature region between 750 and 400 degrees Celsius. Take special care to insure that the sample has access to
plenty of oxygen, especially in during the cool-down from 900 to 300 degrees. Brief interruptions in oxygen flow
when the material is above 900 are unimportant, but continuous flow must be maintained during cool-down. If the
atmosphere in the furnace is not oxygen-rich while the sample is still above about 400 degrees, the material can

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lose vital oxygen from its crystal structure. After the furnace temperature reaches about 500 degrees, the rate of
cooling can be increased. (Often, a good superconductor can be made by using oxygen flow only during the
cool-down period.)

During this final heat treatment, before the final cool-down begins, a superconductor that is more resistant to
cracking during thermal stress can be produced by subjecting the sample to high-temperature thermal cycling. To
do this, vary the temperature between about 750 and 980 degrees at rates of change of about 200 per hour. Then
raise the temperature to about 980 degrees for an hour or more before beginning the final slow cool-down. This
thermal cycling is not a necessity at all. In fact, if you started with a powder with fine particles of about the
same size, this thermal cycling is not even very useful. For many manually-ground powders, though, it will add
significantly to the mechanical strength of the sample.

Additional hints and notes:

HEAT-UP TIME

The rate of heating is not nearly as critical for the material as the rate of cooling. However, it is best not to exceed
300 degrees per hour in order to avoid thermal stress cracks in the labware. The manufacturers of laboratory
alumina recommend not exceeding 150 per hour, but we have not experienced problems with faster heating rates.

COOL-DOWN TIME

The cool-down time during the oxygen annealing is very critical for making these superconductors. If the rate of
cooling is not strictly limited to less than 100 degrees per hour until the sample is below 500 degrees, the sample
will probably not superconduct at liquid nitrogen temperatures. It is especially important to drop the temperature
very slowly through the 750 to 500 degree region. There is evidence that much slower rates of cooling through
this temperature range will produce an even better superconductor.

After the sample reaches a the 400 to 500 degree range, the rate of cooling can be increased. The furnace may be
opened and the sample removed from the furnace whenever the temperature falls below 200 degrees, and you
believe that you can safely handle the hot sample.

OXYGEN

Various types of oxygen supplies may be used as the source of the oxygen flow through the furnace. One option is
to use an acetylene torch setup with the acetylene tank removed. The oxygen control on the torch provides an
additional means of regulating oxygen flow. The tip can be removed from the torch, and plastic tubing clamped
over the open end of the torch. We have also used medical oxygen bottles for the oxygen supply. The oxygen
source is often the greatest problem in making these superconductors in a modestly-equipped laboratory, but there
are a large number of options to choose from. It is difficult to give exact instructions on the oxygen setup, since
this will depend upon what type of oxygen source is most easily accessible to each individual user. Oxygen is
necessary only during the cool-down, and only a very slow flow of oxygen is needed.

The superconducting material can gain or lose oxygen easily when the material is above about 400 degrees
Celsius. Therefore, it is especially important to keep the sample in contact with plenty of oxygen during the
cool-down. Otherwise, it may lose much of the oxygen it has acquired. This material is an exceptionally good
oxygen ion conductor. The amount of oxygen that the superconductor absorbs is likely to be the main factor that
determines the quality of your superconductor.

In most inexpensive furnaces, it is necessary to provide a rate of oxygen flow to the furnace chamber that actually
wastes a considerable amount of oxygen. But considering the relatively low cost of oxygen, this is usually more
economical than the alternatives. If you have a fairly air-tight furnace, the rate of oxygen flow need not be more
than a few milliliters per minute. Unfortunately, most inexpensive furnaces are not very airtight; and the more
easily-available oxygen regulators are not capable of regulating at very low flow-rates.

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If it appears that you may run out of oxygen before the firing is completed, turn off the oxygen flow intermittently
while the sample is in the still above 900 degrees. This material will regain any lost oxygen quickly while at high
temperature, but adequate oxygen during the cool-down is vital. If you run out of oxygen during cool-down, the
material may not superconduct at liquid nitrogen temperatures.

Unless you have a fairly sophisticated oxygen and furnace system, the best regulator setting for your first attempt
at making superconductor is usually about:

1 liter/minute on a medical oxygen tank

These settings will use a considerable amount of oxygen during the oxygen annealings, but it is the least expensive
alternative unless you are going to be making more than just a few superconductors. Regulator settings of one-half
of these values will provide more than adequate oxygen flow, but extremely low settings are difficult to maintain
on ordinary regulators without constant human attention.

The best method of getting oxygen flow to the interior of your furnace will depend upon what type of furnace you
have. Many laboratory furnaces, such as Thermolyne muffle furnaces, are easily modified for oxygen flow by
drilling a hole in the back of the furnace, just below the thermocouple. If your furnace manual includes
instructions for adding an additional thermocouple to your furnace, those instructions can be used as a guide for
adding a clay pipestem to the back of the furnace. A clay pipestem for this purpose can be obtained by
disassembling an ordinary pipestem triangle such as those often used for heating crucibles over a flame.

For Thermolyne muffle furnaces such as the model 1300, first remove the metal plate from the rear of the furnace
(by removing four screws and carefully sliding out the thermocouple). Drill a 3/8" (10 mm.) hole in the metal
plate about an inch below the hole for the thermocouple.

Re-assemble the furnace, and use the newly-drilled hole as a guide for drilling a 3/8" (10 mm.) hole about an inch
into the refractory material. Be very gentle in drilling into the refractory material, as this material is very soft. If
you're not careful, you can drill all the way into the furnace chamber in a fraction of a second. You now have a
hole that the supplied clay pipestem will slide into.

The next step is to use a 1/8" (3 mm.) drill bit to drill a hole the remaining distance into the furnace chamber.
Oxygen can flow through the hole in the clay pipestem, then through this 1/8" (3 mm.) hole, and into the furnace
chamber.

Plastic tubing may be used to connect your oxygen tank to the clay pipestem on the back of your furnace.

If you plan on making a lot of superconductors, you may want to fit your clay pipestem on the inside of the metal
back of the furnace. This requires drilling the 3/8" (10 mm.) hole in the refractory material to a depth equal to the
distance from the center of the clay pipestem to one end of the pipestem.

If you are using a pottery kiln for firing the superconductors, you can feed oxygen into the chamber through one of
the viewing holes. One way of doing this is to fit the clay pipestem into the ceramic plug that is used to plug the
viewing holes in the kiln. This can be done by carefully drilling the appropriate size hole in the ceramic plug. The
clay pipestem can be mounted securely in the hole with high-temperature cement such as muffler cement. If you
are doing the superconductor project in a school with an art department that teaches pottery, you may be able to
persuade the pottery class to make a custom plug for feeding oxygen into the chamber.

CARE OF ALUMINA LABWARE:

The alumina dish may become stained with black superconductor after a few firings. It may be restored to

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like-new condition by soaking it overnight in dilute (10 percent) hydrochloric acid. (To avoid corrosive
hydrochloric acid fumes from oxidizing objects in the room, make sure that even diluted hydrochloric acid
solutions are not left uncovered.) To avoid a situation where the superconductor tends to stick to the alumina dish,
do not pack the powder into the dish before firing. Leave the powder lying loose. Also monitor the temperature
carefully during firing to avoid overheating the material.

PELLETIZING:

In most laboratory preparations of these superconductors, the superconducting powder is pressed into pellets or
disks before the final oxygen annealing. If you have the proper equipment, you may wish to press the
superconductors into pellets or disks. This has definite advantages over just sintering the loose powder. In order
to make pellets of this material that are solid enough to handle until you get to a furnace, add a small amount of
distilled water to the powder before pressing, and mix in the distilled water in a mortar and pestle.

EVEN BETTER SUPERCONDUCTORS

The current-carrying capacity, and the ability of these superconductors to levitate even larger magnets, may be
increased by various methods.

In general, the more often you repeat the re-grinding and oxygen annealing, the better the superconductor will
become. There appears to be no danger of getting too much oxygen into the superconductors using ordinary
equipment.

The use of higher temperatures will improve the quality of these superconductors. All furnaces and kilns have a
temperature gradient inside the chamber. If the sensor for the temperature indicator is high in the chamber, the
actual temperature at the bottom of the chamber may be much cooler. This is a good reason for using pottery
cones for a calibration check.

There are some potential problems when using these higher temperatures, though. The material will come out of
the furnace much harder and more difficult to re-grind. Therefore, it may be better to wait until the last firing
before using these higher temperatures. After the last firing, a harder disk is desirable.

Higher temperatures induce a risk of melting these materials, especially if your temperature indicator is inaccurate.
(These materials can be processed by melting; but that is a different process than sintering. Unintentional melting
tends to make a mess inside the furnace, and may cause the material to stick to the alumina dish.) Melting these
materials is definitely something to be avoided unless you're deliberately experimenting in this area.

The other problem with higher temperature may be the limitations of your furnace. Know the specifications of
your furnace to avoid burning out the heating elements or doing other damage. (We have operated lab furnaces
rated for maximum temperature of 925 degrees Celsius at temperatures exceeding 1000 degrees Celsius for
extended periods and still had the heating elements and thermocouples last for years. But remember that you
exceed the manufacturer's specifications at your own risk.)

Oxygen annealing for longer firing periods will also improve the superconductors. Intermediate grindings,
however, are important since the ultimate goal is to mix the constituent chemicals at the molecular level.

Grinding the material to a very fine powder is especially important just prior to the final annealing. If the material
is very finely ground, tapping the alumina dish with a pestle will reduce the porosity of the material and help to
compensate for not pelletizing the material in a powerful press. It is possible to overdo the grinding, though. If an
electric grinder is used, then the material is pressed into a pellet at high pressure, it can become difficult for oxygen
to penetrate into the material.

There are indications that moisture will slowly destroy the superconductivity of this material. For this reason,
some people suggest coating the finished superconductor with a clear spray-on coating or varnish. However, such
a coating makes it impossible to re-fire the superconductor after re-grinding (as you may want to do if it should

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break). Therefore, we recommend storing the finished superconductors in a sealed plastic bag with a small bag of
desiccant to absorb moisture from the air.

TESTING THE SUPERCONDUCTORS

The most foolproof test for superconductivity is the simplest. This is the test for diamagnetism using small rare
earth magnets made of samarium-cobalt or neodymium-iron-boron. Use a very small rare-earth magnet at first.
Start with a rare-earth disk magnet about 6 mm. in diameter. If you have made a good-quality superconductor, the
magnet will levitate at least 3 mm. above the surface of the superconducting disk. When cooling the disk with
liquid nitrogen, cool the disk slowly by first pouring the cold gas on the disk. (You can "see" the cold nitrogen gas
above the liquid nitrogen because of the moisture it condenses from the air.) When you begin adding the liquid
nitrogen, add only a few drops at first. Wait at least a minute after you first begin chilling the disk before you
cover the entire disk with liquid nitrogen.

If the disk does crack, each piece will still superconduct. If desired, you can re-grind the broken pieces and fire
them in the furnace to put them back into one piece again. This repair job is identical to the last oxygen
annealing. Be sure to supply plenty of oxygen to the furnace chamber during cool-down, though. The oxygen
supply on a re-fire is just as important as the earlier firing.

If you want to try an even more spectacular demonstration of diamagnetism, you can obtain a larger rare-earth
magnet to see if your superconductor will levitate it. (Some rare-earth magnets may still be available from
Futurescience, LLC.) Neodymium-iron-boron magnets are usually more economical than samarium-cobalt
magnets. The larger magnets provide a good test of the quality of your superconductor. With superconductors
made with the techniques described here, we have levitated 1" neodymium bar magnets and 1/2" neodymium disk
magnets, sometimes getting a levitation that was barely noticeable, and other times getting a levitation that was
quite spectacular. A superconductor with poor levitation can usually be improved by re-grinding it a giving it an
additional oxygen annealing.

When a superconductor levitates a magnet, a magnetic mirror image is formed in the superconductor of the
levitating magnet. The magnetic mirror image insures that there is always a north pole induced in the
superconductor directly below the north pole of the levitating magnet. There is a south pole induced in the
superconductor directly below the south pole of the levitating magnet. This mirror image moves with the magnet
as the magnet is moves, so that the disk magnet can be given a rapid spin without affecting its levitation. In fact
the magnet may continue to spin for quite a long time because its spinning encounters no friction other than the
friction of air resistance.

The diamagnetism of the superconductor tends to get stronger as the temperature decreases. One way to decrease
the temperature is to decrease the air pressure around the liquid nitrogen cooling the superconductor. Decreased
air pressure reduces the boiling point of liquid nitrogen. If you place the superconductor and liquid nitrogen in a
bell jar and pump some of the air out, you may see the levitating magnet rise higher (although a very cold bell jar
tends to accumulate a layer of frost).

ADDITIONAL READING (from the earlier days of High-Temperature Superconductors):

Magazine articles:

"Superconductivity seen above the boiling point of nitrogen," Physics Today, pp. 17-23. April, 1987.

"Superconductors," Business Week, pp. 94-100. April 6, 1987

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"Superconductors," TIME, pp. 64-75. May 11, 1987

(various articles), Insight (Washington Times), pp.8-17. May 25, 1987.

"Superconducting", High Technology, pp. 12-18. July, 1987.

"High Tc May Not Need Phonons; Supercurrents Increase," Physics Today, pp. 17-21. July, 1987.

"Do-It-Yourself Superconductors," New Scientist. pp. 36-39. July 30, 1987. (An account of the experiences of the
first high school class to make superconductors.)

"Superconductivity: Hype vs. Reality," Discover. pp. 22-32. August, 1987.

"Industry Warms to Superconductivity," New Scientist. pp. 56-61. October 22, 1987.

(Various articles), Journal of Chemical Education. pp. 836-853. October, 1987.

"A Superconductivity Primer," Nature. pp. 21-24. Nov. 5, 1987.

(Also of interest is the March, 1986 issue of Physics Today, which was a special issue on superconductivity written
before the discovery of the new oxide superconductors.)

Scientific Papers:

Williams, et al. "High-Tc Superconductors: Selective Preparation and Characterization of Tetragonal and
Orthorhombic (93 K Superconductor) Phases of YBa 2Cu3Ox ," Inorganic Chemistry, 1987, 26, pp. 1834-36.

Panson, et al. "Effect of Compositional variation and Annealing in Oxygen on Superconducting Properties of
Y1Ba2Cu3Ox," Physical Review B, pp. 8774-8777, v.35, no.6, June 1, 1987.

Tarascon, et al. "Oxygen and Rare-Earth Doping of the 90-K Superconducting Perovskite YBa 2Cu3Ox ," Physical
Review B, pp. 226-234, v.36, no.1, July 1, 1987.

Barnes, R.L. and Laudise, R.A., "Stability of Superconducting YBa 2Cu3Ox in the Presence of Water," Applied
Physics Letters, pp. 1373-1375, v.57, no.17, October 26, 1987

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