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PREPARATION OF DENTAL PHOSPHATE-BONDED INVESTMENT TO CAST

NICKEL:CHROMIUM ALLOYS AND THE EVALUATION OF ITS MECHANICAL
AND PHYSICAL PROPERTIES

Article  in  World Journal of Pharmaceutical Research · January 2014

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 World Journal of Pharmaceutical Research
Nuzal et al. World Journal of Pharmaceutical Research
SJIF Impact Factor 5.045

Volume 3, Issue 9, 173-179. Research Article ISSN 2277– 7105

PREPARATION OF DENTAL PHOSPHATE-BONDED INVESTMENT

TO CAST NICKEL:CHROMIUM ALLOYS AND THE EVALUATION
OF ITS MECHANICAL AND PHYSICAL PROPERTIES

Najdat H. Abdul-Razzak1, Saadi M. D. Al-Nuzal 2*, Mohammed A. Mustafa1,

Flaih H. Ali1, and Bushra A. Lafta1

1
Ministry of Science and Technology, P.O 765, Al-Jadiryia, Baghdad, Iraq.
2
Environmental Research Center, The University of Technology, Baghdad, Iraq.

ABSTRACT
Article Received on
09 September 2014, An investment composition is described for use in dental investment
Revised on 03 Oct 2014, casting (also called lost wax casting), from Iraqi locally available raw
Accepted on 27 Oct 2014
materials. The major composition is a phosphate bonded material that
contains synthesized mono-ammonium phosphate (MAP) as binder,
*Correspondence for and silica filler (quartz, cristobalite, or a mixture thereof) as refractory
Author
materials. The procedure included many steps among them chemical
Dr. Saadi M. D. Al-
syntheses, and thermal treatments at high temperature (~1100ºC),
Nuzal
Environmental Research followed by chemical analysis for quality control. The high purity
Center, the University of investment was successfully, used to cast Nickel: Chromium alloys for
Technology, Baghdad, dental use. The evaluation of the mechanical and physical properties of
Iraq.
the prepared investment were carefully checked according to the
required specification of the ISO No. 9694/1996, which was adapted
for preparing chemical, physical, and mechanical properties of the prepared dental materials.
The chemical analysis of this formulation showed to be in good agreement with many
imported investments.

INTRODUCTION
Dental investments are refectory compositions suitable for forming mold into which molten
metal may be cast. The cavity is formed in the mold by melting out an expandable wax
pattern, which has been imbedded in the mold. Phosphate bonded investments are one type of
investment material, which is extensively discussed [1]. Most Palladium and base metal alloys
used for partial dentures and porcelain-fused-to metal restoration have high melting

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Nuzal et al. World Journal of Pharmaceutical Research

temperature and this alloy is cast into molds at 850 to 1100C. Although these investments
are some what more difficult to remove from casting than gypsum investment. They are more
[2]
stable at (high casting metal) ceramic alloys . Investment materials for casting alloys
must meet exacting requirements: easy manipulation and handling, no chemical reactions
with alloy at casting temperature, able to provide adequate expansion to compensate for
casting shrinkage.

Many studies were performed to investigate the thermal behavior of MgNH 4PO4.6H2O,
phosphate-bonded investment at elevated temperature, and their deterioration at various
conditions. The rapid growth in use of metal ceramic restorations boost the use of phosphate
or silicate bonded investments. One of the important requirements of an investment material
to be used for a casting mould is that it should expand on setting and heating to compensate
for the cooling of the cast metal as it returns to room temperature. The investment material
should be of a suitable consistency for adaptation to the wax model and have a reasonable
setting time. To withstand the temperatures required for the casting process there should be
no distortion; no decomposition; should not fragment or disintegrate under the impact of the
molten metal; the material should be porous to allow the escape of air and gases and the
investment should be easily removed from the casting after cooling [3-8].

This type of investment usually has less than 20 % binder, and remainder of the investment is
quartz or another form of silica (cristobalite). Each forms of silica expands when heated, with
an expansion varies from one type to another. Pure cristobalite expands to 1.6 at 400C,
quartz 1.54 % at 600 C, and tridym less than 1% at 600 C. In case of cristobalite, the
expansion is somewhat uniform to at 200 C, where its expansion increases sharply from 0.5
% to 1.2 %. These investments can be mixed with water or with other aqueous liquid. The
special liquid in a form of silica solution in water, phosphate-bonded possess higher setting
expansion when they are mixed with the silica solution than when they are mixed with water.
With a mix containing silica solution, the investment mass in is capable of expanding
hygroscopically, whereas if the mix is only water the hygroscopic expansion of such an
investment is negligible. Using silica solution instead of water with phosphate-bonded
[9-11]
investment also increases its strength considerably . The purpose of this work is to
establish a phosphate-bonded investment formula that fit the requirement of the ISO
specification No. 9694/1996 [12], and has the capability to be produced locally.

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Nuzal et al. World Journal of Pharmaceutical Research

MATERIAL AND METHOD

1. The Phosphate-Bonded Investment Preparation
The phosphate-bonded investment was prepared from two main groups of ingredients, fillers
and binders. Fillers are usually quartz, cristobalite or a mixture of the two within the range of
approximately 80 %. The function of the filler is to provide high-temperature thermal shock
resistance, high thermal expansion, and both play small role in the chemistry of the
investment during setting. The binders are essentially (MgO) and NH4H2PO4. A typical
formula for prepared phosphate bonded investment is prepared according to table 1.

Table 1: Composition of Typical Phosphate-Bonded Investment.

Ingredients Weight %
Large cristobalite 38-42
Fine cristobalite 19-21
Quartz 19-21
MAP 8-12
MgO 7-9
Boric acid 1-3

Table 2: Recommended Mechanical Properties of Phosphate Investment [12].

Mixing Ratio 100 g: 25 ml
Working Time 4.5 min
Setting time 25 min
Compressive strength 9-11 M Pa
Total Expansion 3.35 %
Thermal Expansion 1.35 %
Particle size Ranging from size 425-45 micrometer

2. Mechanical Properties
Typical chemical, physical, and mechanical properties which was adapted for preparing of
the prepared dental materials of the phosphate-bonded investments according to the ISO
specification No. 9694/1996 [12] was listed in table 2, A-Setting time (working time): Shall be
not less than 4 min from the moment of first contact of investment and water to measure
setting time, stainless steel rings, with an internal diameter of 10 mm. and a thickness of 2
mm. The investment was manipulated and placed in metallic ring, after 120±10 s from the
beginning of spatulation; the apparatus was placed over a grate inside a hermetically sealed
plastic container after 150±10 s from the beginning of spatulation a 100 g, 2 mm active point
Gillmor needle was positioned vertically on the surface of the material. This test was repeated
every 60s until the needle did not mark the surface of the investment. The setting time was
considered as the average of 5 measurements.

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3. Expansion
All the phosphate-bonded investments currently available casting high-melting alloys have
thermal expansion for setting expansion and hygroscopic expansion. The total dimensional
change is a very important property of casting investments that occurs if the investment is in
contact with water from any source during the setting process after investing the wax pattern.
The mixed investment, when tested 2h after the first contact of investment and water, shall
exhibit a total expansion (covering air setting, hygroscopic and thermal) of not less than 1.7
% if intended for use with base metal alloys. Table 2 shows the results of phosphate-bonded
investment expansion.

4. Compressive Strength
Low temperature: The transverse strength of the set investment test pieces 2h after the
commencement of mixing at a temperature of 23±2ºC shall be not less than 5 MPa. High
temperature determined at the maximum mold temperature shall be not less than 5 M Pa.
Table 2 shows the T.C.S of the investments.

5. Particle Size Test

Grain size particle in weight percentage for 100 g of phosphate-bonded investment ranging
from size 425-45 micrometer.

RESULTS AND DISCUSSION

The required properties of an investment should have the following:

It should be easily manipulated. Not only should it be possible to mix and manipulate the
mass readily and to paint the max pattern easily, but the investment also should harden within
a relatively short time. Its mold have sufficient strength at room temperature to permit ease in
handling, and enough strength temperature to withstand the impact force of the molten metal
the inner surface of the mold should not break down at a high temperature.

1. On being heated to higher temperatures, the investment must not decompose to give off
gasses that could damage the surface of the alloy. It should have enough expansion to
compensate for shrinkage of the wax pattern and the metal that taken place during the
casting procedure.

2. Casting temperature should not be critical preferably the thermal expansion versus
temperature curve should have a plateau of the thermal expansion over a range of casting

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temperature. A dental casting investment should be porous enough to permit the air or to
other gases in the mold cavity to escape easily during the casting procedure. It should
produce a smooth surface and fine dental and margins on the casting.

3. After the casting is completed, the investment should break away readily from the surface
of the metal and should not have reached chemically with it. Because the mold is always
destroyed in the casting process, the investment material must be comparative
inexpensive.

There are three specifications on which the evaluation could be done for the investment, ISO
No.9694 (Imitational organization for standardization), Geneve 1996, was applied for
phosphate-bonded investments according to the following specification. Phosphate-bonded
investment is composed mainly of refractory, binder and other additives many experimental
and a large number of mixes had been done using the standard materials (Particularly the
binder) until the best formula was obtained using the above ISO specification to evaluate
every mix.

The phosphate-bonded investments for alloys having a solidus temperature above 1080C.
Initial setting time must not differ by more than 30 % from the time stated by the
manufacture the compressive strength at room temperature is less than 15 % from the line
stated by the manufacture. Certain phosphate compound, such as ammonium diacid
phosphate (NH4H2PO4), has been found to provide room temperature strength to the increase
the strength of the investment at casting temperature.

A small amount of magnesium oxide that was used at room temperature ammonium diacid
phosphate reacts with magnesium oxide to give the investment green strength, or room-
temperature strength according to the chemical reaction. The chemical reaction for the binder
system that causes the investment to set and harden generally written as follows:

NH4H2PO4 + MgO + 5H2O NH4MgPO4.6H2O

However, phosphate are quite complex, and the reaction is not as simple as indicated by the
[1, 8, 10-11]
above equation . The ammonium diacid phosphate is used in a greater amount than
necessary for this reaction so that the remainder can react with silica at an elevated
temperature. The higher temperature probably causes a superficial reaction between P2O5 and

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SiO2 to form silicophosphate, which increases the strength of the investment at higher
temperature. The water produced by this reaction lower the viscosity of the mix as spatulation
continuous. The investments can be mixed with water or with a special liquid. The special
liquid is a form of silica sol. In water, phosphate-bounds investments posses higher setting
expansion when they are mixed with the silica sol. Than when they are mixed with water,
with a mixed with water, with a mix containing silica sol, the investment mass capable of
expanding hygroscopic, whereas if the mix is only water, the hygroscopic expansion of such
an investment is negligible using silica sol. Instead of water with phosphate-bonded
investment also increases its strength considerably.

CONCLUSION
An investment composition is described for use in dental investment casting (also called lost
wax casting), from Iraqi locally available raw materials. The major composition is a
phosphate bonded material that contains synthesized mono-ammonium phosphate (MAP) as
binder, and silica filler (quartz, cristobalite, or a mixture thereof) as refractory materials. The
high purity investment was successfully, used to cast Nickel:Chromium alloys for dental use.
The chemical analysis of this formulation showed to be in good agreement with many
imported investments.

REFERENCE
1. Ralph, W. Phillips, "Skinner's Science of Dental Materials.", 8th ed., pp. 406-410, W. B
Sander's Co., Philadelphia, 1982.
2. Wang, C., Millstein, P. L., Nathanson, D., "Effects of cement, cement space, marginal
design, seating aid materials, and seating force on crown cementation.", J. Prosthet. Dent,
1992; 67: 786-790.
3. Asaoka, K., Bae, J. Y., Lee, H. H., "Porosity of dental gypsum-bonded investments
in setting and heating process.", Dent. Mater. J, 2012; 31: 120-124.
4. Higuchi, H., Matsuya, S., Yamane, M., "Thermal behavior of phosphate-bonded
investment. Part 1. Thermal behavior of MgNH4PO4.6H2O.", J. J. Dent. Mater. 1982; 23:
1-5.
5. Habu, N., Takahashi, H., Min, Y., Motomura, K., Nakamura, H., Nishimura, F.,
"Properties of a phosphate-bonded dental investment for quick heating.", J. J. Dent
Mater. 1995; 14: 681-690.

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 Nuzal et al. World Journal of Pharmaceutical Research

6. Juszczyk, A. S., Radford, D. R., Curtis, R. V., "Deformation of phosphate-bonded

investment materials at elevated temperatures.", Dental Mater, 2007; 23: 579-585.
7. Raya M. Jawad Al- Ghabban, "The Effect of Different Concentrations of Gilvest with
Water on the Setting Time of Phosphate-bonded investment.", Iraqi Sci. J. Nursing, 2010;
23(2).
8. Miyaji, T., Utsumi, K., Suzuki, E., Shimizu, Y., "Deterioration of phosphate-bonded
investment on exposure to 100 % relative humidity atomosphere.", Bull. Tokoyo Med.
Dent. Univ, 1982; 29: 53.
9. Ayad M. F., Rosenstiel, S. F., Salama, M., "Influence of tooth surface roughness and type
of cement on retention of complete cast crowns.", J. Prosthet. Dent, 1997; 77:116-121.
10. Schnell, R. J. Mumford, G., Philips, R. W., "An evaluation of phosphate bonded
investment used with a high fusing gold alloy.", J. Prasthet. Dent, 1963; 13: 324.
11. Craig, R. G., O’brien, W. J., Powers, J. M., "Dental Materials", 6th Edt, Mosby, 1996.
12. ISO 9694:1996 Dental phosphate-bonded casting investments. International Standards
Organization, Geneva.

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