Melizabeth Santana Silverio

QUIM 4999 Inorganic Investigation

Prof. L. Koscielski

Synthesis and characterization of
low-melting mixed-metal oxides
1
University of Puerto Rico in Cayey
Contents:
Introduction
Elements of the reactions
Descriptions
Compounds known
Investigation
Methodology
Conclusion
Futures work
References

2
Introduction: What is solid state
chemistry?
Solid state chemistry is the study of the synthesis, structure,
and properties of solid phase materials.

Solid state is also referred as the chemistry of materials.
Different kinds of solid states amorphous, crystalline or
polycrystalline.



1
Google image, http://googleimage/amorphous (accessed May 2014)


Figure 1: Kinds of solid states
1

3
Characterization is the analysis of identifying the
properties of a compound.
X-ray crystallography is a technique that allows the 3D
determination of molecular structures.
A synthesis reaction or direct combination reaction is one
of the most common types of chemical reactions.
In a synthesis reaction two or more chemical species
combine to form a more complex product.
Inorganic synthetic methods can be classified roughly
according to the volatility or solubility of the component
reactants, in this case low-melting mixed-metals.

Introduction: What is solid state
chemistry?
4
Oxides are binary or tertiary compounds of oxygen with
another element or group.
The elements used are arsenic (As), tellurium (Te), lead
(Pb), bismuth (Bi), and antimony (Sb).
They have the properties of all having low melting points.

Elements of reaction
5
Elements of reaction
Table 1: Physical and Chemical description of the elements used
2

2
MSDS, http://sciencelab.com (accessed May 2014) 6
With the elements selected reactions were made with
different ratios.
The ratios were selected by numeric order.
Some of the ratios with low numeric order were already
discovered so I selected a higher numeric ratio.

Elements of reaction
Table 2: Discovered compounds
3


Oxygen content
Same group
15/15
3 AsSbO
3

4 AsSbO
4

AsBiO
4

SbBiO
4

5 AsSbO
5

7 SbBi
3
O
7

3
Lukasz Koscielki, Solid state research table MxM'yQx.

7
Elements of reaction
8
Table 3: Compounds to be discovered
Ratio Mix Elements Possible
products
1:2 AsBiO As
2
Bi
4
O
9

As
2
Bi
4
O
11

As
2
Bi
4
O
13

As
2
Bi
4
O
15

PbTeO PbTe
2
O
5

PbTe
2
O
6

PbTe
2
O
7

PbTe
2
O
8

9
Elements of reaction
Ratio Mix Elements Possible
products
2:1 AsBiO As
4
Bi
2
O
9

As
4
Bi
2
O
11

As
4
Bi
2
O
13

As
4
Bi
2
O
15

PbTeO Pb
2
TeO
4

Pb
2
TeO
5

Pb
2
TeO
6

Pb
2
TeO
7

Table 3: Compounds to be discovered
10
Elements of reaction
Ratio Mix Elements Possible
products
1:3 AsBiO AsBi
3
O
6

AsBi
3
O
7

AsBi
3
O
9
AsBi
3
O
10

PbTeO PbTe
3
O
4

PbTe
3
O
8

PbTe
3
O
10

PbTe
3
O
11

Table 3: Compounds to be discovered
11
Elements of reaction
Ratio Mix Elements Possible
products
3:1 SbBiO Sb
3
BiO
6

Sb
3
BiO
7

Sb
3
BiO
9

Sb
3
BiO
10

Table 3: Compounds to be discovered
12
Table 3: Compounds to be discovered
Elements of reaction
Ratio Mix Elements
Possible products
1:3 AsBiO As
3
Bi
5
O
12

As
3
Bi
5
O
15

As
3
Bi
5
O
17
As
3
Bi
5
O
20

PbTeO Pb
3
Te
5
O
13

Pb
3
Te
5
O
16

Pb
3
Te
5
O
18

Pb
3
Te
5
O
24

SbBiO Sb
3
Bi
5
O
12

Sb
3
Bi
5
O
15

Sb
3
Bi
5
O
17

Sb
3
Bi
5
O
20

The elements to be synthesized most of them are new
compounds and analogues.
Analogues have a structure similar to that of another
one, but differing from it in respect of a certain
component.
The only analogue compounds are:

13
Elements of reaction
Compounds Analogue
PbTe
2
O
5

PbTe
2
O
6

PbTe
2
O
7

PbTe
2
O
8

SnPbTe
2

GePbTe
2

Making silica tubes
1. Measure a 48inch silica tube with a marker each 6cm.
2. Cut with a glass cutter each 12inches.
3. Using a Bunsen burner separate each tube and close
the end in a circular way.
4. Wait until its room temperature and insert a small
amount of acetone to make the carbon coating.
5. Heat the tube with acetone until the lower part turns
black.
6. Do a triplicate of carbon coating in each tube.






14
Methodology
15
Methodology
16
Methodology
Synthesizing the reaction
1. Calculate the amount of reactants your going to use like
this example equation:




Note: The element with higher molar mass is always
20mg
2. Weight the elements and insert them in the tubes with
carbon coating through a funnel and a rubber handle.
3. Put the funnel and the rubber handle in a beaker with
aqua regia 3HCl: 1HNO
3.



17
Methodology
4. Repeat steps with al reactions, using a new rubber
handle and funnel in each one.
5. After a day remove the aqua regia and put the funnels
in base for another day and clean the rubbers.
6. Put the tubes in the oven.
7. Characterize the product with X-ray crystallography.

18
Methodology
19
Methodology
Load reactions in oven and characterize them.
Learn the technique of X-ray crystallography.
Make analogue reactions of Thorium with Hafnium.
20
Future work
University of Puerto Rico at Cayey
BRIC
Dr. L. Koscielski

21
Acknowledgements
Google image, http://googleimage/amorphous
(accessed May 2014).
MSDS, http://sciencelab.com (accessed May 2014)
Lukasz Koscielki, Solid state research table MxM'yQx.
J., Blascovich; J., Loomis; A.C. Beall; K. R. Swinth; C. L., Hoyt; J.
N., Bailenson, Inorganic Journal Crystal Research and
Technology, (1984), 19, 109-112, DOI:
10.1207/S15327965PLI1302_01, Tandfonline,
http://www.tandfonline.com/doi/abs/10.1207/.U4Zu_164nFI
(accessed May 2014)
S. G., Parker; J. E., Pinnell; L. N., Swink, Journal of Material
Science Determination of the liquidus-solidus curves form the
system PbTe-GeTe, (1974), 9, 1829-1832, SpringerLink,
http://link.springer.com/article/10.1007%2FBF00541753
(accessed May 2014)



22
References

Melizabeth Santana Silverio
QUIM 4999 Inorganic Investigation
Prof. L. Koscielski

Synthesis and characterization of
low-melting mixed-metal oxides
23
University of Puerto Rico in Cayey