Iridium Platinum Alloys

A CRITICAL REVIEW OF THEIR CONSTITUTION

AND PROPERTIES
By A. s. Darling, Ph.D., A.M.1.Mech.E.
Native crystals of iridium-platinum are Journal of Science, in 1860, remarked some-
frequently found in association with platinum what incredulously: “The platinum makers of
ores. These natural alloys, of rather variable Paris are manufacturing these alloys and
composition, occur as grains, and sometimes contrary to the wishes of the discoverers are
as small cubes with rounded edges. Although extracting higher prices for them than for
the geographical distribution is fairly wide pure platinum”.
the major deposits appear to be in the Urals. Prominent physicists were, at this period
One such crystal, described in I940 by Masing, of the nineteenth century, devoting consider-
Eckhardt and Kloiber (I) had a well-defined able effort to the problems involved in repre-
two-phase micro-structure. senting their fundamental and derived units
Synthetic alloys were produced at an early in concrete form. Iridium-platinum alloys
date. Gaudin (z), who fused spheres of a came to fill a unique position in the scale
10per cent iridium-platinum alloy on hearths of substances capable of retaining indefin-
of lime and magnesia, commented in 1838 itely their mass, form, and linear dimensions.
upon the lustre, malleability and extreme In addition to their corrosion resistance
corrosion resistance of the resultant product. and good mechanical properties they were
Twenty years later, however, iridium was readily workable and of fairly high electrical
still regarded as a troublesome impurity in resistance. No internal transformations were
platinum, but the researches of Sainte-Claire recognised in those days and the alloys were
Deville and Debray (3) did much to dispel established as materials par exceZZence for
this illusion. On behalf of the Russian instrument technology.
Government they carried out extensive trials Iridium-platinum was selected, therefore,
at the French Mint to determine the suit- as the logical material for the construction of
ability of iridium-platinum alloys for coinage. of the International Metre (5). A 250
The crude platinum for these experiments kilogramme ingot for this purpose was cast
came from the mines of Prince Demidoff at on May 13th, 1874, at the Conservatoire des
Nijne Tagilsk and contained 92.55 per cent Arts et MCtiers in Paris. The platinum,
of platinum, 7 per cent of iridium and 0.45 weighing 225 kilogrammes, came from
per cent of rhodium. Alloys prepared from Johnson and Matthey, the iridium being
this material were greatly superior to pure supplied by the Director of Mines, St.
platinum in both strength and corrosion Petersburg. Henry Tresco and George
resistance. The alloy obtained by directly Matthey made the melt in a lime block under
fusing the crude platinum was found to be the general supervision of Sainte-Claire
well suited for coinage, as were the synthetic Deville and Debray and the ingot, which
alloys containing up to 20 per cent of iridium. contained 10 per cent of iridium, was prac-
The 15 per cent alloy was extensively em- tically perfect and very uniform in composi-
ployed for the construction of chemical plant. tion.
Nickles (4), in a letter to the American Prototype metres and geodesique rules

Platinum Metals Rev., 1960, 4, (l), 18-26 18

were in subsequent years manufactured by Iridium-platinum was sometimes used for
George Matthey in accordance with the electrical standards. Klamenri? (9) concluded
requirements of the Comitt Internationale in 1885 that of all the materials available at
des Poids et Measures and the Association the time platinum-silver and platinum-
Geodesique Internationale. Details of the iridium best fulfilled the service requirements
melting, forging and rolling processes adopted of standard resistors. Two iridium-platinum
during this work were published in 1879 (6). coils were included in the group of British
The unique combination of strength and Association resistance standards constructed
high density made the alioys very suitable for by Matthiesen in 1865 (10). The iridium
the production of standard weights. The 10 alloy had a higher temperature coefficient
per cent iridium alloy was used for the than platinum-silver but its resistance varia-
National Kilogramme of France described tions, revealed by careful testing over a total
by Violle in 1889 (7). Prototype kilogrammes period of 67 years, were considerably less
were rigorously tested before acceptance by capricious (I I).
the International Commission of the Metre.
Very high pressures were applied to ascertain The Constitutional Diagram
whether such treatment had any effect upon It was generally believed until compara-
the apparent density. Material submitted by tively recently that platinum and iridium
Johnson and Matthey successfully withstood when alloyed synthetically were completely
this proving treatment, the apparent specific miscible in all proportions. Nearly all the
gravity of eleven standard kilogrammes experimental evidence appeared to confirm
submitted falling within the range 21.548 to this view. Feussner and Miiller’s melting
21.552 g/cm3. point determinations (12), obtained by optical

2500

2000

.* o FEUSSNER AND MULLER

w 0 RAUB AND PLATE
a (RESISTIVITY)
3
c A RAUB AND P L A T E
2 IS00 (DILATOMETER)
w
a 0 RAUB A N D PLATE (x RAY)
2
c B MASING. ECKHARDT AND
KLOleER

1000

500

Pt ATOMIC PER C E N T I R I D I U M Ir

Fig. 1 Equilibrium diagram of the iridium-platinum system

Platinum Metals Rev., 1960, 4, (1) 19

 3.92 (IS), who published their
tn results in 1940, used an
c
z3 3.90 alternating current elect-
Y
X
rolytic etching technique
which revealed with great
3.88
a
w
facility the structure of
k- alloys containing up to
W
2 3.86 40 per cent of iridium.
a
$ Hot forging and heat
W
2 3.84 treatment for long periods
c
t
at temperatures up to
U
A 1725°C were required to
3.82
20 40 60 80 100 eliminate the heavily
ATOMIC PER CENT IRIDIUM cored structure previously
reported by Nemilow.
Fig.2 Variation of lattice parameter with iridium concentration f o r All the micro-structures
alloys quenched from 1700°C (Raub and Plate) shown in this paper were
of typical solid solutions.
methods, lay on a smooth curve which Zvyagintsev, Raikhstadt and Vladimirova
suggested the existence of a continuous range (16) studied the mutual diffusion of platinum
of solubility below the solidus. Nemilow (13), and iridium in the solid state and concluded
who studied the whole system metallo- that platinum diffused into iridium faster than
graphically had previously arrived at the iridium diffused into platinum. Electrical
same conclusion. He prepared alloys by resistivity measurements showed that fairly
oxy-hydrogen melting and drew those con- homogeneous solid solutions could be pro-
taining up to 20 per cent by weight of iridium duced by normal powder metallurgical
into wire. Electrical resistivity measurements processes.
were made upon these wire samples, and
temperature coefficient determinations on cast The Miscibility Gap
and homogenised specimens covering the The behaviour of iridium-platinum alloys
entire composition range. Time and tempera- was, however, incompatible with the view
ture, it was concluded, had little effect upon that no transformations occurred. As early
the electrical properties, which were typical as 1886, for example, Le Chatelier (17)
of those expected from simple solid solution observed transformations in a 20 per cent
alloys. Heavy coring was observed in alloys iridium-platinum alloy which were accom-
containing more than 20 per cent by weight of panied by an absorption of heat at 700°C and
iridium. None of the heat treatments adopted at a second temperature midway between the
completely eliminated this coarse dendritic melting points of gold and silver. Thermo-
structure. electric studies by Barus in 1892 (29) did not,
Weerts (14)~in confirmation of previous however, reveal any e.m.f. discontinuities at
evidence, showed that the lattice parameter these points. Geibel (18) reported in 1911
of quenched alloys varied with concentration that the tensile strength of wires containing
in a perfectly linear manner. more than 10 per cent of iridium could be
Nemilow experienced great difficulty in considerably increased by heat treatment at
etching his alloys, and for those containing 750°C and suggested that the effect was caused
more than 40 per cent of iridium resorted to by an allotropic modification in the iridium.
immersion in a fused bath of manganese Nowack (IS), commenting on these findings
dioxide and sodium chloride. Raub and Buss in 19303 attributed the phenomenon to

Platinum Metals Rev., 1960, 4, (1) 20

precipitation hardening
although he had no evi-
dence to support his
hypothesis.
Ten years later Masing,
Eckhardt and Kloiber (I)
were still unable to dem-
onstrate the existence of
a second phase. These
investigators carried out
resistance measurements
at temperatures up to
I 150°C. The resistance-
temperature curves had
WEIGHT PER CENT I R I D I U M
sharp discontinuities pro-
viding evidence of trans- Fig. 3 Electrical resistivity and temperature coeficient of resistance of
iridium-platinum alloys
formations at tempera-
tures in good agreement
with those obtained from the results of tensile or in vacuum. The slow rate of establish-
testing. X-ray examination provided no ment of equilibrium made the decomposition
evidence of precipitation, however. It was process difficult to follow by X-ray methods,
concluded that the changes in physical pro- and because of the small differences in lattice
perties were caused by an order-disorder constants between platinum and iridium
reaction which was not revealed because of X-ray determinations of the true solubility
the similar scattering power to X-rays of limits were not particularly accurate. Elec-
platinum and iridium atoms. mcal resistance measurements provided the
The true nature of the platinum-iridium most accurate phase boundary determina-
diagram was finally elucidated by Raub and tions.
Plate (zo), who published their results in 20
1956. These investigators provided definite
metallographic evidence of a miscibility gap
which had its highest point at 975°C and
50 atomic per cent of iridium. At 700°C the 15

gap extended from 7 to 99 atomic per cent

of iridiunn. Microscopic evidence of a duplex In
I-

structure over this composition range was

?
confirmed by the results of electrical resist- 5 10
ivity, X-ray diffraction] and dilatometric -J
I
measurements.
Previous workers had not arrived at these
conclusions for the simple reason that they 5

had not annealed their specimens for long

enough periods. Raub and Plate showed that
heat treatment periods of the order of one
year were required to establish some sem- 1
0 20 30
blance of equilibrium in the two-phase region. WEIGHT PER CENT I R I D I U M

In order to avoid loss of iridium due to Fig. 4 Thermal e.m.f. between iridium-platinum
oxidation, heating was carried out in argon alloys and pure platinum

Platinum Metals Rev., 1960, 4, (1) 21

 22.5 50 per cent alloy. The
table below, taken from
v
Raub and Plate, gives the
2 concentration limits of
I
22.0 +
a the duplex region for
m
5 various temperatures
\ between 700 and 976°C.
21.5
5I The equilibrium dia-
> gram shown in Fig. I is
cul
2 based upon the findings
W
P of Feussncr and Miiller
21.0 (12), Masing, Eckhardt
and Kloiber (I), and
Raub and Plate (20).
20 40 60 80 100
WEIGHT PER CENT IRIDIUM Fig. 2 illustrates the
Fig. 5 Density and instantaneous linear expansion coeficients of linear variation of lattice
iridium-platinum alloys parameter with iridium
concentration for alloys
Hardness and electrical conductivity quenched from 1700'C (20).
changes occurred after heat treatment periods
of several hours. The development of a reason- Electrical Properties
ably well-defined duplex microstructure in Fig. 3 shows that the electrical resistivity,
the 50 atomic per cent iridium alloy required after a rather rapid initial rise, reaches a fairly
360 hours of heat treatment at 800°C. X-ray flat maximum of 32 to 34 microhm-cm at an
diffraction examination first detected the iridium concentration of approximately 40
second phase after I440 hours at 8oo0C, but per cent. Differences in purity probably
the lattice parameters of the two phases explain the slight differences between the two
approached constancy only after 3600 hours sets of values quoted. Although Raub and
of heat treatment. After goo0 hours at 600°C Plate illustrate the resistivity of the 50
no sign of decomposition was evident in the atomic per cent alloy as approximately 62
microhm-cm at 20"C, this value requires
verification.
Limiting solubility concentrations of Nemilow's temperature coefficient data
iridium-platinumalloys agree closely with recent determinations made
(Atomic percentage of iridium)
in the Johnson Matthey Research Labora-
Method of Determination tories.
Temper The alloys have a positive thermal e.m.f.
ature Resist- Dilato- X-Ray
"C ance metric Diffraction with respect to pure platinum. Fig. 4
illustrates the effect of composition upon the
976 50 e.m.f.s generated at 700'C and 1200'C (21).
974 50 Above IOOO~C volatilisation and oxidation
958 40 losses render iridium-platinum alloys less
946 40
stable than rhodium-platinum alloys for high
922 30
temperature measurement.
910 20
900 40 and 74
aoo 10
Physical and Mechanical Properties
26-40 and 72-86
700 7-28 and 60 -99 The specific gravity curve, shown in Fig. 5,
displays a slight positive displacement from

Platinum Metals Rev., 1960, 4, (1) 22

 1- I 500
linearity although the effect is not pro-
nounced. The second curve in this illustra-
tion shows an approximately uniform decrease 500
of linear expansion coefficient with iridium
concentration (20).
The mechanical properties of the alloys
400 f
increase rapidly with iridium content as W
2
shown by Fig. 6 (21). With 30 per cent of a
<
iridium the ultimate tensile strength of 300
I
u)
K
quenched test pieces rises to 56 tons per W
Y
square inch. The hardness data show that the I!
>
maximum mechanical properties of the series 200
are obtained with iridium contents of approxi-
mately 60 per cent. The hardness and tensile
strength of all the alloys increases very rapidly 100
with the degree of cold working; the tensile
strength of hard drawn 20 per cent iridium-
platinum wire, for example, frequently
20 40 60
exceeds IOO tons per square inch. Fig. 7
WEIGHT PER CENT I R I D I U M
illustrates the effect of cold rolIing upon the
hardness of the 2 0 and 25 per cent iridium Fig. 6 Ultimate tensile strength, limit of pro-
portionality and hardness o j quenched iridiurn-
alloys. A reduction in thickness of 70 per platinum ulZoys
cent increases the hardness of the 25 per cent
alloy from 246 to 370 V.P.N. (21). heat treatment for 16 hours illustrates the low
Very high hardness values can be developed rate of precipitation in this alloy system (21).
by quenching and subsequently ageing alloys
containing more than 10 per cent by weight Workability
of iridium. Fig. 8 illustrates the hardness Alloys containing up to 40 per cent of
changes which result when alloys quenched iridium have been hot forged for many years,
from 1400OCare subsequently aged at 700°C. although the ease of working decreases
The steady rate of hardness increase after rapidly when the iridium content exceeds
20 per cent. In 1879 for example George
350 o , I Matthey (6) reported that although the 25
per cent iridium alloy could be worked into
sheet and wire great difficulty was experienced
at higher percentages, the 50 per cent alloy
being unworkable. W. C. Heraeus ( 2 2 ) was
able, in 1891,to produce cold drawn 40 per
cent iridium-platinurn wire but regarded this
composition as a practical working limit.
The ease of worldng increases with the
purity of the materials employed, and argon
arc melted material appears to be more
malleable than that melted in the open. Small
samples of sheet capable of being subsequently
PER CENT REDUCTION IN THICKNESS rolled have been produced by carefully hot
forging at temperatures just below the melting
Fig. 7 Work-hurdening curues of iridium-
platinum alloys point of the alloy, argon arc melted ingots

Platinum Metals Rev., 1960, 4, ( 1 ) 23

 chloride in hydrochloric acid facilitates the
solution of this material (IS).
500
Alloys containing more than about 5 per
cent of iridium oxidise when heated in air.
The bluish film which develops above 700°C
400 disappears at temperatures above 1200°C
u)
Q
W
leaving a clean matt surface upon the alloy,
z Iridium-platinum thermocouples were shown
0
4 by Burgess in 1908 (24)to be less stable than
u)
300 those of rhodium-platinum. Crookes in 1912
a
W (25)emphasised that the volatility of iridium
->
Y
U in air was many times higher than that of
platinum, and Wise, at a later date, quoted an
200
evaporation ratio, a t 1227°C of one hundred
to one. The high evaporation losses from
heated iridium-platinum alloys can, in fact, be
attributed to the volatility of iridium oxide.
5 10 IS 20
The table below, taken from Raub and Plate
TIME O F AGING - HOURS
(26) summarises the results of some tests
Fig. 8 Age-hardening curves of iridium-platinum made upon sheets of iridium-platinum alloys,
alloys quenched from 1400°C and subsequently
heat treated at 700°C 0.5 mm thick, heated for 23 hours at IIOO"C
in a current of oxygen. The weight loss of the
containing up to 60 per cent of iridium (21). alloy with 10per cent of iridium amounts to
Raub and Plate in their recent work employed 2.8 per cent of the iridium content, while the
drawn 50 per cent iridium-platinum wire (20). corresponding value for the 40 per cent iridium
Such alloys are, however, even more difficult alloy is 46.6per cent.
to work than pure iridium, and fabrication Fig. 9 illustrates some results obtained at
has so far been restricted to purposes of 900°C. SmalI sheet samples were suspended
research. for various periods in a furnace through
which an oxygen current of 0.4 litre per
Corrosion and Oxidation Resistance minute was passed. The weight losses at
Iridium additions increase considerably 900°C are less than a tenth of those at I 103°C.
the corrosion resistance of platinum. At a The sudden increase in volatility when the
very early date it was appreciated that iridium- iridium content exceeds 20 per cent is
platinum boilers used for sulphuric acid
concentration resisted the attack initiated by Evaporation losses from iridium-platinum
alloys heated in a current of oxygen at
nitrous compounds better than those of pure 1100°C for 23 hours
platinum. Heraeus (23)stated for example (After Raub and Plate)
I
that the rate of corrosion of the 10 per cent
iridium-platinum alloy in sulphuric acid was
only 58 per cent that of the pure metal. The
resistance to halogen attack increases with Iridium
Decrease
in wt.
Evaporation loss related
t o iridium content

mgig of
I
iridium content in a similar fashion. The Wt.%) (mg/cm2) alloy content
40 per cent iridium alloy is virtually un-
10 I .35 2.8
attacked by boiling aqua regia but can be 20 13.99 29.2 14.6
slowly etched by nascent chlorine at elevated 30 58. I 0 123.6 41.2
temperatures. An alternating current process 40 89.29 186.4 46.6
utilising a saturated electrolyte of sodium I
I

Platinum Metals Rev., 1960, 4, (1) 24

 associated with the fact that the 30 and 40 per a value of A H,,, -41 h 10Kcals was arrived
cent alloys are, at 900"C, well within the at. At very high temperatures it was suggested
duplex region. Raub and Plate postulated that evaporation occurred via an Ir,O
that under such conditions most of the molecule, since this was the only one having
evaporation occurred from the iridium-rich a positive entropy of formation from atomic
phase. The evaporation mechanism suggested oxygen. Iridium-platinum alloys melt before
was simple volatilisation of the oxide formed such conditions arise.
when metal atoms diffused to the surface of
an oxygen layer adsorbed on the solid metal. Applications
The rather limited thermodynamic data Electrical contact applications account for a
support this hypothesis. Holborn and Austen fair proportion of the iridium-platinum alloys
(27) reported that the volatility of iridium at supplied to industry. The high hardness and
1670°C increased less rapidly than the first low contact resistance of the 10 and 20 per
power of the oxygen pressure. Raub and cent iridium alloys make them particularly
Plate demonstrated that the rate of volatilisa- suitable for low current, low pressure
tion of iridium-platinum alloys was practic- applications where dust contamination pre-
ally independent of oxygen pressure except judices the performance of softer materials.
when this was very low indeed. This In medium current applications when resist-
behaviour suggests the volatilisation of an ance to hammering becomes important alloys
oxide rather than the dissociation of an un- containing up to 20 per cent of iridium are
stable oxide. Brewer (28) assumed the oxide sometimes employed. A recent study showed
to be IrO, and estimated A H,,, for the that material transfer from the cathode was
expression proportional to the number of coulombs
passed through the arc and decreased steadily
IrO,(solid) =IrO,(gas)
with iridium contents up to 35 per cent (30).
to be 85 57Kcals. For the reaction Pfann (31) has shown that interesting results
Idsolid)+ O,(gas) =IrO,(gas) can be achievcd by pairing a negative 20 per
cent iridium-platinum contact with a positive
contact of pure gold. With medium currents
the material transfer caused by an asym-
metrical molten bridge was found to balance
the other transfer processes, thus minimising
2
contact wear.
N
Precision resistors and slide wire potentio-
: meters utilise considerable quantities of 10
b4
E
c and 20 per cent iridium-platinum wire. The
I
-u
w
combination of moderate resistivity, low
s 6 temperature coefficient and high corrosion
t resistance exhibited by these alloys is of great
value in the construction of high quality
transducers. In the temperature measure-
ment field we find the 10 per cent iridium-
platinum alloy used in combination with a
10
10 20 30 40
40 per cent palladium-gold wire. This
TIME IN HOURS thermocouple, capable of generating 34
millvolts at 6oo0C, has wide applications at
Fig. 9 Evaporation losses from iridium-platinum
alloys heated i n a current of oxygen at 900°C moderately high temperatures.
(Raub and Plate) The bridge wires used in electric detonators

Platinum Metals Rev., 1960, 4, (1) 25

fuses, and cartridge igniters must be very freedom from corrosion is essential the age
strong and resistant to corrosion, and iridium- hardening properties of the 20 per cent
platinum alloys have long been preferred for iridium alloy render it very suitable for the
such applications. Needles used for the initial production of high quality hairsprings.
perforation of diamond dies by electro- Little is known about the creep properties
sparking are sometimes made from the t o per of iridium-platinum at high temperatures.
cent iridium alloy. Some tests by Stauss (32) suggested that the
The elasticity and high mechanical pro- 10 per cent iridium alloy was slightly inferior

perties of alloys containing up to 30 per cent to the 10 per cent rhodium alloy, but the
of iridium can be successfully employed in results were not conclusive. To avoid fracture
instrument suspensions. Over the range at I I O O O C , the applied stress, it was concluded,
O-IOO"Cthe modulus of rigidity of the 10 per should not exceed 1.5 per cent of the normal
cent iridium-platinum alloy decreases by room temperature tensile strength or 6 per
only 0.8 per cent (21). Where complete cent of the short term strength at IIOO'C.

References
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2 A. Gaudin .. .. . . . . Compt. rend., 1838, ( 6 ) , 862
3 M. H. Jacobi . . .. . . .. Compt. rend., 1859, 49, 896
J. Pelouze .. .. . . , . PoZyt. J. (Dingler), 1860, 155, 118
H. Sainte-Claire Deville and H. Debray N . arch. Sci. phys. nat., 1873, 48, 45
H. Sainte-Claire Deville .. .. Compt. rend., 1875, So, 589
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5 H. Morin .. . . .. .. Compt. rend., 1874, 7 8 , 1502
6 G. Matthey .. .. .. .. Proc. Roy. SOC.,1879, 28, 463
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8 J. S. Stas .. .. * . . . J . phurm. chim., 1885, 12,(5), 45
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1888, 12, 1080)
I0 British Association Report on Electrical Standards,
Fourth Report, 1865
I1 British Association Report on Electrical Standards,
1932,P. 417
12 0. Feussner and L. Miiller .. .. Heraeus Festschrift, Hanau (Main), 1930, pp. 14-15;
Ann. Physik, 1930, 7, 9
13 W. A. Nemilow .. .. .. Annals. Inst. Platine, (U.S.S.R.), 1929, 7, 13-20
Z. anorg. allgem. Chem., 1932, 204, 41
14 J. Weerts .. ..
.. .. Z. Metallkunde, 1932, 24, 139
15 E. Raub and G. Buss . . .. .. Z.Elektrochem., 1940, 46, (3), 195
16 0. E. Zvyagintsev, A. G. Raikhstadt Zhur. Priklad. Khim., 1944, 17, 22-30
and M. A. Vladirnirova
17 H. Le Chatelier .. .. .. Bull. SOC.Chim., 1886, 45, (2), 482
18 W. Geibel .. .. * . .. Z . anorg. allgem. Chem., 1911, 70, 249
19 L. Nowack . . .. . . .. Z . Metallkunde, 1930, 22, 140
20 E. Raub and W. Plate . . .. .. Z. Metallkunde, 1956, 47, 688493
21 Johnson Matthey Research Laboratories Unpublished data
22 W. C. Heraeus . . .. .. .. Z. Instrum. Kunde, 1891, 11, 262
23 W. C. Heraeus . . .. . . .. Z . angew. Chem., 1892, 34
24 G. K. Burgess . . .. .. . . Bull. Standards, 1908, 5, 199-225
25 W. Crookes .. .. .. .. Proc. Roy. SOC.,I 9 12, A, 86,46 1-476
26 E. Raub and W. Plate . . .. .. Z. Metallkunde, 1957, 48, 529
27 L. Holborn and L. W. Austin .. Phil. Mag., 1904, 7, (6), 388
28 L. Brewer .. .. .. .. Chemical Reviews, 1953, 52, 1-75
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30 W. B. Ittness and H. B. Ulsh.. .. Proc. Inst. Elec. Eng., Part B, 1957, 104,63-68
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Platinum Metals Rev., 1960, 4, ( 1 ) 26