A]I)S TO PRODUCTION ENGINEERS

SALT BATHS FOR HEATING METALS

E. A. SmolTnikov UDC (047): 621.78

In the past ten y e a r s the n u m b e r of salt baths used in heating metals for heat treatment has i n c r e a s e d
in all branches of industry and salt baths have also come into use for heating metals to forging and extrusion
t e m p e r a t u r e s [1], and for aluminizing, soldering, and cleaning [2].
The design of salt baths has been improved and perfected [3, 4], the size and power have been in-
c r e a s e d , and new apparatus and complex automatic production lines have been developed for heat treating
various parts that c o n s i s t of a s e r i e s of s a l t baths for different purposes [5, 6].
New compositions of salts have been developed for the baths and also r e c t i f i e r s for purifying them
[7]. Methods of monitoring the baths during use have been developed and perfected [8].
In recent y e a r s a good deal of work has been done on the principles of heat treating metals in fused
salts [9, 10] and on the theoretical basis and practical techniques of heat treating different parts in salt
baths [11].

The Characteristics of Heating in Salt Baths

The c h a r a c t e r i s t i c feature of heating in salt baths is the even distribution of the t e m p e r a t u r e through-
out the bath, even heating of the part, the high heating rate - and thus high productivity - of salt baths; the
possibility of local heating of one end of a part and obtaining a difference in hardness along the length of the
part; complete or partial protection of the s u r f a c e of the part against the atmosphere and prevention of scale
formation, and, with the p r o p e r salts, prevention of d e c a r b u r i z i n g of the surface.
Since the density of fused salts [12] is far s m a l l e r than that of the metal parts and the parts a r e easily
i m m e r s e d in the bath, salt baths, unlike lead baths, p e r m i t heating of long p a r t s held in tongs or with special
devices in a vertical position. F o r this r e a s o n the warping due to
the weight of the part itself is eliminated and distortion f r o m
quenching is reduced. Heating in salt baths is facilitated by such
equipment as multiplace devices to prevent contact of one part
a b
with another and ensure even wetting of the parts on all sides [11].
The use of such devices facilitates mechanization and automation
of heat t r e a t m e n t p r o c e s s e s , makes it simple to t r a n s f e r parts
c d e from one bath to another, and permits constant holding times for
identical p a r t s .
Since fused salts can be s t i r r e d , the t e m p e r a t u r e of salt
baths can be controlled within fairly n a r r o w limits. The presence
of a film of salts on parts withdrawn f r o m the bath protects them
Fig. 1. Diagram of various salt baths
against oxygen in the air during subsequent cooling. These ad-
a n d p l a e e m e n t of e l e c t r o d e s , a, b, g)
vantages and c h a r a c t e r i s t i c s of heating in fused salts permit wide
Baths w i t h t h r e e stacks of flat e l e c -
use of salt baths for heat t r e a t m e n t of parts, consistent results in
t r o d e s ; c) bath with three flat e l e c t r o d e s
operation, obtaining the n e c e s s a r y quality, and eliminate or sharply
lowered into the salts; d, e) baths with
reduce the number of r e j e c t s from overheating, decarburizing,
t h r e e round e l e c t r o d e s lowered into the
reduction of the hardness below the allowable limit, distortion,
salts; f) bath with six p a i r s of flat e l e c -
and cracking.
t r o d e s lowered into salts.
All-Union S c i e n t i f i c - R e s e a r c h I n s t r u m e n t Institute. T r a n s l a t e d f r o m Metallovedenie i T e r m i e h e -
skaya Obrabotka Metallov, No. 11, pp. 71-78, November, 1970.

9 1971 Consultants Bureau, a division of Plenum Publishing Corporation, 227 West 17th Street, New York,
N. Y. I0011. All rights reserved. This article cannot be reproduced for any purpose whatsoever without
permission of the publisher. A copy of this article is available from the publisher for $15.00.

972
 Ka The Classification of Salt Baths and

Their Purposes
.. / ! i !
x /i ! I !
/ I I I I I
._-~. . . . .~_-_.___+-__~---~-_-~ Salt baths, like heat t r e a t m e n t f u r n a c e s , differ in the means
/i ! !
[ i ! i by which they are heated [12,13], operating t e m p e r a t u r e s , purpose,
x,./i I ', I I
I I I I design, and the composition of the salts [7].
I I I

#;> 1 2 3 5 6 days
In wide use at the p r e s e n t time are electrode salt baths of
various types, crucible e l e c t r i c baths with external (resistance)
elements and internal elements ( p r i m a r i l y tubular electric heaters).
N With special instruments and devices the t e m p e r a t u r e of the bath
r~ can be controlled automatically within limits of ~5~
24 28 ~? 36 00 44,h
Salt baths are used for heating p a r t s to t e m p e r a t u r e s of
140-1350~ Salt baths can be classified [14] as h i g h - t e m p e r a t u r e
(1000-1350~ m e d i u m - t e m p e r a t u r e (720-950~ and l o w - t e m -
p e r a t u r e (140-700~ However, in view of the difference in p u r -
i
I
iI
i i I
l ..i : pose, it s e e m s advisable to subdivide the l o w - t e m p e r a t u r e baths
1 2 3 4 5 G days - t h o s e operating at 120-380~ and those operating at 400-700~
Operating time
H i g h - t e m p e r a t u r e baths, containing up to 100% BaC12, are used
C
p r i m a r i l y to heat h i g h - s p e e d and other high-alloy steels f o r final
Fig. 2. Change in the decarbur-
quenching, but are also used in automated heat t r e a t m e n t lines
izing activity of salt baths during
for p r e l i m i n a r y heating of these s a m e steels to 1050-1070~ in-
operation, a) Operation without
stead of the commonly used 850~ in baths containing 78% BaCI 2
rectification; b) with periodic
+ 22% NaCI.
rectification; c) BM5 mixture
with periodic rectification. - - - ) This use of h i g h - t e m p e r a t u r e salt baths has proved to be
P e r m i s s i b l e value of K a. v e r y efficient, since the elevated t e m p e r a t u r e of p r e l i m i n a r y h e a t -
ing reduces the time of final heating to quenching t e m p e r a t u r e ,
and the absence of sodium chloride in the bath eliminates smoking
of the bath during final heating and the resultant e r r o r in measuring the bath t e m p e r a t u r e with a radiation
pyrometer.

M e d i u m - t e m p e r a t u r e salt baths are used for various p u r p o s e s - f i n a l heating to quenching t e m p e r a -

ture of c a r b o n and low-alloy steels, p r e l i m i n a r y h e a t i n g in hardening parts of h i g h - s p e e d and other high-
alloy steels, annealing o r n o r m a l i z a t i o n of blanks, and heating of billets for forging or extrusion. L o w - t e m -
p e r a t u r e salt baths operating at 120-380~ are used mainly for tempering parts of c a r b o n and low-alloy
steels and also for cooling in stepped and i s o t h e r m a l quenching.
Salt baths operating at 400-700~ are c o m m o n l y used for t e m p e r i n g p a r t s of high-alloy steels and
also cooling such p a r t s in stepped quenching.

Electrode Salt Baths and Electrode Materials

The type and design of a salt bath depend on its purpose.

Along with increasing use in the past ten y e a r s we have seen i n c r e a s e s in the size of the bath, the
power, and the efficiency. Salt baths with a power of 35 kV are now r a r e ; m o r e often the power is 60, 75,
100, and even 160 kV.
The shape of salt baths and the position of the e l e c t r o d e s have changed considerably. Along with baths
in the f o r m of a r e g u l a r s i x - s i d e d p r i s m with e l e c t r o d e s on three sides (Fig. la), square salt baths with
e l e c t r o d e s on t h r e e sides are also widely used (Fig. lb). This a r r a n g e m e n t of the e l e c t r o d e s p e r m i t s b e t t e r
utilization of the bath. Also, these baths are e a s i e r to manufacture and r e p a i r , and r e p l a c e m e n t of e l e c -
t r o d e s is s i m p l e r . The salt baths shown in Fig. la, b, have electrodes in the f o r m of plates o r a stack of
square b a r s with only one side touching the bath. Enclosing the b a r s i n c r e a s e s the working life of the e l e c -
t r o d e s but c o m p l i c a t e s r e p a i r s , a n d t h e r e f o r e baths used individually frequently employ flat (Fig. lc) or
round (Fig. ld, e) e l e c t r o d e s lowered into the bath. In some baths the e l e c t r o d e s are i n s e r t e d through the
side wall below the s u r f a c e of, the salts, which p r o t e c t s them against the effects of the atmosphere. A c c o r d -
ing to [12], the working life of these s u b m e r g e d e l e c t r o d e s at 1200~ is around one y e a r . However, it is

973
TABLE 1
Country where Temperaturel ~
Salt mixture trademark Composition,% Use
used melting operating
i

USSR 100 BaC1z 960 1050-1300 Final quenching, high-speed

USSR BM5 95 BaClz+5 MgF2 940 1200-1300 and high-alloy steels
USSR BM3 97 BaClz+ 3 MgF2 950 1050-1300
Czechoslovakia GS960 98 BaClz* 950 1050-1300
West GermanY,
Italy Cassel HS 970 94 BaCI2+ 5 Na2B407+ 1SiOz 950 1050-1300
USA, Italy Holden-hardening
17- 24AA10 95 BaCI2~ 1050-1300
East Germany E 97.3 BaClz+0.65 NaB407 1050-1300

USA - 9'0 BaClz+10 NaC1 850 950-1050 Quenching of high-chromium

steels

USSR BNM2 68 BaC12+30 NaCI+2 MgF2 780-950 Final quenching of low-alloy

USSR 78 BAC12+22NaC1 700-950 and carbon steels
USSR 44 NaC1+ 56 KC1 720-900
Czechoslovakia GS670 50 BaC12+50 NaC1 700-1000
Czechoslovakia GS540 50 BaC12+ 20 NaC1+ 30 KC1 600-900
East Germany 630 61.7 BaC1z+ 36.5 NaC1* 730- 930
East Germany 550 46.4 BaC12+26.5 NaC1+ 26.5 KC1 600-900
West Germany,
Italy Cassel NC-660 48 BaC12+30 NaCl+22 KC1 720-960

* Other components not specified.

I" The rest consists of calcium, magnesium, and sodium compounds.

d i f f i c u l t to s e a l the o p e n i n g s i n w h i c h the e l e c t r o d e s a r e i n s e r t e d , and this p l a c e m e n t of the e l e c t r o d e s is

not w i d e l y u s e d f o r t h a t r e a s o n .

The s a l t b a t h s u s e d in h e a t t r e a t m e n t l i n e s a r e of v a r i o u s d e s i g n s with the b a t h e l o n g a t e d in the d i r e c -

t i o n of m o v e m e n t of the p a r t s . F o r e x a m p l e , r e c t a n g u l a r b a t h s a r e u s e d with t h r e e o r f o u r p a i r s of e l e c -
t r o d e s on one s i d e (Fig. If) c o n n e c t e d to t h r e e d i f f e r e n t p h a s e s , and a l s o s i x - s i d e d b a t h s (Fig. lg).
To i m p r o v e t h e i r d u r a b i l i t y the e l e c t r o d e s a r e m a n u f a c t u r e d f r o m h e a t - r e s i s t a n t s t e e l s Kh25, K h l S ,
e t c . , i n s t e a d of the p r e v i o u s l y u s e d l o w - c a r b o n s t e e l s 1 0 , 1 5 , and 20 [15]. Nickel e l e c t r o d e s a r e s o m e t i m e s
u s e d , which a c c o r d i n g to [16] h a v e a s e r v i c e life t h r e e to f o u r t i m e s that of s t e e l e l e c t r o d e s .

To p r e v e n t an a b r u p t drop in t e m p e r a t u r e when the p a r t s a r e i m m e r s e d the s i z e of the b a t h is s u c h

that the weight of the f u s e d s a l t s is 10 t i m e s that of the m e t a l l o a d e d in the bath at one t i m e .

The s e l e c t i o n of t r a n s f o r m e r s f o r s a l t b a t h s d e p e n d s on the v o l u m e of the b a t h and the m a x i m u m t e m -

p e r a t u r e . Soviet i n d u s t r y e m p l o y s t r a n s f o r m e r s T P T - 3 5 0 , T P T - 6 0 0 , T P T - 1 0 0 0 , and T P T - 1 6 0 0 with s e v e r a l
s e t t i n g s to m a i n t a i n v a r i o u s t e m p e r a t u r e s . The t h e r m a l and e l e c t r i c a l c a l c u l a t i o n s f o r s a l t b a t h s a r e g i v e n
in [4, 17] and will not be c o n s i d e r e d h e r e .
F o r e l e c t r o d e s a l t b a t h s the r e f r a c t o r y m a t e r i a l is u s u a l l y c l a s s A e h a m o t t e c o n t a i n i n g at l e a s t 30?0
A120 3 that h a s b e e n w e l l r o a s t e d and h a s a s o f t e n i n g p o i n t of at l e a s t 1730~ and c o m p r e s s i v e s t r e n g t h of
100 k g / m m 2 [3]. Rough e s t i m a t e s of the q u a l i t y of c h a m o t t e b r i c k s c a n be o b t a i n e d by a s i m p l e t e s t : p i e c e s
of b r i c k a r e p l a c e d i n the b a t h , w h e r e they float on the s u r f a c e due to t h e i r low d e n s i t y . If no t r a c e s of
d a m a g e a r e v i s i b l e a f t e r 3 h at 1300~ t h e n the b r i c k s a r e s u i t a b l e f o r l i n i n g the bath. We have found that
the d u r a b i l i t y of s a l t bath l i n i n g s c a n be i n c r e a s e d s u b s t a n t i a l l y if h i g h - a l u m i n a b r i c k s m a d e f r o m v a r i o u s
h i g h - q u a l i t y n a t u r a l h i g h - a l u m i n a m a t e r i a l s a r e u s e d i n p l a c e of s i m p l e c h a m o t t e b r i c k s . A c c o r d i n g to [4],
s u c h b r i c k c o n t a i n s o v e r 45% A120 3. A b r o a d , l i n i n g s of p r e s s e d m a r b l e dust a r e s o m e t i m e s u s e d .

Crucible Salt Baths

C r u c i b l e s f o r b a t h s with e x t e r n a l h e a t e r s c a n be c a s t with a wall t h i c k n e s s of 12-30 m m (cast i r o n ,
c a r b o n s t e e l s , o r a l l o y s of the Kh18N9T, Kh25N20S2, o r K h l 5 N 6 0 type), o r p r e s s e d o r w e l d e d ( l o w - c a r b o n

974
TABLE 2 steels with 0.08-0.05% C). Sometimes a single salt bath has
Temperature, ~ s e v e r a l crucibles for p r e l i m i n a r y and final heating as well as
Composition of salt mix- cooling.
tures, wt,% melting Operating
In electric crucible baths the salts are heated by coils
100 KNQ 335 380--600 and bands in rows around the side walls. Usually these baths
50 KNOa+50 NaNO~" 137 160--400
85 KNOa+15 NaOt-I 380--600 are 200-400 m m in d i a m e t e r and of low power (10-30 kV). C r u -
50 KCI+50 Na.~CO3 577 600--700 cible baths with gas h e a t e r s are r a r e l y used f o r heat t r e a t m e n t
50 BaCI~-t-25NaCI+25KCI 590 620--700
and crucible baths are almost n e v e r heated with liquid fuels due
Note; These salt mixtures are used for tem-
to the difficulty of regulating the t e m p e r a t u r e p r e c i s e l y .
pering,
All crucible baths with external h e a t e r s have a low p r o -
ductivity and the s e r v i c e life of the crucibles and h e a t e r s is corn-
paratively short. Baths with internal h e a t e r s have recently been used. They are heated by alternating c u r -
rent at a potential of 220 and 380 V by means of tubular elements (TI~N), consisting of s e a m l e s s tubing 15-
40 m m in d i a m e t e r with an internal Nichrome element insulated f r o m the tubing by s o m e substance such as
powdered m a g n e s i u m oxide [12]. Tubular e l e c t r i c a l h e a t e r s are most suitable for use in U-shaped salt
baths.
Extensive tests of salt baths with internal heating elements in the tool industry have shown their ef-
fectiveness in t e m p e r i n g and cooling in stepped quenching of tool steels, where p r e c i s e t e m p e r a t u r e s are
of p a r t i c u l a r importance.

Salt Baths in Production Lines

Heat t r e a t m e n t of m a s s - p r o d u c e d p a r t s has proved to be effective with automated lines consisting of
mechanized equipment - s a l t b a t h s placed in sequence. The use of salt baths in the tool industry began in
the e a r l y 50s and at the p r e s e n t time hundreds of automated and mechanized salt baths are in use.
Abroad, salt baths were f i r s t used in production lines considerably e a r l i e r and for s m a l l e r n u m b e r s
of p a r t s [5, 6]. The v e r y l a r g e size of the baths, the mechanized t r a n s f e r of p a r t s f r o m bath to bath in a
specifiecl time interval controlled by an o p e r a t o r , and automatic control of the t e m p e r a t u r e e n s u r e a l a r g e
throughput with high and consistent quality of the heat t r e a t m e n t .
The r a c k s with p a r t s can be t r a n s f e r r e d f r o m one bath to another by means of l e v e r s o r chains or
special devices and moved along the length of the bath by c o n v e y e r chains. The most widely used s e m i -
automatic quenching apparatus are the AAZ-1 and AAZ-2 at the S e s t r o r e t s k and L ' v o v Tool Plants, the
s e m i a u t o m a t i c quenching apparatus VZS-3 and the t e m p e r i n g apparatus VZS-O at the Vil'nyus Drill Plant,
and the s e m i a u t o m a t i c t e m p e r i n g apparatus M F - O at the F r e z e r Plant. Mechanized lines are widely used
for heat t r e a t i n g tools in salt baths and cleaning them - t h e A L Z P line, for example, used in heat treating
spherical c u t t e r s of steel 9KhS at the K h a r ' k o v Tool Plant, the OIZ-K1 line f o r h i g h - s p e e d steel drills at
the Orenburg Tool Plant, the MF-518 line for drills at the F r e z e r Plant, etc. Data on this equipment and
these lines can be found in [11, 12].

Measuring, Checking, and Regulating Salt Bath Temperatures

It is r e c o m m e n d e d that the t e m p e r a t u r e of salt baths operating at 1000-1300~ be checked during
operation by means of a T e r a 50 telescope p y r o m e t e r and electronic potentiometer with an RK-15 s c a l e
(700-1400~ P o t e n t i o m e t e r s of the t~PP-16AM2 or ]~PD-107 types are r e c o m m e n d e d as s e c o n d a r y i n s t r u -
ments.

Graduation of the p o t e n t i o m e t e r makes it possible to obtain the m a x i m u m emf (19.75 mV at 1300~

for example) and p e r m i t s a c c u r a t e control of the t e m p e r a t u r e by means of d e c r e a s i n g the amplitude and in-
c r e a s i n g the period of oscillation of the t e m p e r a t u r e .

It was found in [18] that the bath t e m p e r a t u r e can be m e a s u r e d by means of radiation p y r o m e t e r s with
an a c c u r a c y of ~10~ However, it should be kept in mind that domestic p y r o m e t e r s p r e s e n t l y used ensure
an a c c u r a c y of only =~20~ with c o r r e c t installation of the telescope, and this a c c u r a c y is inadequate f o r high-
t e m p e r a t u r e baths. These baths are used for heating p a r t s of high-alloy steels that must be held within v e r y
n a r r o w limits. Before operation is begun the t e m p e r a t u r e of h i g h - t e m p e r a t u r e baths is carefully checked
with an a c c u r a c y of -1~ by means of a thermocouple; the bath is brought to the p r o p e r operating t e m p e r a -
ture by calibration of the s e c o n d a r y i n s t r u m e n t s . In this case the a c c u r a c y of the t e m p e r a t u r e m e a s u r e -
ments made with the radiation p y r o m e t e r i n c r e a s e s greatly, usually reaching ~5~ Smoke above the bath

975
 TABLE 3
Country where Rectifier
used trademark Composition of rectifier, wt. '70 Use

USSR - Borax (Na2B4OT) For all high- and medium-tem-

perature baths

USSR - 75% ferrosilicon

For high-temperature baths
USSR - KrO crystalline silicon

East Germany BT 19.6 BaC1+12.7 NaC1+10.6 For mixtures 580 and 630
KC1+43 Si+9 Fe

West Germany, Cassel A 98.46 Si+0.27Ca For mixture NC 660

Italy 0.47 Fe + 0.39 A1

Czechoslovakia Carboneutral 92 BaC1z + 6 Na2B407 For mixture GS 960

r e s u l t i n g f r o m d i s s o c i a t i o n and e v a p o r a t i o n of s a l t s is r e m o v e d b y m e a n s of a v e n t i l a t i o n h o o d o r c o m -
p r e s s e d a i r t h r o u g h a t u b e b e n e a t h the t e l e s c o p i c s i g h t .

A c c o r d i n g to d a t a f r o m t h e f i r m of H a r t m a n and B r a u n , t h e t e m p e r a t u r e of b a t h s o p e r a t i n g at 1200-
1300~ c a n b e m e a s u r e d m o r e a c c u r a t e l y b y u s i n g c e r a m i c t e l e s c o p i c s i g h t s t h a t a r e s e a l e d and with the
end i m m e r s e d in the m o l t e n s a l t . A r a d i a t i o n p y r o m e t e r m e a s u r e s t h e t e m p e r a t u r e in a g i v e n s e c t i o n of
t h e t u b e , w h i c h is h e a t e d to the t e m p e r a t u r e of the m o l t e n s a l t . T h i s c o m p l e t e l y e l i m i n a t e s e r r o r s in m e a -
s u r e m e n t due to s m o k e , s c a t t e r i n g of l i g h t , and f i l m s on the s u r f a c e of the b a t h , a l l of w h i c h r a i s e s t h e a c -
c u r a c y of the m e a s u r e m e n t s to ~3~
At t h e p r e s e n t t i m e s a l t b a t h t e m p e r a t u r e s a r e u s u a l l y c o n t r o l l e d a u t o m a t i c a l l y . The Soviet tool i n -
d u s t r y m a k e s w i d e u s e of a u t o m a t i c c o n t r o l s w i t h an a c c u r a c y of ~10~ The t e m p e r a t u r e is c o n t r o l l e d by
m e a n s of an e l e c t r o n i c p o t e n t i o m e t e r , i n t e r m e d i a t e r e l a y , and e l e c t r i c a l c o n t a c t s . The s a l t b a t h is o p e r a t e d
on t h e o n - o f f p r i n c i p l e .
M o r e a c c u r a t e c o n t r o l (:~5~ i s p o s s i b l e w i t h t h e A l I - U n i o n S c i e n t i f i c - R e s e a r c h I n s t i t u t e ' s P T R T
( h i g h - p r e c i s i o n t e m p e r a t u r e c o n t r o l ) , w h i c h d o e s not cut off t h e b a t h but a u t o m a t i c a l l y s h i f t s t h e s t a g e of
the t r a n s f o r m e r [11].

W i t h m o r e f r e q u e n t s h i f t s of t h e t r a n s f o r m e r the t h e r m a l i n e r t i a of the f u s e d s a l t and c h a n g e s in t h e

t r u e t e m p e r a t u r e of t h e b a t h d e c r e a s e , w h i c h p e r m i t s m o r e p r e c i s e c o n t r o l of the t e m p e r a t u r e r a n g e .
A p l a t i n u m - p l a t i n u m r h o d i u m t h e r m o c o u p l e a n d the p o r t a b l e P P - 6 3 o r K P - 5 9 p o t e n t i o m e t e r a r e u s e d
to c h e c k the r e a d i n g s of t h e s t a t i o n a r y i n s t r u m e n t s d a i l y b e f o r e o p e r a t i o n is b e g u n and, when n e c e s s a r y ,
d u r i n g o p e r a t i o n . S o m e t i m e s s p o t c h e c k s a r e m a d e w i t h an i n e r t i a l e s s a n g l e C h r o m e l - A l n m e l t h e r m o c o u p l e
w i t h a h i g h e m f a s c o m p a r e d w i t h p l a t i n u m , and c o n s e q u e n t l y g r e a t e r s e n s i t i v i t y . H o w e v e r , C h r o m e l - A l u m e l
t h e r m o c o u p l e s c a n b e u s e d to c h e c k t h e t e m p e r a t u r e o f h i g h - t e m p e r a t u r e s a l t b a t h s o n l y b y q u a l i f i e d m a i n -
t e n a n c e p e r s o n n e l , s i n c e t h e s e t h e r m o c o u p l e s w i t h s t a n d only 100-200 i m m e r s i o n s in a few t e n s of m i n u t e s
[19].
The t e m p e r a t u r e of m e d i u m - t e m p e r a t u r e s a l t b a t h s is m e a s u r e d and c o n t r o l l e d b y m e a n s of e l e c t r o n i c
p o t e n t i o m e t e r s of the I~PD-120 o r ]~PD-107 t y p e s of g r o u p KhA with s c a l e r e a d i n g s of 600-1100~ in c o m -
b i n a t i o n w i t h a C h r o m e l - A l u m e l t h e r m o c o u p l e . When t h e e f f e c t of e l e c t r o m a g n e t i c v i b r a t i o n s on t h e t h e r m o -
c o u p l e is e l i m i n a t e d t h e t e m p e r a t u r e of t h e b a t h c a n u s u a l l y be c o n t r o l l e d w i t h i n l i m i t s of ~10~ and w i t h i n
~-5~ w h e n t h e P T R T i s u s e d .
T h e t e m p e r a t u r e of s a l t b a t h s o p e r a t i n g at 400-700~ is m e a s u r e d a n d c o n t r o l l e d with C h r o m e l - A l u m e l
t h e r m o c o u p l e s and a l s o e l e c t r o n i c i n s t r u m e n t s , a s in t h e c a s e of m e d i u m - t e m p e r a t u r e b a t h s , but with s c a l e
r e a d i n g s of 0-800~
T h e t e m p e r a t u r e o f s a l t b a t h s o p e r a t i n g a t 150-400~ is m e a s u r e d a n d c o n t r o l l e d with an e l e c t r o n i c
p o t e n t i o m e t e r of t h e ] ~ P P - 0 9 o r ]~PD-107 t y p e of g r o u p KhK with a s c a l e of 0-400~ in c o m b i n a t i o n w i t h a

976
C h r o m e l - Copel thermocouple. The r e s i s t a n c e of thermocouple jackets in f~sed salts d e c r e a s e s with in-
c r e a s i n g t e m p e r a t u r e and i n c r e a s e s with d e c r e a s i n g concentrati~ns of carbon in the steel used for the
jacket, and t h e r e f o r e t h e r m o c o u p l e jackets a r e usually made of l o w - c a r b o n steels 10 o r 20. To i n c r e a s e
the r e s i s t a n c e of t h e r m o c o u p l e jackets in high- and m e d i u m - t e m p e r a t u r e salt baths the jackets are made
of steel of the Kh25 type, and steel of the Khl8 type for l o w - t e m p e r a t u r e baths. The use of these steels also
makes it possible to reduce the d i a m e t e r of the jacket, reduce the t h e r m a l inertia, and i n c r e a s e the a c -
c u r a c y of the m e a s u r e m e n t s .

Requirements for the Salts Used in Salt Baths

The composition of salt baths for heating metals should be selected in relation to the purpose, p a r -
t i c u l a r l y the t e m p e r a t u r e of the p r o c e s s , although o t h e r f a c t o r s a r e also important.
It has been found in p r a c t i c e that the following are the most important r e q u i r e m e n t s for the salts
used in heating steel p a r t s .
In the solid state the salts and salt mixtures must be capable of prolonged s t o r a g e in air, have a low
h y g r o s c o p i c i t y , and not pass into the liquid o r semiliquid state at 30-40~ after absorption of moisture.
Salts for m e d i u m - and h i g h - t e m p e r a t u r e baths must not dissociate during drying at 200-400~ which is
c a r r i e d out to prevent spattering f r o m the bath when salts a r e added. The salts should be easily soluble in
water, which is n e c e s s a r y in o r d e r that the film of salt clinging t o h e a t - t r e a t e d p a r t s be r e m o v e d by washing
o r pickling in weak acid solutions with subsequent passivation in aqueous solutions of n i t r i t e - s o d a . The
salts must not induce c o r r o s i o n , d e c a r b u r i z i n g , or strong oxidation of the t r e a t e d p a r t s .
The molten salts o r salt mixtures must have a low volatility but high fluidity f o r good wetting of the
p a r t s . The fluidity of the fused salts is d e t e r m i n e d with instruments [20] o r e s t i m a t e d f r o m the amount of
salt c a r r i e d out on fiat s a m p l e s . In addition to these p r o p e r t i e s , salts for electrode salt baths must have
a f a i r l y high e l e c t r i c a l conductivity, must not dissociate under the influence of electric c u r r e n t passing
through them, and must not have a s t r o n g effect on the chamotte lining of the bath. To avoid substantial
evaporation and dissociation of salts or salt mixtures, each should be used in a n a r r o w t e m p e r a t u r e range
(not exceeding 200-300~ A m a j o r f a c t o r in selecting salts is the melting point. The operating t e m p e r a -
ture of the bath should be at least 40-70~ above the melting point of the salt o r salt mixture to attain the
p r o p e r fluidity and reduce c a r r y o u t .

The n u m b e r of salts in the bath should be kept to the minimum. To simplify the composition, only
one salt is used o r a b i n a r y o r m o r e r a r e l y t e r n a r y euteetic mixture with a lower melting point.
When mixtures of salLs a r e used that f o r m continuous solid solutions (NaC1 and KC1, for example)
the mixture usually selected is that c o r r e s p o n d i n g to the minimum point onthe liquidus curve.

Decarburizing of Metal during Heating in Salt Baths and

Methods of Checking It
In high-temperature and medium-temperature salt baths the basic components are high-melting
chlorides, while in low-temperature baths they are mixtures of sodium and calcium nitrates and nitrites.
In electrode salt baths operating at 750-1300~ the molten chlorides react chemically with the oxygen
from the air, and with the metal of the treated parts and the furnace, and therefore the composition of the
salt bath changes continuously during operation.
The interaction with oxygen f r o m the air and iron in the salt bath results in the format'ion of BaO,
Na20 , K20 , and Fe203 [14], which a r e e i t h e r dissolved in the bath, suspended in it, or precipitated as sludge.
Aluminum and silicon oxides a r e washed out of the furnace lining and also enter into the bath. At the
beginning of operation of a bath with a new lining w a t e r v a p o r f r o m the lining also e n t e r s into the reaction,
and t h e r e f o r e in the f i r s t days of operation the d e c a r b u r i z i n g activity of the bath is high; it d e c r e a s e s after
elimination of the m o i s t u r e and then gradually i n c r e a s e s again with accumulation of metal oxides in the bath
(Fig. 2a).

During operation of the bath the salts a r e s a t u r a t e d with oxygen f r o m the air and g a s e s f o r m e d in
chemical reactions [21]. Thus, with time the salt bath b e c o m e s m o r e and m o r e contaminated with oxides
and s a t u r a t e d with g a s e s , resulting in intense d e c a r b u r i z i n g and c o r r o s i o n of the t r e a t e d p a r t s .

977
 It was found in [15] that f e r r i c oxide has a p a r t i c u l a r l y strong d e c a r b u r i z i n g effect.
It should be kept in mind that the intensity of d e c a r b u r i z i n g is affected, a p a r t f r o m the composition
of the fused s a l t s , by the c h e m i c a l composition of the t r e a t e d m e t a l and the t e m p e r a t u r e and heating t i m e .
The concept of the " d e c a r b u r i z i n g activity of fused s a l t s " [22] and c r i t e r i a for d e t e r m i n i n g it have been
f o r m u l a t e d to d e t e r m i n e the condition of the bath. The d e c a r b u r i z i n g activity of h i g h - t e m p e r a t u r e baths at
a given t e m p e r a t u r e is evaluated by two methods.
1. F r o m the change in the c a r b o n content of thin (0.1-0.2 mm) bands of steel 13Kh or U13 a f t e r heating
of the s a m p l e f o r 1 min at the s t a n d a r d quenching t e m p e r a t u r e for h i g h - s p e e d steel (foil method). An a c -
c e l e r a t e d t e s t consisting of d e t e r m i n i n g the c a r b o n content of quenched bands by m e a s u r i n g the t h e r m o - e m f
that has been developed r e c e n t l y [23] p e r m i t s r a p i d and a c c u r a t e analysis of all s a l t baths 9
2. F r o m the depth of d e c a r b u r i z i n g on a c u t e - a n g l e d s a m p l e s (angle 55~ of high-alloy steel (high-
s p e e d steel, for example) heated 15 rain at s t a n d a r d quenching t e m p e r a t u r e 9 D e c a r b u r i z i n g can be detected
by Sadovskii's method [24] o r i s o t h e r m a l heating in the p e a r l i t i c range [25].
The d e c a r b u r i z i n g activity of m e d i u m - t e m p e r a t u r e s a l t baths is d e t e r m i n e d by e i t h e r of the two m e t h -
ods on s a m p l e s of s t e e l U13 o r 13Kh. Samples of low-alloy s t e e l s a r e t e s t e d for 10 min at quenching t e m -
p e r a t u r e , since d e c a r b u r i z i n g is c o n s i d e r a b l y s l o w e r than in h i g h - t e m p e r a t u r e baths. Acute-angled s a m -
ples a r e usually made of s t e e l 9KhS and heated at 870~ f o r 1 h. D e c a r b u r i z i n g is r e v e a l e d by cooling to
the bainitic r a n g e with holding at 380~ for 1 h e i t h e r d i r e c t l y a f t e r the t e s t o r a f t e r r e p e a t e d heating to
900~

Rectification of Salt Baths

It has been found [14, 15] that the decarburizing activity of high- and medium-temperature salt baths
depends on several factors -the initial composition, temperature, operating time, amount of metal heated
per unit time, its composition, the amount and frequency of rectifier added to reduce or completely neu-
tralize metal oxides, dissolved oxygen, and other gases on the surface of the treated parts. Three groups
of rectifiers are used. The first group consists of strong reducing agents that decompose metal oxides in
high-temperature baths (crystalline silicon, 85-75% ferrosilicon),which are finely ground. Usually 400-
600 g of these rectifiers are added every four hours of operation, the decarburizing activity of the bath
dropping immediately and then rising until more rectifier is added (Fig. 2b). Charcoal and graphite are
sometimes used for medium-temperature baths.
The second group of rectifiers includes various salts (borax, magnesium fluoride, etc. ), which com-
bine oxides into complex insoluble compounds that precipitate as sludge.
The additionof rectifiers results in the formation of complex compounds - BaO 9 B203; 2FeO. 2F203
9 3BzO3; MgO 9 FeO. 2AI203Fe203; and MgO 9 Fe203 [14] - which are then precipitated. The elimination of
ferric oxide sharply reduces the decarburizing activity.
Rectifiers of the second group (magnesium fluoride and borax) can be added to the bath separately or
mixed with chlorides. In high-temperature baths they are added with barium chloride and in medium-tem-
perature baths with barium and sodium chlorides.
The third means of rectification involves a pipe carrying methyl chloride, methane, and other gases,
which reduce the metal oxides. This method is effective at temperatures up to 1000~ [i].
In using the foil method the decarburizing activity of the bath O a can be determined from the absolute
reduction of the carbon content of the sample after heating in the bath:
Oa=C,,--Ck, (I)
where C u is the initial carbon content, %; C k is the final carbon content, %.
However, the eondition of the bath can be determined m o r e accurately from the relative reduction of
the carbon content by the formula proposed in [22]:

c~-ck (2)
Ka- C~ '
w h e r e K a is the coefficient of the d e c a r b u r i z i n g activity of the bath.

978
Composition of Salts for Baths
The most commonly used eompositions for high- and medium-temperature salt baths are given in
Table I, and for low-temperature baths in Table 2.
Barium chloride baths (90-100% BaCl2) are also used for heating parts in automated produetion lines.
Of the mixtures listed in Table I, the best is BM5 [15], which has the lowest decarburizing activity
(Fig. 2e). In baths of this mixture there is no deearburizing of any high-speed steel, including those most
susceptible to deearburizing - molybdenum and cobalt steels.
In this bath (BM5 mixture) the electrodes last two to three times longer than in high-temperature
borax baths with rectification.
However, in the initial period of operation a film is formed on the surface of the BM5 bath. To avoid
this it is recommended that the bath be started with only one-quarter to one-half the amount of the BM5
mixture, and the remainder barium chloride, leaving the initial concentration of MgF 2 at 1.25 or 2.5%. In
the course of operation only the BM5 mixture is added.
For quenching tools of steels less susceptible to decarburizing or held for shorter times in high-
temperature baths the BM3 mixture can be used, which contains 3% MgF 2 (Table i). To lower the operating
temperature of this bath from 1050 to 950~ it is reeommended that up to 10% NaCI be added to the barium
chloride [I].
Baths for heating parts subjected to stepped quenching should not contain salts that interaet chemically
with the quenching medium. Thus, for bright stepped quenching of parts in fused alkali the heating bath
should not contain barium chloride, which forms insoluble residues with alkali. In this case the heating
bath should consist of sodium and calcium chlorides, which do not react with alkali. Highly toxic salts
should not be used in any of the baths.
The rectifiers used periodically to prevent decarburizing of parts are listed in Table 3. Borax is
commonly added every 4 h to high-temperature baths in amounts of 1% of the salt by weight, and to medium-
temperature baths in amounts of 0.8%.
Ferrosilicon and crystalline silicon in fine powders are added to high-temperature baths in amounts
of 0.5% by weight every 4 h. Table 3 also lists the recommendations of foreign firms for the addition of
these rectifiers separately or in the BT mixture for medium-temperature baths. The BT mixture is added
to medium-temperature baths every 8 h in amounts of 4-20%. Additions of Carboneutral are made to baths
containing mixture GS 960 (Table i). The bath is first filled with one-third of the salt mixture and two-
thirds Carboneutral. In the course of operation only Carboneutral is added.

LITERATURE CITED
I. William A. Curtis, Metal Progress, 90, No. 6 (1966).
2. Q. Merkam, Tooling and Product, 33, Nos. 3 and 4 (1967).
3. P.A. Krylov, Electric Salt Furnaces and Baths [in Russian], Gos6nergoizdat (1962).
4. S.L. Rustem, Equipment and Layout of Heat Treatment Shops [in Russian], Mashgiz, Moscow (1962).
5. J. Iron Steel. Inst., 42, No.2, 101-103 (1969).
6. Iron Age, 203, No. 7, 107 (1969).
7. E.A. Smol'nikov and F. I. Zhdanova, Salt Baths for Heat Treatment of Parts [in Russian], Mashgiz,
Moscow (1963).
8. E.A. Smol'nikov, Zavod. Lab., No. 5 (1967).
9. H. Brandis et al., H~rteritechische Miteilungen, 22, No. 3 (1967).
I0. E.A. Smol'nikov, Metal. i Term. Obrabotka Metal., No. 6 (1961).
II. In: Standard Technology of Heat Treating Metalworking Tools [in Russian], Parts 1 and 2, NIIMASh,
Moscow (1967).
12. D. Ya. Vishnyakov, G. N. Rostovtsev, and A. A. Neustruev, Equipment, Mechanization, and Automation
of Heat Treatment Shops [in Russian], Metallurgiya, Moscow (1964).
13. A.A. Shmykov, Heat Treatment Handbook [in Russian], Mashgiz (1961).
14. I.F. Afonskii and A. A. Kroshkin, Salt Baths for Heat Treatment [in Russian], ONTI (1934).
15. E.A. Smol'nikov, Metal. i Term. Obrabotka Metal., No. 3 (1962).
16. W. Barcroft, Metal Progress, I0, No. i0 (1946).

979
 17. L. A. Mikhailov, V. G. Kaufman, and V. M. Pulaev, Method of Calculating the Electrical P a r a m e t e r s of
Salt Baths [in Russian].
18. T r a i t e m - T h e r m . , No. 22 (1966).
19. K. A. Mironov and L.I. Shipetin, Thermotechn[cal Measuring Instruments, Handbook Data [in Russian],
Mashgiz, Moscow {1958).
20. A.I. Zot'ev, in: New Methods of Heat Treatment in Fused Salts and Alkalis [in Russian], VNIITOMASh,
Gor'kovskoe Kn. Izd. (1955).
21. S.Wilmes et al., Arch. Eisenhiittenw., 32, No. 9 (196t).
9 22. E. A. Smol'nikov, Tekhnologiya Mashinostroeniya, No. 5 (1966).
23. E. A. Smol'nikov, Zavod. Lab., No. 5 (1967).
24. V. D. Sadovskii, Zavod. Lab., No. 6 (1934).
25. E. A. Smol'nikov, in: Methods and Practices in Metallographic Studies of Tool Steels [in Russian],
Mashgiz, Moscow (1961).

980