growth of copper (1)
TRANSCRIPT
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Growth of Copper (II) Sulphate Pentahydrate
(CuSO4 5H2O) from Aqueous Solution
Tutor:Hess
Student:
Jingwei Wang Nr.3557579
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Abstract:
Crystal growth of CuSO4 5H2O from an aqueous
solution by means of the temperature reduction method
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Content
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1.Introduction1.1 Methods of crystal growth
Methods of crystal growth consist of simple cheap techniques
and complex process relatively. The growth time for
crystallization varies. Crystals may be produced in the solid,
liquid or vapour phase.On this basis, methods of crystal growth
can be sorted into three categories below,
Solid Growth - Solid-to-Solid phase transformation
Liquid Growth - Liquid to Solid phase transformation
Vapour Growth - Vapour to Solid phase transformation
Based on the phase transformation process, crystal growth
techniques are classified as solid growth, vapour growth, melt
growth and solution growth (Pamplin 1979).
1.2 Growth from solution
Materials, which possess high solubility and have variation in
solubility with temperature can be grown easily by solution
method. This method is simpler and cheaper compared with
other methods. But growth process is slow and it takes a long
time for crystallization. There are several methods in solution
growth depending on the solvents and the solubility of the
solute. They are
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1 Temperature reduction method
2 Isothermal evaporation method
3salting out
1.2.1 Temperature reduction method
This method is applicable to those crystals which possess a
higher solubility constant and a certain temperature range. And
this range is limited: The upper limit supposed to not be too high
due to more evaporation. Too lower limit will be disadvantage
of crystal growth. Generally, the starting point should be
50~60,the reduction range should be 15~20. It is better that
the solubility of crystal via this method not be lower than
1.5g/1000g* . During whole growth process, the key is to
control suitable temperature reduction rate which enable
solution to stay in metastable area.
2.Theory
2.1Ostwalds Diagram
The relationship between temperature of spontaneous
crystallization and solubility is shown by the dashed , called
supersolubility curve. The significance of this curve is not as
clear as solubility curve due to external factor effection.
The three areas are stable, metastable and labile separately.
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(1) In stable area, it is impossible to crystallize.
(2) In metastable area, spontaneous crystallization doesnt occur.
But crystal growth is possible if seed crystals exist.
(3) In labile area, spontaneous crystallization is possible but not
inevitable. But it may generate many seed crystals
instantaneously.
Figure 2.1Ostwald-Miers diagram for a solute/solvent system
2.2Nucleation and Growth Kinetics
The accomplishment of supersaturation is not able to start
crystallization. The formation of nuclei with a number of minute
solid particles present in the solution is a prerequisite. Then
nucleation may occur spontaneously.
The formation of nuclei can be sorted by homogeneous and
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heterogeneous.
2.2.1 Homogeneous nucleation
The liquid structure is disorder from long rang, but unstable in
short range, which means possessing some ordered atom group.
When temperature reduces below melting point, these ordered
atom group are possible to form embryo. So when embryo
emerge in supercooling liquid, on one hand, the atom inside are
ordered and possess a lower Gibbs free energy, which drive
phase change. One the other hand, formation of new embryo
generates more surface which increase surface free energy.
Thats the resistance. So the sum change in free energy G is:
G reaches maximum value when radius is r*.See in Fig.2.2.1.
When rr*, the growth of nuclei
reduce free energy. These embryos are stable ones.
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Fig.2.2.1
2.2.2Heterogeneous nucleation
Heterogeneous nucleation occurs much more often than
homogeneous nucleation. Usually, it forms in phase boundaries
or sticks on impurities like dust and wall. The initial energy is
less than that of homogeneous nucleation. At such
heterogeneous phase, the effective surface energy is lower. The
more infiltrated they are, the less energy for facilitating
nucleation and is the lower nuclear barrier is.
3.Growth Process3.1Cleaning
First clean all the apparatus which mentioned in the scription.
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3.2Growth of seed crystals
Preparation of solution:
Prepare 30 g CuSO 5 H O with 100 ml 18 Mcm H O in a 300
ml cooking cup.
Dissolve the CuSO 5 H O at about 50 C under stirring (on
heating plate). If a residue remains one can
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a) add 18 Mcm H O,2
b) heat a little more, or
c) filter it out.
Let it stay over night at room temperature (there should be
some crystals formed, see Fig. 3).
3.2 Preparation of Saturated Solution
3.3Determination of the Saturation Point of the Solution
By Schlieren Method, we can find out the saturated point using
seed crystal with cord.
The principles are as follows:
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