Infiltration UMD

“Low Viscosity Resin Infiltration Technique Used in Rapid Tooling,” M. Kokkengada, Z. He, Y. Kim, and J. G.
Zhou,
International Conference of Flexible automation and Intelligent Manufacturing, UMD, Maryland, June 2000.
LOW VISCOSITY RESIN INFILTRATION TECHNIQUE USED IN RAPID TOOLING
Monnappa Kokkengada, Zongyan He, Yun S. Kim and Jack G. Zhou

Department of Mechanical Engineering and Mechanics
Drexel Univeristy, Philadelphia PA 19104
ABSTRACT: Common infiltration methods used in rapid tooling have certain limitations viz.,
cracks, distortion and shrinkage caused by the high temperature of processing. Poor surface quality
also is a limitation of most infiltration techniques. In addition, the high temperatures involved in
conventional infiltration techniques make the process more costly, complex and difficult to control.
To overcome the above mentioned difficulties a low temperature polymer infiltration method is
studied and used in a rapid tooling technique, Rapid Pattern Based Powder Sintering (RPBPS).
Based on the curing principles of polymer materials, several potential infiltration materials were
selected. Using various infiltration methods and materials a series of testing samples were made and
their mechanical properties were tested. In order to calculate the necessary amount of polymer
materials and the height of infiltration into the sintered mold/part an infiltration model is also
proposed and the results are compared with experimental data. The low temperature infiltration
resulted in a 39.8% increase in the bending strength of the sintered and infiltrated part as compared
to the sintered-only part. The low temperature infiltration helped to control the shrinkage during
infiltration to less than 0.5% and also eliminate distortion of the final product.
INTRODUCTION
Rapid Tooling is a process that allows a tool for injection molding and die casting operations to be
manufactured quickly and efficiently so that the resultant part is representative of the production
material. Rapid prototyping /tooling and manufacturing have experienced tremendous growth and
have drawn a great deal of attention in the national and international manufacturing industry1.
Although rapid prototyping has brought in a new revolution in manufacturing processes of materials
by using additive and layer by layer material processing techniques, its focus has gradually shifted to
rapid tooling/manufacturing. The development list of Rapid Tooling (RT) technologies based on
rapid prototyping and manufacturing has been growing in recent years2 .Examples of RT techniques
are 3D Systems Keltool process, DTM’s Rapid Steel process and Extrudehone’s ProMetal process
developed by MIT. Rapid Pattern Based Powder Sintering (RPBPS)3 is a new rapid tooling
technique developed at Drexel University that aims to become a cost-effective and efficient
alternative to existing RT technologies. Often in a product development life cycle, prototypes made
from the final product material are required to generate accurate test results; in order to achieve this
it is desirable to generate tooling capable of producing a small number of production parts (150-
1000). The research presented in this paper is an effort towards developing such a technique by
utilizing and modifying the existing RPBPS to include a low temperature infiltration stage.
Based on RPBPS some special polymer materials to infiltrate the sintered mold/part at room
temperature have been identified. First, a brief introduction to the RPBPS technique and the main
processing steps are discussed. A variety of potential infiltration materials and their characteristics
are analyzed and those with desired characteristics are identified. A model for the infiltration process
is deduced and the selected materials were tested against that model. Further the mechanical
properties of the infiltrated samples were tested and illustrated.
“Low Viscosity Resin Infiltration Technique Used in Rapid Tooling,” M. Kokkengada, Z. He, Y. Kim, and J. G. Zhou,
TECHNICAL PROCESSES OF RPBPS

RPBPS is an integration of three techniques: Lost wax casting, Rapid Prototyping and
Powder Sintering. The main steps are shown in Fig. 1.
Design mold and cores in a 3D
CAD software package
(STL FILE)
Produce polymer prototype

of mold and core using a RP
machine
Mix metal
Cast the mixture under pressure powder and epoxy
binder in
Remove Master Pattern from the

casting
Cure the casting

(GREEN COMPACT)
Sinter the green compact

(SINTERED COMPACT)
Infiltrate the sintered compact
FINAL PRODUCT
Figure 1. The main technical processes of RPBPS technique
The initial step under RPBPS is the fabrication of the master pattern out of a thermoplastic material
using a rapid prototyping machine. This master pattern is produced directly from a 3 D solid model
of the part designed in any CAD system. The master pattern includes shrinkage allowances to
accommodate the linear shrinkage that occurs during sintering and infiltration. The RP pattern is
then positioned on a flat metallic substrate and placed in a metal frame with a size designed keeping
in mind the final dimensions of the mold and thereby incorporating machining allowances for the
runners and gates. The second step is the casting of a mixture of metal powder and binder around the
pattern under pressure. The binder is then cured under the application of heat. The third step of
RPBPS is the removal of the pattern. The RP pattern is made of a polymer crystal material that has a
melting temperature of 800 C, so by heating the green compact we can remove the pattern by
melting. If the pattern is simple enough so as to be able to incorporate draft angles then we can
remove the pattern by hand drawing. Thus at the end of this step we get a green compact with the
desired geometry and size. In general under medium casting pressure, the green compact contains
about 57% powder, 9% binder and 34% porosity by volume. The next step is sintering the green
compact in a furnace under a protective atmosphere of nitrogen. Experiments have shown that the
linear shrinkage during the sintering process is much higher than that which occurs in the steps
above. It is known that the density of the compact, sintering time and temperature, type and grain
size of the powder as well as the ratio and nature of the binder all affect the shrinkage and distortion
of the green compact during sintering. Increasing the density of the compact by increasing the
compacting pressure is one of the techniques that we use to control shrinkage3 during sintering
Shrinkage Vs Compacting Pressure
0.35
Linear Shrinkage(%)
0.3
0.25
0.2
0.15
0.1
0.05
0
0 2 4 6 8 10 12
Compacting Pressure (tons/sq.in)
Figure 2. Variation of linear shrinkage with compacting pressure

As can be seen from Fig. 2 increase in the compacting pressure results in a corresponding decrease
in linear shrinkage. In our technique a very large compacting pressure will result in damage to the
master pattern so we use an optimum compacting pressure that reduces the linear shrinkage while at
the same time preventing damage to the master pattern. In addition to this we have carefully
designed the sintering program (Fig. 3) and by using this program we have been able to control
shrinkage to less that 1% and eliminate distortion of the sintered product.
Figure 3. Program for sintering the mold.

After sintering the sintered compact has a composition of about 64% powder and 36% porosity by
volume. The final step is infiltration. This involves filling up the remaining pore structures after
sintering. Traditional infiltration under RPBPS involves infiltrating the steel compact with copper
alloys, such as brass and bronze. Capillary wicking of liquid copper alloy occurs due to the small
pore sizes and low contact angle. Using this technique we have been able to produce molds that are
more than 95% dense with a hardness of HRC 50. Copper alloy infiltration of the steel compact has
its attendant problems:
• The high temperature of infiltration leads to the formation of cracks in the mold.
• Linear shrinkage increases due to the high melting temperature of the infiltrating alloy.
• Distortion caused by non-uniform temperature distribution in the furnace especially in parts that
have complex geometry and thin walls.
RPBPS overcomes most of the common concerns for Rapid Tooling1 as shown below:
1) Size and Material Limitations
RPBPS has been effectively demonstrated using a variety of metal powders, ceramic materials and
composite materials. Size of the mold is limited only by the size of the largest pattern that can be
produced. The Sanders MM2 with its larger build envelope (12” × 6” × 9”) has helped us to take
RPBPS forward by increasing the size of the mold cavities that we can produce.
2) Shrinkage
A combination of effective design of sintering profile, low temperature infiltration and high
compacting pressure have enabled us to control linear shrinkage to within 1%.
3) Postprocessing
The elimination of finishing operations and thereby producing molds as close as possible to the final
product is one of the primary goals of RT and we have had considerable success in achieving this.
The use of subsieve steel powder (particle size < -325 mesh) helps reduce the postprocessing
involved in RPBPS.The very fine powder is able to effectively capture minute surface designs and
improve the surface quality of the finished mold virtually eliminating any additional finishing
operations.
(a) (b)
Figure 4 (a). Surface details on pattern Figure 4(b). Surface details on green compact
As can be seen from Figure 4 we are able to capture the very fine detail from the pattern shown in
(a) and reproduce it as shown in (b). We are able to capture surface details as small as 0.2 mm
NEW RESIN INFILTRATION TECHNIQUE

The research presented in this paper is an effort toward evolving a new infiltration technique at low
temperature and enabling the mold to be used for most injection molding applications. This modified
technique aims to overcome the difficulties encountered during high temperature infiltration viz.,
large shrinkage and distortion and produce molds that can be used for short run production parts. An
overview of the comparative aspects of the new RPBPS with other rapid tooling techniques is
tabulated below.
Requirements of Potential Infiltrants

The ideal infiltrant will completely fill the pore space, exhibit good flow and wetting of the pore
structure and will not leave a residue. Hardness and strength are most improved by infiltration.
Based on our experience with RPBPS we identified the following requirements for any suitable
infiltrant:
• It should be a liquid at room temperature but should transform to a solid under suitable
conditions.
• The liquid to solid transformation should be irreversible.
• The change in volume during the liquid to solid transformation should be as small as possible.
• The infiltrant should have a low viscosity and a high wettability for the metal powder so as to
enable the infiltrant to soak into the sintered compact and fill the pores.
• On solidification the infiltrant should possess reasonable strength, hardness and chemical
resistance so as to be used for injection molding.
• The infiltrant material should be able to resist temperatures of 100-150oC, which is what an
injection mold needs to withstand when processing common polymers like PVC, Polycarbonate
and PE.
TABLE 1:Comparison of competitive rapid tooling techniques
Process Time Cost ($) Qty Advantages Disadvantages
(weeks)
Silicon 1-2 1000- 1-50 Very Low Cost Low Quantities
Rubber(RTV) 5000 Short Lead Time Non-production
material
Short tool life
Epoxy 6-8 2000- 50-2000 Production Design Limitations
Composite 10000 Material
Composite 10000 Material Poor Surface Finish
High Cost
Long Lead Time
Keltool 4-6 2000- 50-20000 Production Design Limitations
7000 Material Surface Finish
Large Volume High Cost
Long Lead Time
RPBPS 1 < 2000 50-2000 No Cracks Low Quantities
with resin Low Shrinkage
infiltration Low Distortion
Fine Geometry
Economical
Short Lead Time
Selection of Suitable Infiltrants

A quick overview of the above conditions automatically eliminated metals and ceramic materials, as
they do not satisfy most of the above conditions. Organic materials have low strength and hardness
and they cannot withstand higher temperatures but certain polymers, especially thermosetting resins,
do meet the above-mentioned requirements and merit further investigation. We identified potential
infiltrants after a survey of available thermosetting resins that satisfy our criteria. The resin that we
identified as the ideal candidate was an acrylic resin sold under the brand name Imprex SuperSeal.
An added advantage would be the enhanced corrosion resistance and the improved machinability
afforded by the resin infiltration6.
The IMPREX SUPER SEAL 95-1000A is a thermosetting resin composed of mixed methacrylate
monomers and unsaturated polyester. This resin is pre catalyzed with azodiisobutyronitrile and
water. This has a specific gravity of 1.064 and a boiling point of 325 F. It is a pale straw colored
liquid with a slight blue tinge and a pleasant odor. This resin is free from any hazardous components
and is not carcinogenic. From experiments we have observed that the viscosity of the resin (16 cP at
25oC) is relatively stable with increase in temperature. Any heating above 80o C will result in the
resin crosslinking to form a white translucent solid. This crosslinking at higher temperatures, low
viscosity and stability at room temperatures are the most attractive properties of the resin that urged
us to investigate its usefulness as an infiltrant for our technique. Additionally the polyester
component provides enhanced chemical and thermal resistance properties.
Methods of Infiltration
Before infiltration the green compact is sintered and the surface of the sintered compact is cleaned to
remove surface oxidants that may have been formed during the sintering. Some resins have a high
viscosity at room temperature and they cure with time i.e. their viscosity increases with time even at
room temperature. Infiltrating a mold with large wall thickness using this material may leave the
central core of the mold uninfiltrated and porous. To overcome these problems we have devised
three of infiltrating methods based on the viscosity of the infiltrant and their curing properties (see
Figure 5)4.
Method (A) shown is employed when the mold wall thickness is large and the curing occurs
at room temperature. In this method the inner surface of the mold does not come into contact with
the resin and the resin infiltrates from bottom upwards. In order to ensure total infiltration of the
mold before curing occurs we place the whole container in a refrigerator until the entire mold in
infiltrated. The mold is then exposed to ambient temperature or warmed to cure the resin.
Method (B) shown is used when the infiltrant has a low viscosity that remains constant at
ambient temperature. In this method the entire mold is submerged under the resin until all the pores
are filled with the infiltrant. The infiltrated mold is then heated to the curing temperature of the
infiltrant until all the resin cures.
Method(C) is employed when the mold has thin walls and the inner surface of the mold is
free from any surface designs that might be damaged from contact with the resin. In this method the
rein is poured directly into the mold cavity to allow it to infiltrate the sintered compact from top
downwards. More resin is added as and when required until the whole mold is infiltrated and the
mold is then heated to cure the resin.
Figure 5. Methods for infiltrating a sintered mold.
For the infiltration to be successful all the pores of the green compact should be filled and the mold
surface should be clean and free from any imperfections. In order to achieve this we should be able
to model the infiltration process and calculate the amount of infiltrant needed to infiltrate a given
mold.
Model of the Infiltration Process

For a liquid the capillary pressure δP varies inversely with the pore size as given by5
δP = 2 γ cosθ / d (1)
Where γ denotes surface energy of the liquid, θ denotes contact angle and d denotes radius of the
pore.
We can see from the equation that the capillary effect depends on several factors: surface tension of
the resin, size of the pore and the angle between the sintered powder and resin which is
representative of the wettability of the resin to the powder. The height that the liquid (resin) rises due
to the capillary pressure is given by
δH = δP / ρ (2)
Where ρ is the density of the resin.
From the above equation (1) we see that greater capillarity is achieved when the pore sizes are
smaller and the contact angle is lower. The above equations cannot be used directly to calculate the
infiltration height of a sintered mold because the voids in the sintered mold are not straight circular
tubes as assumed in the derivation of the above equation. We must derive their equivalent radius r’
i.e., the radius of a circular cross section that has the same area as that of the void in the sintered
mold. The equivalent radius r’ is related to the size of the powder particles and the gap ratio (λ). As
shown in Fig. 6 we assume that the microstructure of the sintered mold can be simplified to be a
collection of straight circular cylinders that are bonded together during sintering4.
Figure 6. Microstructure of sintered mold
The packing arrangement of these cylinders can be any one of those shown in Fig. 7. Each mode has
its own gap ratio based on the structure of packing.
Figure 7. Packing modes of sintered powder particles

For mode (a) we have λa = [Sabc – 3(πR2)/6]/Sabc ≈ 0.092 where R is the radius of the particle & Sabc
is the area of equilateral triangle abc. For mode (b) we have λb = [Sabcd – 4(πR2/4)]/Sabcd ≈ 0.215
where Sabcd is area of square abcd. For mode (c) we have λc = [Sabcdef – 4(πR2/4)]/Sabcdef ≈ 0.395
where Sabcdef is area of hexagon abcdef.
Our experiments have shown that the gap ratio in sintered parts is between 0.30 – 0.40 so
mode (b) and (c) would be appropriate models for our infiltration process.
Now we can deduce the equivalent radius r’ for mode (b). The area occupied by the infiltrated resin
= Area of Square abcd – 4*(Area of quadrant), i.e., Sr = (2R)2 - 4(πR2/4)] = πr’2 where Sr is the
equivalent circular cross section, so we have
r’ = ( (4 / π ) − 1 ) R (3)
We know that λb = Sr /(2R)2 therefore
r’ = [ 4λb / π ]R (4)
We can also deduce the equivalent radius for mode (c). The area occupied by the infiltrated resin =
Area of hexagon abcdef - 6*(Area of sector), i.e., Sr = [6 3 (R2) - 2πR2]= πr’2 where Sr is the
equivalent circular cross section, so we have
r’ = ( (6 3 / π ) − 2 ) R (5)
We know that λc = Sr /(6 3 R2) therefore
r’ = 6 3λc / πR (6)
Let the d in Eq. (1) be replaced by the r’ derived in Eqs. (4) and (6). Substituting the result in Eq. (2)
we deduce the following relationships
δH = π σ cosθ / (ρR λ ) ≈ 1.77σ cosθ / (ρR λ ) (7)
and
δH = 2 π σ cosθ / ( 6 3 ρR λ ) ≈ 1.10σ cosθ / (ρR λ ) (8)

For water as the infiltrant: ρ = 1 g/cm3, R = 50 x 10-6 m, λ = 0.3, σ = 7.3 x 10-2 N/m. From the above
equation the height that water can infiltrate due to capillary pressure is 2.932m.
For brass as the infiltrant: ρ = 6.4 g/cm3, R = 50 x 10-6 m, λ = 0.3, θ = 00, σ = 0.12 N/m. From the
above equation the height that brass can infiltrate due to capillary pressure is 0.75m.
For acrylic resin as the infiltrant: ρ = 1.064 g/cm3, R = 50 x 10-6 m, λ = 0.3, θ =150,σ = 5.5 x 10-2
N/m. From the above equation the height that the acrylic resin can infiltrate due to capillary pressure
is 2.004m.
The above calculations show that depending on the thickness of the mold and the nature of
the infiltrant the appropriate mode of infiltration should be chosen. The real infiltration height will
be less than the calculated value because the real microstructure of the sintered mold is not
composed of uniform tubes and the contact angle is not so small due to the bad surface state of the
powder particles.
MECHANICAL TESTING
The main aim of the low temperature infiltration is to overcome the drawbacks of traditional
powder sintering techniques, while at the same time generating tooling that can be used for
producing injection molded plastic parts. In order to test the effect of the infiltration the 3 point
bending test was conducted on a sintered sample as well as on an infiltrated sample. Bend tests
establish the ductility of a metal under bending stress and show the ability of the metal to withstand
breakdown in use; additionally the bend test provides a reasonable guide to tensile strength too7. A
curve of bending stress versus strain was plotted using the results generated in the bending test. The
maximum bending stress was calculated before and after infiltration in order to investigate the
outcome of the infiltration.
A sample of required dimensions is made out of the sintered compact. As the infiltrant is one
that has low viscosity that remains constant with temperature we use Method (B) (see Figure 5) to
infiltrate the sample. The infiltration was done for 24 hrs to ensure total infiltration. The infiltrated
sample was then heated to 80oC to cure the infiltrant resin and ensure that the pores are filled up.
The sample was weighed before and after infiltration and an 8.14% increase in the weight of the
sample was found as a result of the infiltration. The sample dimensions were measured before and
after infiltration and there was no appreciable shrinkage as the temperature of the infiltration was
low. The stress – strain curve for the sintered sample as well as for the sintered and infiltrated
sample are shown in Fig. 8(a) and Fig 8(b) respectively.
90
80
70
60
Stress (MPa)
50
40
30
20
10
0
-0.12 -0.1 -0.08 -0.06 -0.04 -0.02 0 0.02
-10
Strain
Figure 8(a). Stress-strain relationship of sintered part.

70
60
50
40
Stress (MPa)
30
20
10
0
-0.16 -0.14 -0.12 -0.1 -0.08 -0.06 -0.04 -0.02 0 0.02
-10
Strain
Figure 8(b). Stress-strain relationship of sintered and infiltrated part.
From the graphs we see that the maximum bending stress before infiltration is 59.3 MPa and after
infiltration is 82.8 MPa. There is a 39.8 % increase in the bending stress thus proving the
effectiveness of this infiltration method.
The low viscosity resin makes the infiltration stage faster than traditional metal infiltration
techniques. The resin infiltration method does away with the use of a high temperature furnace and
hence is easier to control and monitor. In conventional RPBPS the shrinkage encountered during the
infiltration stage is between 5% to 6%. The low temperature infiltration reduces the shrinkage during
the infiltration stage to less than 0.5%.
The final product after infiltration suffers no distortion as a result of the infiltration hence making it
easier to generate good surface quality and maintain close tolerances.
CONCLUSIONS
RPBPS as a rapid tooling technique has been proven to be suitable for a variety of materials
and complex geometry. By including a low temperature infiltration stage we have taken this
technique further so as to be able to generate soft tooling capability for short run production parts
both economically and rapidly. We have also deduced an infiltration model to analyze the low
temperature infiltration so as to be able to estimate the quantity of resin and the infiltration height in
the sintered compact and verified the model with experimental data. The new technique overcomes
the defects of conventional high temperature infiltration and also serves to reduce shrinkage and
distortion appreciably.
REFERENCES
1) Jacobs P.F, Stereolithography and other RP&M Technologies from Rapid Prototyping to Rapid
Tooling, SME Press, New York (1996).
2) Vanputte D.A, “Rapid Tooling is a key factor in future achieving Rapid Product Development”,
Proceedings of 27th ISATA Conference, Auchen, Germany, (1994)
Paper No.94RA024.
3) J Zhou and Z He,“Rapid Pattern Based Powder Sintering Technique and Related Shrinkage
Control”, Journal of Materials and Design, Vol. 19 (1998) pp.241-248.
4) Z He, Y Kim, M Kokkengada and J Zhou, “Rapid Pattern Based Powder Sintering with Low
Temperature Polymer Infiltration”, Proceedings of 10th Annual Solid Freeform Fabrication
Symposium (1999), Austin, Texas.
5) German R.M, Powder Metallurgy Science, 2nd Edition, Metal Powder Industries Federation,
New Jersey (1997).
6) Charles M. Muisener, Resin Impregnation of Powder Metal Parts, Powder Metal Technologies
and Applications, ASM Handbook Vol.7 (1998).
7) Eric N.Simons, Testing of Metals, Great Albion Books 1972.

Infiltration UMD

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“Low Viscosity Resin Infiltration Technique Used in Rapid Tooling,” M. Kokkengada, Z. He, Y. Kim, and J. G.

LOW VISCOSITY RESIN INFILTRATION TECHNIQUE USED IN RAPID TOOLING

Monnappa Kokkengada, Zongyan He, Yun S. Kim and Jack G. Zhou

TECHNICAL PROCESSES OF RPBPS

Produce polymer prototype

Remove Master Pattern from the

Cure the casting

Sinter the green compact

Infiltrate the sintered compact

Figure 1. The main technical processes of RPBPS technique

Shrinkage Vs Compacting Pressure

Figure 2. Variation of linear shrinkage with compacting pressure

Figure 3. Program for sintering the mold.

NEW RESIN INFILTRATION TECHNIQUE

Requirements of Potential Infiltrants

Selection of Suitable Infiltrants

Figure 5. Methods for infiltrating a sintered mold.

Model of the Infiltration Process

Figure 6. Microstructure of sintered mold

Figure 7. Packing modes of sintered powder particles

We know that λc = Sr /(6 3 R2) therefore

δH = 2 π σ cosθ / ( 6 3 ρR λ ) ≈ 1.10σ cosθ / (ρR λ ) (8)

Figure 8(a). Stress-strain relationship of sintered part.

Figure 8(b). Stress-strain relationship of sintered and infiltrated part.

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