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Typical analysis of gallium obtained as a side product from the Bayer process.
Element Bayer process (ppm) After acid/base leaching (ppm) 500 zone passes (ppm)
aluminum 100-1,000 7 <1
calcium 10-100 not detected not detected
copper 100-1,000 2 <1
iron 100-1,000 7 <1
lead <2000 30 not detected
magnesium 10-100 1 not detected
mercury 10-100 not detected not detected
nickel 10-100 not detected not detected
silicon 10-100 ≈ 1 not detected
tin 10-100 ≈ 1 not detected
titanium 10-100 1 <1
zinc 30,000 ≈ 1 not detected
Schematic representation of a zone refining apparatus.

Isolation and purification of elemental arsenic

Elemental arsenic (L. arsenicum, yellow orpiment) exists in two forms: yellow (cubic, As 4 ) and gray or metallic (rhombohedral). At a natural abundance of 1.8 ppm arsenic is relatively rare, however, this is offset by its presence in a number of common minerals and the relative ease of isolation. Arsenic containing minerals are grouped into three main classes: the sulfides realgar (As 4 S 4 ) and orpiment (As 2 S 3 ), the oxide arsenolite (As 2 O 3 ), and the arsenides and sulfaresenides of the iron, cobalt, and nickel. Minerals in this latter class include: loellinginite (FeAs 2 ), safforlite (CoAs), niccolite (NiAs), rammelsbergite (NiAs 2 ), ansenopyrite or mispickel (FeAsS), cobaltite (CoAsS), enargite (Cu 3 AsS 4 ), gerdsorfite (NiAsS), and the quarturnary sulfide glaucodot [(Co,Fe)AsS]. [link] shows the typical impurities in arsenopyrite.

Typical impurities in arsenopyrite.
Element Concentration (ppm) Element Concentration (ppm)
silver 90 nickel <3,000
gold 8 lead 50
cobalt 30,000 platinum 0.4
copper 200 rhenium 50
germanium 30 selenium 50
manganese 3,000 vanadium 300
molybdenum 60 zinc 400

Arsenic is obtained commercially by smelting either FeAs 2 or FeAsS at 650-700 °C in the absence of air and condensing the sublimed element (T sub = 613 °C), [link] .

The arsenic thus obtained is combined with lead and then sublimed (T sub = 614 °C) which binds any sulfur impurities more strongly than arsenic. Any residual arsenic that remains trapped in the iron sulfide is separated by forming the oxide (As 2 O 3 ) by roasting the sulfide in air. The oxide is sublimed into the flue system during roasting from where it is collected and reduced with charcoal at 700-800 °C to give elemental arsenic. Semiconductor grade arsenic (>99.9999%) is formed by zone refining.

Synthesis and purification of gallium arsenide.

Gallium arsenide can be prepared by the direct reaction of the elements, [link] . However, while conceptually simple the synthesis of GaAs is complicated by the different vapor pressures of the reagents and the highly exothermic nature of the reaction. Furthermore, since the synthesis of GaAs at atmospheric pressure is accompanied by its simultaneous decomposes due to the loss by sublimation, of arsenic, the synthesis must be carried out under an overpressure of arsenic in order to maintain a stoichiometric composition of the synthesized GaAs.

In order to overcome the problems associated with arsenic loss, the reaction is usually carried out in a sealed reaction tube. However, if a stoichiometric quantity of arsenic is used in the reaction a constant temperature of 1238 °C must be employed in order to maintain the desired arsenic overpressure of 1 atm. Practically, it is easier to use a large excess of arsenic heated to a lower temperature. In this situation the pressure in the tube is approximately equal to the equilibrium vapor pressure of the volatile component (arsenic) at the lower temperature. Thus, an over pressure of 1 atm arsenic may be maintained if within a sealed tube elemental arsenic is heated to 600-620 °C while the GaAs is maintained at 1240-1250 °C.

[link] shows the sealed tube configuration that is typically used for the synthesis of GaAs. The tube is heated within a two-zone furnace. The boats holding the reactants are usually made of quartz, however, graphite is also used since the latter has a closer thermal expansion match to the GaAs product. If higher purity is required then pyrolytic boron nitride (PBN) is used. One of the boats is loaded with pure gallium the other with arsenic. A plug of quartz wool may be placed between the boats to act as a diffuser. The tube is then evacuated and sealed. Once brought to the correct reaction temperatures ( [link] ), the arsenic vapor is transported to the gallium, and they react to form GaAs in a controlled manner. [link] gives the typical impurity concentrations found in polycrystalline GaAs.

Schematic representation of a sealed tube synthesis of GaAs.
Impurity concentrations found in polycrystalline GaAs.
Element Concentration (ppm) Element Concentration (ppm)
boron 0.1 silicon 0.02
carbon 0.7 phosphorus 0.1
nitrogen 0.1 sulfur 0.01
oxygen 0.5 chlorine 0.08
fluorine 0.2 nickel 0.04
magnesium 0.02 copper 0.01
aluminum 0.02 zinc 0.05

Polycrystalline GaAs, formed in from the direct reaction of the elements is often used as the starting material for single crystal growth via Bridgeman or Czochralski crystal growth. It is also possible to prepare single crystals of GaAs directly from the elements using in-situ, or direct, compounding within a high-pressure liquid encapsulated Czochralski (HPLEC) technique.

Bibliography

  • K. G. Baraclough, K. G., in The Chemistry of the Semiconductor Industry , Eds. S. J. Moss and A. Ledwith, Blackie and Sons, Glasgow, Scotland (1987).
  • L. D. Crossman and J. A. Baker, Semiconductor Silicon 1977 , Electrochem. Soc., Princeton, New Jersey (1977).
  • M. Fleisher, in Economic Geology, 50th Aniv. Vol. , The Economic Geology Publishing Company, Lancaster, PA (1955).
  • G. Hsu, N. Rohatgi, and J. Houseman, AIChE J. , 1987, 33 , 784.
  • S. K. Iya, R. N. Flagella, and F. S. Dipaolo, J. Electrochem. Soc. , 1982, 129 , 1531.
  • J. Krauskopf, J. D. Meyer, B. Wiedemann, M. Waldschmidt, K. Bethge, G. Wolf, and W. Schültze, 5th Conference on Semi-insulating III-V Materials, Malmo, Sweden, 1988, Eds. G. Grossman and L. Ledebo, Adam-Hilger, New York (1988).
  • J. R. McCormic, Conf. Rec. 14th IEEE Photovolt. Specialists Conf., San Diego, CA (1980).
  • J. R. McCormic, in Semiconductor Silicon 1981 , Ed. H. R. Huff, Electrochemical Society, Princeton, New Jersey (1981).
  • W. C. O’Mara, Ed. Handbook of Semiconductor Silicon Technology , Noyes Pub., New Jersey (1990).
  • W. G. Pfann, Zone Melting , John Wiley&Sons, New York, (1966).
  • F. Shimura, Semiconductor Silicon Crystal Technology , Academic Press (1989).

Questions & Answers

how to know photocatalytic properties of tio2 nanoparticles...what to do now
Akash Reply
it is a goid question and i want to know the answer as well
Maciej
Do somebody tell me a best nano engineering book for beginners?
s. Reply
what is fullerene does it is used to make bukky balls
Devang Reply
are you nano engineer ?
s.
fullerene is a bucky ball aka Carbon 60 molecule. It was name by the architect Fuller. He design the geodesic dome. it resembles a soccer ball.
Tarell
what is the actual application of fullerenes nowadays?
Damian
That is a great question Damian. best way to answer that question is to Google it. there are hundreds of applications for buck minister fullerenes, from medical to aerospace. you can also find plenty of research papers that will give you great detail on the potential applications of fullerenes.
Tarell
what is the Synthesis, properties,and applications of carbon nano chemistry
Abhijith Reply
Mostly, they use nano carbon for electronics and for materials to be strengthened.
Virgil
is Bucky paper clear?
CYNTHIA
so some one know about replacing silicon atom with phosphorous in semiconductors device?
s. Reply
Yeah, it is a pain to say the least. You basically have to heat the substarte up to around 1000 degrees celcius then pass phosphene gas over top of it, which is explosive and toxic by the way, under very low pressure.
Harper
Do you know which machine is used to that process?
s.
how to fabricate graphene ink ?
SUYASH Reply
for screen printed electrodes ?
SUYASH
What is lattice structure?
s. Reply
of graphene you mean?
Ebrahim
or in general
Ebrahim
in general
s.
Graphene has a hexagonal structure
tahir
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Sanket Reply
what's the easiest and fastest way to the synthesize AgNP?
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Cied
types of nano material
abeetha Reply
I start with an easy one. carbon nanotubes woven into a long filament like a string
Porter
many many of nanotubes
Porter
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Yasmin
what is the function of carbon nanotubes?
Cesar
I'm interested in nanotube
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what is system testing?
AMJAD
preparation of nanomaterial
Victor Reply
Yes, Nanotechnology has a very fast field of applications and their is always something new to do with it...
Himanshu Reply
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AMJAD
what is system testing
AMJAD
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Stotaw
In this morden time nanotechnology used in many field . 1-Electronics-manufacturad IC ,RAM,MRAM,solar panel etc 2-Helth and Medical-Nanomedicine,Drug Dilivery for cancer treatment etc 3- Atomobile -MEMS, Coating on car etc. and may other field for details you can check at Google
Azam
anybody can imagine what will be happen after 100 years from now in nano tech world
Prasenjit
after 100 year this will be not nanotechnology maybe this technology name will be change . maybe aftet 100 year . we work on electron lable practically about its properties and behaviour by the different instruments
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name doesn't matter , whatever it will be change... I'm taking about effect on circumstances of the microscopic world
Prasenjit
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silver nanoparticles could handle the job?
Damian
not now but maybe in future only AgNP maybe any other nanomaterials
Azam
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I'm interested in Nanotube
Uday
this technology will not going on for the long time , so I'm thinking about femtotechnology 10^-15
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how did you get the value of 2000N.What calculations are needed to arrive at it
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Source:  OpenStax, Chemistry of electronic materials. OpenStax CNX. Aug 09, 2011 Download for free at http://cnx.org/content/col10719/1.9
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