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Stress strain curves for thick electroformed Cu pieces

F. Arranz, M. Serrano, A. Muñoz, B. Szcepaniakb, B. Brañas, O. Nomen, J. Castellanos.


a
CIEMAT. Avda. Complutense 40. 28040 Madrid. Spain.
b
Galvano-t. Raiffeisenstrasse 8. 51570 Windeck/ Rosbach. Germany

ABSTRACT
Electroforming copper is a technology that allows manufacturing pieces with shapes difficult to achieve using other
technologies, low amount of impurities and excellent mechanical properties that together with the heat conductivity of the
material makes it ideal for some applications in the fusion and particle accelerator devices. Furthermore joining two
independent parts can be done at room temperatures with material having the same properties than the base pieces.
The published data concerning the mechanical properties of electroformed copper are referred to the direction tangent
to the surface of the mould on top of which the copper is deposited. Some researchers have suggested there could be non-
isotropic behavior but, to the best knowledge of the authors there have not been tests to confirm or deny such suggestion.
The current article exposes the results of tensile tests carried out on specimens made of electroformed copper,
machined in different directions with respect to the surface of the mould. The effect of heat treatments is also analyzed.
The different mechanical response depending on the direction of the specimens was first detected during the
acceptance tests of samples corresponding to different parts of a dump for the deuterons accelerator LIPAc that is being
installed in Rokasho (Japan). Some modifications in the production of the dump were proposed as a consequence of such
tests.

Keywords: electroformed copper, yield strength, ultimate tensile strength, elongation.

1. Introduction characteristics due to its fine grain, (3) the copper is very
pure and (4) the joint of the pieces is done at room
The linear IFMIF prototype accelerator (LIPAc) ends temperature.
up in a dump which stops a beam of deuterons 9 MeV,
125 mA in continuous wave. The Beam Dump (BD) is Compared to laminated copper, electroformed copper
estimated to withstand a radiation of 10^6 MGy. has the inconvenience of long times required for
manufacturing and therefore it is more adequate for
The BD is a cone made of copper electroformed on a prototypes than for large batches of pieces.
stainless steel mandrel. The cone is 2500 mm long with
varying thicknesses, from 5 mm (most of the wall) up to For the evaluation of this manufacturing technology,
30 mm in the flange (see fig.1). A second piece made of tensile tests were carried out with a range of specimens :
truncated cones used as a shroud coaxial with the specimens electroformed as a whole without any joint,
previous cone, was made as well by electroforming. specimens with a joint at the center electroformed in two
steps and specimens with a joint at the center made of
Cu and stainless steel [1,2].
During the manufacturing of the definitive pieces,
acceptance tests were carried out including tensile tests
which yielded different results depending on the
direction of the specimen relative to the surface of
electrodeposition. The plastic deformation was different
for specimens tangent to the surface of electrodeposition
(T) or orthogonal to the surface of the electrodeposition
(O). The results of these tests and the effect of thermal
treatments are the objective of this article and have not
been reported before in the open literature to the best
knowledge of the authors.
Electroformed copper in thick layers has already
been used in linear accelerator dumps [3] (0.5 mm) and
it is as well used in the fusion field for some parts of the
Fig. 1 Electroformed BD cone and shroud neutral beam injector system [4, 5] (1.5 mm). Agostinetti
[4] presents an extensive analysis of tensile test results
and fatigue test, deriving functional relationships
The technology chosen to manufacture the cone was
including temperature as a parameter.
electroforming because of several reasons: (1) allows
manufacturing of such geometry very difficult to obtain Thick pieces of electroformed copper are also used
in other way, (2) provides good mechanical in the field of astrophysics detectors [6, 7], thicknesses
_______________________________________________________________________________
author’s email: fernando.arranz@ciemat.es
in the order of 12 mm are manufactured. Overman [7] determined as the ratio between the highest measured
suggests the influence of anisotropy in the deformation load and the initial section of the specimen.
and failure modes.
After electroforming the samples to obtain the
An extensive study of the different additives that can specimens, the material underwent a vacuum baking
be used for electroformed copper and the application to treatment (180ºC x 3h in a vacuum oven), except for a
the manufacturing of a thrust chamber of a rocket engine batch of specimens that was tested without such
can be found in [8]. treatment for comparison. This heat treatment is
compulsory for the final manufactured pieces that will
have surfaces in ultra- high vacuum.
2. Testing procedure and materials Different materials have been tested:
The tests were carried out with a MTS 810 universal A) Laminated bar (named LB):
test machine with up to 100 kN capacity, under stroke
control at a displacement rate of 0.3 mm/min Specimens from a laminated bar were tested in order
(corresponding to a strain rate of 4 x 10^-4 /s). No to use them as a reference for comparison. The diameter
extensometer is used due to the small size of the of the bar is 63 mm, with treatment “hard”. The
specimens. The crosshead displacement values were manufacturer´s certificate include the values Rp0.2 =
recorded and used to obtain both the uniform elongation 280 N/mm^2 and Rm = 288 N/m^2. The material is Cu
and the strain. No machine compliance correction has OFE with a content of 99.998 % of copper. Figure 3
been made and thus the values are only indicative but shows the location of the samples in the bar. The
useful for the purpose of comparison. The tensile tests specimens were cut in both the longitudinal direction
were carried out at room temperature and at 150ºC, (LB_L) and orthogonal in the shape of discs (LB_D).
being this last temperature the highest value expected at
the BD during operation of the accelerator.
The specimens were obtained from samples with
thicknesses in the order of centimeters and with different
orientations with respect to the mould surface (tangent,
orthogonal and inclined). The dimensions of the
specimens are shown in figure 2. These specimens are
obtained by wire electrodischarge machining with no
further surface finish applied. The use of these reduced
specimens yields results that are equivalent to those of
standard size concerning engineering stress and
engineering strain [9]. Fig. 3. Tests specimens from laminated bar.

B) Electroformed Cu (named BI02), used to check


anisotropy:
A sample of electroformed copper was manufactured
on top of a plastic flat support painted with silver paint.
The diameter was 125 mm and the thickness reached 47
mm. From such sample specimens were cut in two
directions: T (tangent to the surface of the support) and
O (orthogonal to the surface of the support).
Identification of the specimens tested (BI02_T and
BI02_O).

Fig. 2. Tensile test specimen

The main goal of these tests was to compare values


of yield strength (Rp0.2), ultimate tensile strength (Rm)
and plastic behavior in different orientations. The yield
strength (Rp0.2) is obtained from the stress-strain
diagram drawing a parallel line to the straight part of the
curve at a distance 0.2 % in elongation axis and Fig. 4 Test specimens from BI02 sample O
calculating the intersecting point of such line with the (Orthogonal) and T (Tangent).
test curve. The ultimate tensile strength (Rm) is

2
Thermal treatments to improve ductility at
temperatures 200ºC and 250ºC for 5h in vacuum were
applied to orthogonal as well as tangent specimens and
then tensile tests were performed at 150ºC. The
identification of the specimens tested: BI02_T_HT200,
BI02_T_HT250 for specimens from tangent sample and
BI02_O_HT200, BI02_O_HT250 for specimens from
orthogonal samples.
C) Electroformed Cu cylinder (named SAM03):
A copper bar was manufactured rotating a stainless
steel cone and enlarging it with a copper piece of cable
(see figure 5). The manufacturing process required
several stops for smoothing the outer surface. The
diameter of the final piece was 48 mm. five discs were
cut from the ending part corresponding to the copper
cable and from each disc, 3 specimens were obtained.
Identification of samples: SAM03_O. These specimens
are basically orthogonal to the surface of the Fig. 6 Specimens cut from inclined slices for tests
electrodeposition. with and without vacuum baking

The ASTM B832 standard provides guidelines for


the manufacturing of nickel and copper electroformed
pieces. All the parameters indicated there (additives,
current intensity, agitation, electrolyte components
concentration) have been taken into account in order to
get optimal results for each of the samples used in the
tests.
For the electroformed copper, chemical analyses
were carried out using chips from the samples in order to
Fig. 5 Specimens from copper electroformed in
assess the amount of impurities. The techniques used
cylindrical shape.
were: elemental combustion analysis, plasma
spectroscopy and flame emission. The impurity levels
D) Electroformed Cu, inclined discs (named
were below the detection threshold in all the cases. The
CON01):
elements considered and the threshold levels are shown
A sample was electroformed on top of a plastic flat in table I.
support covered with silver paint. Several stops and
Elements Detection level
smoothing of the surface cycles were made until a
thickness of 21 mm was reached. Several slices were cut Ag, Al, As, B, Ba, Be, Ca, Cd, 6 ppm
with an inclination of 12º with respect to the tangent Co, Cr, Fe, Mg, Mn, Mo, Ni,
surface of the support piece (see figure 8). Half of the Pb, Sb, Se, Si, Sr, Ta, Te, Ti, V,
specimens underwent the usual vacuum baking treatment Zn, Zr
whereas the other half was tested without such treatment.
Identification of specimens: CON01_VB (if vacuum Bi, K, Na 20 ppm
baking was applied), CON01_NOVB (if no vacuum C_total, S_total 0.01 %
baking was applied).
P 200 ppm
Table 1 Results of chemical analyses. All analyzed
impurities below detection level

3. Tensile tests results


In order to facilitate the comparison of the curves, the
results of the tensile tests have been included in just two
figures (fig. 7 and 8). Table II summarizes the average
values of Rp0.2 and Rm at room temperature and at
150ºC, together with the standard deviation computed
for each value.

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Fig. 7. Stress strain curves for specimens from laminated bar LB and electroformed samples BI02

4
Fig. 8. Stress strain curves for specimens inclined 12º with respect to electroforming surface. NO VB (no vacuum
baking applied). VB (vacuum baking applied)

Room T. Rp0.2 SD Rp Rm SD Rm 150ºC Rp0.2 SD Rp Rm SD Rm


[MPa] [MPa] [MPa] [MPa] [MPa] [MPa] [MPa] [MPa]
LB_L 270.0 7.0 278.9 3.0 LB_L 233.9 3.7 241.2 2.2
LB_D 258.7 7.3 267.2 5.6 LB_D 228.0 4.7 236.2 1.4
BI02_T 248.8 16.4 299.3 9.3 BI02_T 202.1 6.4 226.2 5.6
BI02_O 246.8 6.2 286.8 25.6 BI02_O 199.1 3.2 215.1 8.1
SAM03_O 251.7 14.3 312.3 6.7 SAM03_O 201.7 10.5 235.3 2.9
CON01 NOVB 272.9 9.6 312.1 1.5 CON01 NOVB 200.7 6.7 226.8 5.7
CON01 VB 257.3 12.4 307.7 5.5 CON01 VB 200.9 10.3 229.3 7.5
BI02_T HT200 195.0 7.7 234.7 14.9
BI02_T HT250 164.7 5.7 219.3 2.5
BI02_O HT200 199.0 11.4 221.3 6.8
BI02_O HT250 167.2 4.2 197.1 2.6
Table 2. Values of Rp0.2 and Rm. Averages and their standard deviations. Tests at Room Temperature (left) and
at 150ºC (right).

4. Discusion. additives in the bath. These layers are thought to be


responsible for the brittle behavior.
For laminated copper the values of Rp0.2 and Rm
obtained in our laboratory are slightly lower than the During the manufacturing of the pieces and the
values provided by the material´s certificate. The values samples for the specimens some stops have been
for the specimens obtained in the direction of the applied performed to remove irregularities on the surface. These
cold work are slightly bigger (see Table II), but this stops are unavoidable and, if the surface is properly
difference is smaller than twice the standard deviation of deoxidazed and activated before the piece is again
the sample. The ductility behavior is pretty similar (see introduced in the bath, the new material should be
Fig. 8 LB_L and LB_D) therefore; it could be considered bonded to the previous one without any discontinuity in
an isotropic material. properties.
The results of the specimens from electroformed
copper BI02 with just vacuum baking treatment show a
strong effect of specimens orientation at 150ºC (see Fig.
8 BI02_T vs BI02_O). The specimens with orthogonal
orientation show a loss of ductility and in some cases
brittle behavior when tested at 150ºC. Fig. 9 shows the
comparison of fracture surface of specimens type O at
room temperature and at 150ºC.
An orthogonal slice was etched with sulfuric solution
and the successive layers of electroformed copper could Fig. 9 Specimens from orthogonal sample tested at
be easily distinguished (see figure 10). The successive room temperature (left) and 150ºC (right)
layers correspond to the replenishment of organic

5
Electroforming cylindrical pieces with small initial
diameters (around 1 or 2 mm) can lead to brittle behavior
in the layers next to the original electroforming surface.
The vacuum baking heat treatment has no effect for
the specimens tested at 150ºC (expected maximum
working temperature for the BD of LIPAc).

Acknowledgments
This work has been partially funded by the MINECO
Ministry under project FIS2013-40860-R and the
Fig. 10. Successive electroformed layers for an
agreement as published in the Spanish BOE (BOE n14,
orthogonal slice.
p. 1988)
The authors want to acknowledge the careful
The heat treatments at 200ºC and 250ºC during 5
technical work of Daniel Plaza providing the necessary
hours in vacuum, do not improve the behavior of the
measurements and pictures.
electroformed material named BI02, in the T orientation,
on the contrary, has pernicious consequences with
respect to Rp0.2, Rm and plastic behaviour. Concerning
specimens type O, these heat treatments lead to small References
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that some specimens displayed, (see Fig.8 BI02_T HT “Evaluation of the electroforming technique for IFMIF-
and BI02_O HT). EVEDA Beam Dump manufacturing”. Fusion Science
and Technology. Vol. 60. (538-543). 2011.
The tensile tests results for the electroformed bar
named SAM03, show quite significant scatter and in [2] F. Arranz, B. Brañas, D. Iglesias et al.
some cases a brittle behavior (see Fig. 8 SAM03_O). “Manufacturing prototypes for LIPAc beam dump”.
This brittle behavior is observed in the specimens Fusion Engineering and Design. Vol. 89. (2199-1103).
machined from the central part of the bar, and could be 2014.
attributed to the high current intensity at the initial steps
of the electroforming in that area. The wire used as a [3] C. Logan, J. Dini, W. Ludeman et al.
mandrel for the electroforming had initially around 2 “Development of manufacturing methods for 50 cm
mm diameter, and a sharp end. diameter neutron source targets for RTNS-II”. Journal of
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Concerning the curves in Fig. 8, the comparison of
the curves and the values of the specimens with and [4] P. Agostinetti, M. Dalla Palma, S. Dal Bello et
without the vacuum baking of the inclined disc, the only al. “Investigation of the thermo-mechanical properties of
effect is observed in the tests at room temperature, where electrodeposited copper for ITER”. Journal of nuclear
the value of Rp0.2 decrease about 8% when the vacuum materials. 417 (2011) 924-927
treatment is applied. The manufacturer indicates that this [5] F. Fantini, P. Agostinetti, V. Cervaro et al.
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could take place simply by the pass of time if a long Prototypes for the SPIDER grids”. Fusion Engineering
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150ºC. This treatment is an unavoidable step to prepare
surface that will become vacuum boundaries. [6] S. Borjabad. “Copper electroforming at the
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“Majorana Electroformed Copper Mechanical Analysis”.
The values of Rp0.2 and Rm are independent of the
PNNL-21315. 2012
orientation of the tensile test sample (tangent vs.
orthogonal relative to the surface of electroforming), [8] G. A. Malone, W. Hudson, B. Babcock and R.
whereas the plastic behaviour is dependent of the Edwards. “ Improved Electroformed Structural Copper
orientation. and Copper Alloys”. NASA/CR-1998-208680
For the electroformed copper the values of Rp0.2 and [9] M. N. Gussev, J. T. Busby, K. G. Field et al.
Rm decrease around 20% when the tests are carried out at “Role of Scale Factor During Tensile Testing of Small
150ºC compared to the values at room temperature. Specimens”. Small Specimen Test Techniques: 6th
Volume. ASTM. 2015.
The applied heat treatments (200ºC and 250ºC x 5h)
have a detrimental effect on mechanical properties.
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