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Zone Refining.
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HAuCl4
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Zone Refining.
January18th,2011,7:54pm
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Found this old paper online.

Anybody seen one of these machines up close?.
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Harold_V
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Re: Zone Refining.

January19th,2011,12:00pm
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Not likely to be found. It's generally done with an induction heating furnace. It's reputed to work well and can yield gold of high quality.
Each successive pass through the molten stage should improve the quality of the gold, assuming additional passes are needed.
Harold
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HAuCl4
ActiveMember

Re: Zone Refining.

January19th,2011,3:02pm
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In that paper, I found many interesting things:

The machine they describe melts in a vacuum, with no crucible, using electron bombardment, the list of contaminants have some
substantial contaminants that I wasn't expecting to see, etc, etc.
All in all, very different from what I had imagined the method to be. (The metal refined and discussed in the paper was platinum). Maybe

this is a for a specific application in the 70s, and more effective methods are in use?. I added all impurities and calculated the refined
platinum to be just a little better than 9999 after 3 passes. I was expecting something like 6N or more.
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HAuCl4
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Re: Zone Refining.

January21st,2011,1:27pm
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Zone Melting
a crystallophysical method of refining materials that consists in the movement of a narrow fusion zone along a long solid rod made of the
material that is being refined. Nearly all industrially important metals, semiconductors, dielectrics, and inorganic and organic compounds
more than 120 substancesmay undergo zone melting.
The first mention of the use of zone melting dates to 1927, when the method was used to purify iron. Zone melting became widely known
in 1952 as a result of the works of W. Pfann (USA), who used it to produce germanium of high purity in a special container (container zone
melting).
To perform container zone melting on a solid load placed in a container, a small melted region called a zone, which is shifted along the
load, is created. In the process crystallization of the material takes place on one surface of the interface between the solid and liquid
phases (the crystallization front), and the raw material is supplied at the other surface (the melting front). Container zone melting is used
to refine a material that does not interact with the material of which the container is made. In 1953, P. Keck and M. Golei (USA) proposed
a crucibleless method for zone melting of a vertical rod (the socalled floating zone method) for purifying semiconducting silicon. In this
method, the fusion zone is restrained mainly by the forces of surface tension; therefore, crucibleless zone melting is widely used for
refractory and active materials with sufficiently high surface tension and not very great density in liquid state (silicon, germanium,
molybdenum, tungsten, platinum, palladium, rhenium, and niobium). Since 1955 zone melting has been widely used in laboratory and plant
practice to produce pure materials with an impurity content of as little as 107109 percent (socalled zone refining), for alloying
and uniform distribution of the impurity throughout the ingot, and for growing single crystals, concentrating impurities in analytical
practice, creating highpurity standards, and studying phase diagrams.
Zone refining is based on the fact that under conditions of equilibrium between the liquid and solid phases, the solubility of the impurities
is different in the two phases. To produce pure metals the fusion zone is usually shifted through the ingot several times, or several shifting
fusion zones are created simultaneously in the ingot, with sections of solid material between them. The rate of shifting of the fusion zone
is usually 0.110.0 mm/min, and the number of passes is 1015 or more. Refining is concluded when the maximum (final) distribution of
the impurity, which cannot be changed by subsequent shifts of the zones, is attained.
The effectiveness of zone removal of impurities from a material depends on the distribution ratio of the impurity (the ratio of the
concentration of the impurity in the solid phase to the concentration in the liquid phase), the number of passes and the rate of shifting of
the zone, and the ratio of the length of the ingot to the length of the zone. Zone equalization consists in the introduction into the first
zone of an alloying additive, which is uniformly distributed throughout the ingot upon repeated shifting of the zone. Alternate motion of
the zone from the head to the tail of the ingot and back is sometimes used to achieve uniform distribution of the impurity throughout the
ingot.
Zone melting may be used simultaneously with refining and to produce single crystals; a seedthe nucleus of a single crystal, oriented in a
predetermined crystallographic directionis used for this purpose. The first fusion zone is created at the interface of the seed with the rod
that is to undergo zone melting, and part of the rod and part of the seed are fused. Thermal conditions that, upon solidification of the
liquid metal, ensure controlled crystallization of the seed in the direction induced by the seed, are created at the interface of the seed and
liquid metal phases. A special type is zone melting with a temperature gradient (a method of producing pn transitions and producing
phosphides and arsenides of gallium and indium). In this case a temperature and concentration difference is created between the
boundaries of the liquid zone. Because of the different solubility of the components of the system at different temperatures, a shift of the
zone in the direction of the temperature gradient takes place. The rate of shifting of the zone is usually 0.11.0 mm/hr, and the
temperature difference may be as high as 80 deg/mm.
Various equipment is used for zone melting, depending on the function, conditions, and output of the process. Depending on the method of
accomplishment, a distinction is made between container and crucibleless units, which in turn are divided into periodic, methodical, and
continuous types according to the character of the process; into horizontal and vertical types according to the attitude of the melting
material; into units with a moving ingot or heater according to the method by which the zone is shifted; into units that use resistance
heaters (for materials with a melting point of up to 1500C), induction heating (for melting substances with high electrical conductivity in
a vacuum or inert gaseous medium), electronbeam heating (for in vacuo melting of materials with a high melting point), radiation heating
(for materials with a low melting point), heating by thermal conductance and Joule heat according to the method of heating the zone; and
according to the method used to mix the zone (convective, mechanical, or electromagnetic) and the composition of the atmosphere

(vacuum or inert or shielding gas).

The equipment for container zone melting is a horizontal . pipe, within which a container with the load to be refined travels. The heaters
are mounted outside the tube and heat either the load or the container. Zonerefined tin ingots weigh up to 60 kg; germanium ingots, 10
kg, and gallium arsenide ingots, 1 kg. Crucibleless zone melting is performed in a vertical tube in which the rod to be refined is mounted.
The heater is located around the rod on the outside or within the pipe. The diameter of zonerefined silicon ingots may be 3550 mm; of
beryllium and iron ingots, 25 mm; and of vanadium ingots, 15 mm.
Container zone melting is developing in the direction of continuous zone melting units and processes (the zonespace, zonetransport, and
electrodynamic methods), increased intensity of refining, reduced heterogeneity of the resultant crystals, and increased purity. The
development of crucibleless zone melting is progressing toward an increase in the size of single crystals (a diameter of 5565 mm),
intensification of the refining process, and achievement of homogeneous distribution of impurities and structural flaws. The general trend
in the development of zone melting is characterized by work on optimum conditions, the creation of more advanced equipment, the
automation of the process, and the use of programming methods.
REFERENCES
Parr, N.Zonnaia ochistka i ee tekhnika. Moscow, 1963. (Translated from English.)
Zonnaia plavka, sb. Edited by V. N. Vigdorovich. Moscow, 1966.
Romanenko, V. N.Poluchenie odnorodnykh poluprovodnikovykh kristallov. Moscow, 1966.
Vigdorovich, V. N.Ochistka metallov i poluprovodnikov kristallizatsiei, Moscow, 1969.
Pfann, W. G.Zonnaia plavka. Moscow, 1960. (Translated from English.)
K. N. NEIMARK
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HAuCl4
ActiveMember

Re: Zone Refining.

January24th,2011,5:25pm
P

http://en.wikipedia.org/wiki/Czochralski_process
I imagine something like this can be done with gold, silver and other metals. May not be economical.
http://www.youtube.com/watch?v=6jv6ncV ... re=related
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HAuCl4
ActiveMember

Re: Zone Refining.

February7th,2011,3:06pm
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While researching this zone refining process, and by totally unrelated coincidence I found that a compound called sodium aurate(III),
NaAuO2, exists and it is soluble in excess of NaOH solutions.
The HAuCl4 first converts to insoluble Au(OH)3 along with AgCl which converts to AgOH, then it becomes soluble again in excess NaOH as
NaAuO2, while AgOH converts to Ag2O and is left behind as a solid, that separates more easily than the persistent AgCl in acid solution.
Can gold be refined by iterative recrystallization of NaAuO2?.
What a simple avenue to get rid of persistent traces of silver chloride!.
"PlatinumistheonlymetalfitforaKing".KingLouisXVofFrance
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HAuCl4

ActiveMember

Iterative Refining.
February19th,2011,7:12pm
P

Lou wrote:

A test for purity: take a sample of pure silver powder and dissolve it in quality nitric acid. Note if there is ANY color whatsoever to the
solutionit should be colorless. Evaporate this (still watch color) to dryness and heat in a porcelain dish to 440*C. Cool this and dissolve
in hot distilled water and look for any sediment on the bottom. Sediment on the bottom indicates metal oxides that formed during the
fusion of the silver nitrate at 440C...just about every impurity will form an oxide at that temperature. No oxides and no color mean that
your silver is over 99,995% pure.
This procedure can be repeated and high quality reagents used to yield silver that is factors of ten more pure. Eventually, however,
there comes a point where Ksp and solution equilibria put a cap on what ultimate level of purity you can get. Just think, 107g of silver,
roughly a mole, contains 6.02214 X 10^23 atoms. Even if your silver were 99,9999999% pure you would still have a large number of other
atoms!! There is interesting chemistry behind the purification of metals, both from the analytic and from the physical standpoint!

I tried this suggestion from Lou on a small scale with double distilled cation resined water and it worked like a charm with silver nitrate. A
guy in a lab asked me if he could keep my sample (6 iterations). He had never seen a silver sample that was so clean and so closely
matched the standard he had for the ICP. I traded the silver sample for 5 free ICP's...to be collected whenever...
Now I'm wondering if and what gold, platinum, palladium salts would be suitable to a similar physical/chemical recrystallization iteration
refining process. We already know that gold chloride isn't suitable. Any ideas guys?.
I posted in this thread to keep all my wacky ideas in the same place.
"PlatinumistheonlymetalfitforaKing".KingLouisXVofFrance
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