Heat Treat Doctor 11.

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Daniel H. Herring | 630.834.3017 | [email protected]

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Using Partial Pressure in Vacuum Furnaces

t is of primary importance to understand vapor pressure where Qmax = evaporation rate (g/cm3-sec), Pv = vapor pres-
in the vacuum heat treatment of metals. Operating in sure (torr), T = temperature (K) and M = molecular weight.
vacuum can often lead to significant evaporation, or In vacuum furnaces, metals tend to volatize at tempera-
“boiling away,” of elemental constituents in the materi- tures below their melting points. Table 1 shows this rela-
als being processed, affecting surface integrity and in some tionship for a number of common metals. The longer parts
cases altering the chemical composition of the base (or filler) are held at the temperature and at the vacuum level
metal. One way to overcome this problem is to shown, the greater the loss of the metallic element by
introduce a gas partial pressure higher than that evaporation. Where the element is part of a metal alloy
of the material’s vapor pressure. Different gas system the vapor-pressure relationship changes (total
choices, introduction methods and controls are vapor pressure of the alloy is the sum of the vapor pressures
available to the heat treater. The natural ques- of each constituent times the percentage in the alloy,
tions are how and when should they be used? Let’s although this relationship has been debated by those
learn more. knowledgeable in the field).
For example, processing aluminum, cadmium, magnesium,
Vapor pressure manganese and zinc or their alloys at temperatures as low as
The vapor pressure of a material is the partial pres- 400˚C (750˚F) may be marginally or totally impractical. This
sure present in the atmosphere which surrounds it. In other is why processing brass (Cu-Zn alloy) is normally not done in
words, the vapor pressure tells us how much vapor a material a vacuum system, or if it is, it is carried out at partial pressures
will produce; a high vapor pressure means that the material will near atmospheric. As the temperature increases, fewer materi-
readily evaporate. Every material has a characteristic vapor als can be run without being affected.
pressure associated with it, which varies with temperature; the Stainless and tool steels and more exotic alloys often are
vapor pressure increases with increasing temperature. processed in vacuum. Chromium present in these materials
All metals evaporate as a function of temperature (first- evaporates noticeably at temperatures and pressures within
order effect) and vacuum level (second-order effect). Equation normal heat treatment ranges. Processed above 990˚C
1 allows the determination of the evaporation rate (Q), and (1815˚F), chromium will vaporize if the vacuum level is less
shows that the vapor pressure/temperature relationship is near- 1 × 10-4 torr and the parts are held for a prolonged time. Heat
ly logarithmic: treaters often observe a greenish discoloration (chromium
oxide) on the interior of their vacuum furnaces, the result of
Qmax=0.058Pv M
chromium vapor reacting with air leaking into the hot zone.
T
Otherwise, the evaporation deposit is bright and mirror-like.
To avoid this, an operating partial pressure between 0.3 and 5
torr is typical for most chromium-containing parts.
For vacuum brazing (silver, copper, nickel), depletion of the
filler metal alloy can be avoided by raising the pressure in the
furnace to a level above the vapor pressure of the alloy at braz-
ing temperature. For example, copper, having an equilibrium
vapor pressure at 1120˚C (2050˚F) of 1 ×10-3 torr is usually run
at a partial pressure between 1 and 10 torr. Nickel brazing nor-
mally is done in the 10-3 to 10-4 torr range. However, in the
10-5 to 10-6 torr range, you run the risk of losing some nickel,
which has an equilibrium vapor pressure of 1 × 10-4 torr at
1190˚C (2175˚F).

Which gases can we use?

Argon, hydrogen and nitrogen are the most common partial
pressure gases. Often, argon is preferred as it tends to “sweep”
the hot zone; that is, the heavy molecule tends to reduce evap-
Load of flat-plate heat exchangers ready for brazing at 5 torr nitrogen oration compared with nitrogen and hydrogen. Specialized
partial pressure at 1120˚C. Photo courtesy of Solar Atmospheres Inc. applications such as those in the electronics industry may use

10 November 2005 – IndustrialHeating.com

Heat Treat Doctor 11.05 10/21/05 12:16 PM Page 12

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helium or even neon (if an ionizing gas vent oxidation of sensitive process work or ed by gas species, because they are calibrat-
is needed). Gases having a minimum for furnace/fixture bakeout/cleanup cycles. ed for air. It is not uncommon to believe,
purity of 99.99% and a dew point of Embrittlement by hydrogen is a concern for example, that you are running an argon
-60˚C (-76˚F) or lower should be specified. for certain materials (e.g., Ti, Ta). partial pressure at 1 torr when in reality
Certain cautions are in order. For exam- you are running at 0.4 torr, or with hydro-
ple, nitrogen may react with certain stain- Measurement and control gen (or helium) that you are at 10 torr
less steels and titanium-containing materi- It is critical to know the exact pressure, when you are really at 1 torr. Absolute-
als resulting in surface nitriding. In the flow and type of gas being injected into the pressure gages, such as the BOC Edwards
case of hydrogen, the normally near neu- vacuum furnace so the process being run is Barocel® (Wilmington, Mass.; www.boc
tral vacuum atmosphere can be sharply under control. Thermocouple gages typi- edwards.com/industrial) should be used to
shifted to a reducing atmosphere to pre- cally found on vacuum furnaces are affect- determine precise partial pressure values.
For flow accuracy, flowmeters should
Table 1 Vapor pressures for selected elements have a micrometer needle valve installed
Element Temperature (°C) at which specific vapor pressure (torr) exists
in the downstream line. On many units,
0.001 0.01 0.1 1.0 10 100 760
the gas is pulsed in using a solenoid valve
Al 889 996 1123 1279 1487 1749 2327
and set-point control on the vacuum gage,
Be 1029 1212 1367 1567 1787 2097 2507
similar to continuous flow with a needle
B 1239 1355 1489 1648 3030 3460 2527
valve installed. Also, it is extremely impor-
Cd 220 264 321 394 484 611 765 tant to inject the partial pressure gas
Ca 528 605 700 817 983 1207 1482 directly into the hot zone so the gas does
C 2471 2681 2926 3214 3946 4373 4552 not short circuit the work area.
Cr 1090 1205 1342 1504 - - 2222
Co 1494 1649 1833 2056 2380 2720 3097 Summary
Cu 1141 1273 1432 1628 1879 2207 2595 Partial pressure atmospheres are required in
Ga 965 1093 1248 1443 1541 1784 2427 many heat treating and brazing operations
Ge 1112 1251 1421 1635 1880 2210 2707 to achieve the desired results. Introduction
Au 1316 1465 1646 1867 2154 2521 2966 of the partial pressure gas into the furnace
Fe 1310 1447 1602 1783 2039 2360 2727 hot zone at one or more locations and con-
Pb 625 718 832 975 1167 1417 1737 trolling the partial pressure injection gas
Mg 383 443 515 605 702 909 1126 stream as a continuous flow rather than
Mn 878 980 1103 1251 1505 1792 2097 trying to operate at a specific pressure are
Hg 18 48 82 126 184 216 361 critical considerations. The choice of par-
Mo 2295 2533 2880 3102 3535 4109 4804 tial pressure gas is also important both from
Nd 1192 1342 1537 1775 2095 2530 3090 a cost and quality standpoint. IH
Ni 1371 1510 1679 1884 2007 2364 2837
Pd 1405 1566 1759 2000 2280 2780 3167 Bibliography
P 160 190 225 265 310 370 431 • Jones, W.R., Partial Pressure Vacuum
Pt 1904 2090 2313 2582 3146 3714 3827 Processing – Part I and II, Ind. Htg,
K 161 207 265 338 443 581 779 Sept./Oct., 1997
Re 2790 3060 3400 3810 - - 5630 • Vacuum Technology: Practical Heat Treating
Rh 1971 2149 2358 2607 2880 3392 3877 and Brazing, R. Fabian, Ed., ASM Intl, 1993
Se 200 235 280 350 430 550 685 • Practical Vacuum Systems Design, The
Si 1223 1343 1585 1670 1888 2083 2477 Boeing Company
Ag 936 1047 1184 1353 1575 1865 2212
• William Jones, Solar Atmospheres Inc.,
Na 238 291 356 437 548 696 914
private correspondence
• R. Houghton Jr., Hayes Heat Treating,
S 66 97 135 183 246 333 444
private correspondence
Ta 2820 3074 3370 3740 - - 6027
Sn 1042 1189 1373 1609 1703 1968 2727
Additional related information may be found
Ti 1384 1546 1742 1965 2180 2480 3127 by searching for these (and other) key
U 1730 1898 2098 2338 - - 3527 words/terms via BNP Media LINX at
V 1725 1888 2079 2207 2570 2950 3527 www.industrialheating.com: vacuum furnace,
Zn 292 343 405 487 593 736 907 vacuum heat treating, vacuum brazing, vapor
Zr 1818 2001 2212 2459 - - 3577 pressure, partial pressure, evaporation rate.

12 November 2005 – IndustrialHeating.com