A Foaming Bath Method For Direct Heat Treatment Systems

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A Foaming Bath Method for Direct Heat Treatment System for

Wire Rod Manufacture*

By Katsuhiko YAMADA,** Yoshihiro HASHIMOTO,*** Kunio OJIMA* *


and Takashi ASAKURA**

Synopsis process covers all kinds of heat treatments from


Thebehavior of thehotrolledwirerodsduringcoolingin waterwas annealing to quenching.
preciselyinvestigated
bya laboratory
testandit has beenmadeclearthat (2) The mechanical properties of the treated coil
coolingbysubcool-boilingina gaswatermixedfluidcanbea newcooling must have the uniformity which is equivalent to that
methodand thisfluidcanbe takenas a newcoolantwhichhasexcellent of off-line treated one.
characteristics
for patenting. As the concrete means, the air cooling conveyor
The newdirectheattreatmentsystemhavingtheverywiderangeof
cooling
speeds, in whichthisnewcoolingmethodandnewcoolant wasap- having the heat isolation tunnel was adopted for the
cooling speed below 10°C/s, and the process of
pliedas theprincipaltechnology,
wasdeveloped.
Thetreatedwirerodshavenotonlythegoodmechanical properties
but continuously dipping into cold or warm water was
alsothehighuniformity withina coil. adopted for above 50°C/s. One of the most difficult
heat treatments is patenting whose cooling speed is
Key words: heat treatment;wire rod; coolingmethod;patenting; 10' 30°C/s and the subcool-boiling method has not
mechanical
property. been applied for this purpose in spite of its possibility.
The reason is that the film boiling transits to nucleate
I.Introduction boiling at the early stage of cooling and then cooling
The advantages of controlled cooling for hot rolled speed is extremely accelerated and finally the trans-
wire rods are widely known as follows : formation finishes not through the formation of pear-
(1) It eliminates the heat treatment before cold lite but through martensite. Few technical reports
drawing. have been found which refer what metallurgical fac-
(2) In some cases it provides the better quality tors affect this transition from film boiling to nucleate
than that given by off-line heat treatment. boiling.7)
(3) It reduces the indirect manufacturing costs Therefore, the boiling phenomenon was carefully
by preventing the defects caused by coil handling and investigated and the cooling behavior was analyzed.
rust, shortening the leading time from rod to final It was made clear that the growth of FeO whisker on
wire products, and reducing the amount of wire rod the surface greatly affected the transition from film
stock. boiling to nucleate boiling. Finally, the new coolant
(4) It improves pollution problems caused by of gas-water mixed fluid by which the growth of FeO
heat and surface treatment. whisker can be suppressed and the cooling speeds can
Stelmor process (the forced air cooling), and ED easily be controlled was found out and the new cooling
(Easily Drawable)1~ process (the cooling by boiling system based on this new coolant was developed.
water) are both quite popular as the partial substitute On the other hand, wire rod is generally heat
of lead patenting for the past more than 10 years. treated in the form of overlapping nonconcentric
Recently, the new processes such as EDC (Easily spirals. Therefore, it is difficult to avoid the lack of
Drawable Conveyor),2'3> D0,4) DLP5~ and other new uniformity of cooling within a coil. As the counter-
controlled cooling processess~ have been developed measure for this problem, a few analyses were carried
and commercialized and they have extended the varia- out and the results were reflected to the design of the
tion of cooling and improved the quality of treated equipment.
products. Though each of them has superior charac-
teristics, the cooling function is not multiple but single. II. Cooling Behavior of Wire Rod in the Gas-
It means that they are not always advantageous as Water Mixed Fluid
the controlled cooling system which must accept the The trial to utilize the subcool-boiling phenomenon
production of small lots with many grades and the was carried out to get high tensile strength (TS)
reduction of investment cost as one of the trend of and good drawability which were equivalent to those
steel manufacturing technology from now on. by lead patenting. It has already been made clear
The following two targets were aimed by Sumitomo through the preliminary investigation that the coolant
Electric Industries, Ltd. at the planning stage of new temperature, the flow rate of coolant and the surface
controlled cooling process. condition of wire rod greatly influence the cooling
(1) Any cooling speed in the range of 2 N speed and also that the characteristics of the coolant
100°C/s must be able to be chosen so that the extremely depend on the gas bubbles injected in warm
* Based on the papers presented to the 110th ISIJ Meeting, October 1985, S1135 to S 1137, at Nii Bata University in N iigata. Manu-
script received on April 28, 1986; accepted in the final form on September 12, 1986. © ISIJ 1987
** Special Steel Wire Division, Sumitomo Electric Industries, Ltd., Koya Kita, Itami 664.
*** Itami Research Laboratories, Sumitomo Electric Industries, Ltd., Koya Kita, Itami 664.

(42) Technical Report


Transactinos Is", Vol. 27, 1987 (43)

water.

1. Specimensand Experimental Method


The material used was JIS SWRH 82B whose
chemical compositions were 0.80 % C, 0.25 % Si,
0.68 % Mn, 0.015 % P, 0.011 % S and 0.017 % Al
(wt%). As the specimen, wire of 11.0 mm in diam-
eter whose surface was mechanically shaved from
the wire of 11.3 mm in diameter after cold drawing
from 12.3 mm dia. wire rod was prepared in order to
avoid the influence of surface conditions.
UµJ 11V YY 1µ1,l,. V'~L..! 111111111 •111

Figure 1 shows the equipment used in this experi-


Fig, 1. Schematic drawing of quenching unit.
ment. The bubbles were uniformly provided by
injecting certain volume of air from the bottom of
the tank and the temperature of the coolant was
controlled by electric heater and the specimen stage
was repeatedly movable in the horizontal and the
vertical directions. The specimen was heated up to
950 °C in the furnace followed by keeping for 15 min
in N2 gas atmosphere, and then dipped into the
cooling tank after keeping it for a predetermined
period of time in air.
The temperature of specimen was measured by Fig. 2. Cooling curves at the center of wire rod in warm

CA thermocouple inserted into the axial center of it. water.

The experiment factors that influence the cooling


were selected as follows:
1) time of preoxidation by air before immersion in
coolant
2) temperature of coolant
3) kinds of injection gas
4) volume of injection gas
5) relative flow velocity between specimen and
coolant
6) overlapping conditions of specimens.

2. CoolingCurve of the Specimen


Figure 2 shows one of the examples of cooling
curve measured at the axial center of the specimen
cooled in warm water. In this figure, the variables
are time of preoxidation by air to and temperature of
coolant T. The to corresponds to the time spent
till dipping after rolling in actual operation. As to
temperature of coolant T two cases are selected, Fig, 3. Effect of coolant temperature on cooling curve.
namely saturated boiling which occurs similarly in
the ED process and subcool-boiling whose cooling tioned above on temperature T~ at which the transi-
ability is about double in comparison with ED tion from film boiling to nucleate boiling takes place.
process. The figure suggests that to delicately influ- In the case of cooling in warm water, T~ revealed
ences the cooling curve and that the occurrence of some peculiar changes. In other words, when to
pearlite transformation is observed when tp is long was about 4 s T. rose with drop in water tempera-
and T is high. ture, while when to was below 0.5 s T, remained
Figure 3 is the cooling curve when to is fixed at at about 500°C level and was independent of water
about 4 s and variables are the temperature of temperature. On the other hand, in the case of
coolant and the condition of with/without air bub- cooling in the air-water mixed fluid TTY always stood
bling. It was recognized that the film boiling was at about 500°C with stability. It may be concluded
stable enough to perimit pearlite transformation in from these facts that the air-water mixed fluid is
the air-water mixed fluid even if the coolant tempera- a good coolant on its stability and reappearance.
ture was as low as 80°C. Furthermore, it was found
that the cooling speed during the film boiling stage 3. Tensile Strength of Treated Wire Rod and Treating
clearly relates to the coolant temperature. These Conditions
two facts suggest that the air-water mixed fluid has 1. Preoxidation Time, Coolant Temperature and Kind
the great ability to be a new coolant for patenting. of Coolant
Figure 4 shows the effects of three factors men- Figure 5 shows the influence of t0, T and kind of
(44) Transactions ISIJ, Vol. 27, 1987

Fig. 6. Effect of gas flow rate on tensile strength.

equivalent to that attained by lead patenting.


2, Gas Flow Rate
Secondly, the experiment was carried out varying
the injection rate of air from zero to 2.7 m3/min.m2
under the constant condition in which t0=4 s and
T=80°C and the other experiment was carried out
Fig. 4. Influence of coolant temperature Tand air bubbling by injecting N2 gas instead of air. Figure 6 shows
on critical temperature T,.. the influence of gas flow rate v on TS. In the case
of air injection, the figure shows that when v is below
0.3 m3/min. m2, martensite transformation (marked
as the abnormal low TS spot) takes place due to the
nucleate boiling which is usual in warm water. It
also indicates that TS increases with increase in v
and film boiling becomes stable enough to suppress
the occurrence of an abnormal spot. However, in
the case of N2 gas injection, the nucleate boiling takes
place at the early stage of cooling resulting in abnor-
mal low TS. This is the very significant phenomenon
in the case where the gas-water mixed fluid is applied
as a coolant.
3. Relative Flow Velocity between Wire Rods and Coolant
Hot rolled wire rods are heat treated in the form
of overlapping non-concentric spirals during trans-
portation in the coolant vessel. In this case, the
effect of the relative flow velocity necessarily generated
between wire rods and coolant probably cannot be
ignored.
In this point of view, the experiment was carried
out to reveal the cooling behavior of specimens giving
the flow velocity by reciprocated motion of which
direction was normal or parallel to the wire rod axis.
Fig. 5. Effect of temperature of coolant on tensile strength As the coolant temperature, three levels were
of wire rod. selected, i.e., 100, 85 and 80°C. Figure 7 shows the
relation between TS and relative flow velocity and
coolant on TS. It is suggested as the general trend the following behavior has been made clear.
as follows : (1) Tensile strength increases linearly with in-
(1) Tensile strength increases linearly with de- crease in relative flow velocity.
crease in coolant temperature. (2) The flow velocity of which direction is per-
(2) In the case of subcool-boiling when the cool- pendicular to the rod axis gives higher rate of increase
ant temperature is below 90°C, the abnormal low in TS than that parallel to the rod axis.
TS values caused by martensite transformation due (3) The coolant temperature is the lower, the
to the nucleate boiling are apt to appear. rate of increase in TS is the higher.
In the case where to was about 4 s, TS of wire The cause of these phenomena can be explained
rods produced by cooling in gas-water mixed fluid that the flow velocity varys the thickness of steam
at 80°C was 10 kgf/mm2 above that produced by film generated on the rod surface and the coolant
cooling in boiling water. The wire rod was obtained temperature distribution close to the wire rod surface.
with TS as high as about 125 kgff mm2, which was Large variety of flow velocity necessarily take place
Transactions ISI1, Vol. 27, 1987 (45)

Fig. 7. Effect of relative flow speed between rod and coolant


on tensile strength of rod.
Fig. 8. Effect of various overlapping conditions of wire rods
on tensile strength.
in the actual operation and the informations obtained
through this experiment are reflected to a designing
point to secure the uniformity of mechanical properties on the specimen cooled in the gas-water mixed fluid.
within a coil. This fact suggests that whiskers are closely related to
4. Overlap of Rod Rings cooling behavior.8~
At the actual operation of direct heat treatment, 2. Time of Preoxidation and Reheating Temperature
wire rods are not treated in the shape of streight Figure 9 shows the surface condition observed by
bars but of rings. Therefore, rings are necessarily SEM as a function of to. Under the condition in
overlapped to some extent. Concerning to the varia- which t0=0.2 s, whiskers are not formed whether
tion in TS caused by overlap, it is reported that the bubbles are injected into the coolant or not. Under
cooling by dipping in boiling water (ED process) the condition in which to=1 ~4 s, the whisker forma-
gives smaller influence than the cooling by forced air tion was observed on the specimen cooled in warm
(Ste].mor process). The relation between TS and water, though it was suppressed when cooled in the
overlapping conditions in a gas-water mixed fluid gas-water mixed fluid.
is given in Fig. 8. This figure shows that the differ- Next, in order to clarify the condition which drives
ence in TS extends to 5 kgf/mm2 according to the whisker formation, many specimens cooled in warm
overlapping conditions. Therefore, in order to pro- water varying to and reheating temperature T,. were
duce the wire rod with better uniformity in mechan- prepared and then they were investigated by SEM
ical properties, it is necessary to take effective counter- whether whisker is formed or not. Figure 10 shows
measures to overcome this overlap problem. the bounds where whisker is formed and it is tolerably
limited.
4. Factors Concerningto the Behavior of Boiling 3. Kind of Gas
It was already mentioned in the previous section Since the whisker was not formed under the condi-
that the transition from film boiling to nucleate tion in which plenty of air was injected in warm
boiling greatly affects the characteristics of heat water, the key to cooling behavior seemed to be the
treatment. It was also made clear that in the case oxidation ability of bubbles. As the kinds of injec-
of cooling by subcool-boiling, the cooling behavior tion gas, 02, N2 and Ar were picked up and the same
and the TS obtained were definitely influenced by the experiment was carried out. The result came up
time of preoxidation and the existence of air bubbles to our expectations, namely when injection gas 02,
in the warm water. These are all deeply significant whisker was not observed and when N2 and Ar,
facts and the further analysis was carried out. whisker was formed.
1. Surface of Heat-treated Wire Rod
First, two specimens cooled by dipping in warm 5. Application of New Coolant of Gas-Water Mixed
water and the gaswater mixed fluid were prepared Fluid for ControlledCooling
under the condition in which the time of preoxidation Gas-water mixed fluid is the quite different coolant
was about 4 s. Evaporated Au was coated onto from the simple warm water and has excellent charac-
the rod surface and close observation was carried out teristis useful for heat treating the steel.
using SEM (Scanning Electron Microscope). It was (1) It provides the stable film boiling suppressing
found that whiskers were formed on the specimen the nucleate boiling at the cooling stage of 7O0'-
cooled in warm water and they appeared to be Fe- 500°C, which is the very important range of tempera-
Oxide. On the other hand, no whisker was found ture for heat treatment.
Transactions ISIJ, Vol. 27, 1987
(46)

Fig . 9. Scale morphology of rod surface and preoxidation time to (a) in warm water

and (b) in air-water mixed coolant.

III. Design and Operation of Multi-f unction


Direct Heat Treatment Equipment
Many systems have already been developed as the
direct heat treatment for hot rolled wire rod. Sumi-
tomo Electric Industries, Ltd. have newly developed
and installed the multi-function direct heat treatment
equipment of which principal technology is the new
coolant and the new cooling method. The equipment
covers a very wide range of cooling speeds of 2
100°C/s, which means each wire rod is enabled to
be subjected to the necessary heat treatment just after
being rolled.
The design policy, the structure and the operation
Fig . 10. Influences of preoxidation time to an d preoxidation
of the equipment are described below.
temperature on scale morphology.
1. Design of the System
1. Design Policy
(2) The cooling ability depends on the coolant Three principal points were decided at the begin-
temperature and it is greater than that of forced air ning of design as follows :
cooling. (1) The new process must cover several kinds of
(3) The cooling ability can be enhanced by the heat treatment from annealing to quenching, and for
relative flow velocity between wire rod and coolant. this purpose the cooling speeds have to be variable
Furthermore, for practical application, we have from 2 to 100°C/s. Table 1 shows the contents of
made clear quantitatively the way how to deal the treatments planned.
factors such as (1) rolling temperature (2) time of (2) The heat treatment must give rods enough
preoxidation, (3) coolant temperature, (4) kind, uniformity within a coil equivalent to that by off-
quantity and way of gas injection, (5) relative flow line (indirect) heat treatment. For instance, the
velocity, (6) overlap of rod rings, and so on. standard deviation of TS of the patented rod must
Transactions ISIJ, Vol. 27, 1987 (47)

be below 1.5 kgff mm2. When wire rod treavels through the coolant in the
(3) Several kinds of heat treatment must be shape of nonconcentric spirals, wire rod encounters
quickly converted from one to another in order not two kinds of lack of uniformity. One is that the
to decrease the productivity. rings are piled up at conveyor edge sides and the other
2. Designing is that the relative flow takes place between rod rings
(1) Structure and coolant and these are both important problems
As shown in Fig. 11, a laying head, a roller con- especially for the patenting treatment by the new
veyor for preoxidation and a dry/wet convertible coolant. For the former problem, the conveyor was
conveyor were successively arranged. designed to be able to (1) give the enough ring pitch,
For cooling below 10°C/s, the popular air cooling and (2) move the contact points among rings by
method consisting of roller conveyors was adopted. cascade conveying method at different speeds.
This roller type has the advantage of uniformity in For the later problem, the coolant circulation
heat treatment within a coil. For cooling above system by which the coolant is caused to flow in the
10°C/s, two continuous dipping and pulling up same direction as that of movement of rods in the
methods were adopted using warm water and gas-- vessel was installed to exclude the effect of relative
water mixed fluid as coolants. Buffer tanks were flow velocity.
prepared for each coolant. The new coolant was
made by skillfully injecting the oxidating gas into 2. Actual Operation
warm water so that the bubbles were plenty, uniform The operational conditions of wet line are as
and fine. follows:
(2) Control of the Cooling Speeds 1. Control of the Coolant Temperature
At the dry line, cooling speed was controlled by The importance and the way of temperature control
ring pitch, isolation covers and air blowers. At the for the new coolant is already mentioned above.
wet line, it was done by coolant circulating system Figure 12 shows the appearance of coolant tempera-
and hot/cold water mixing system using a micro- ture control in actual operation. The coolant tem-
computer which enables to control coolant tempera- perature at the inlet of processing tank was kept
ture precisely and easily. constant regardless of the rolling intervals, on the
(3) Improvement in the Uniformity of Cooling other hand the coolant temperature of the outlet
Generally speaking, in order to obtain the higher changed according to the wire rod existence. The
TS the more sensitive cooling conditions is necessary reason why the changes are not square comes from
and results in the worse uniformity within a coil. the fact that the movement of the wire rod and the

Table 1. Kinds of heat treatment.

Fig. 12. Change in temperature of coolant during opera-


tion of new process by gas-water mixed coolant.

Fig. 11. Sc hematic view of new process.


( 48 ) Transactions ISIJ, Vol. 27, 1987

coolant is not perfectly synchronous. erties of SWRS 82B steel rod, 13 mm in diameter
2. Flow Velocity of Coolant and it supports the feature that the new cooling
Figure 13 shows the distribution of flow velocity process is equivalent to lead patenting in the prop-
within a cross section perpendicular to a direction of erties of rod.
rod movement in the processing tank. Though the Figure 17 shows the mechanical properties of PC
flow velocity was not uniform through vertical direc- wire, 5.0 mm in diameter, which is cold drawn from
tion, it was comparatively uniform at near the pass a wire rod of 13 mm in diameter and it reveals that
height. This distribution was measured when the the wire has enough TS and ductility to satisfy the
conveyor was not carrying wire rod and the velocity specification of the final product.
measured at upper portion in actual operation was Equation (1) is the result of regression analysis on
lower than that shown in Fig. 12. This informs us TS of wire rod, 13 mm in diameter, cooled by this
that the distribution of flow velocity in actual opera- new method.
tion may be considerably uniform.
3. Troubles with Traveling TS= 31-0.7X TTw+93X[%C]+23X[%Mn]
At the early stage of start-up operation, many kinds +52 X [%Cr]+0.051 X T1+o.006+ T,.......... (1)
of traveling problem took place within a half year.
Almost all problems had been solved and now the
operation conditions are stable enough.

IV. Quality of Wire Rod Directly Heat Treated


The new process provides several kinds of a neces-
sary heat treatment for carbon steel, low alloy steel
and stainless steel wire rods whose diameters are in
the range of 5.0.'14.3 mm.

1. EDC Rod -
The feature of this EDC treatment is that the
appropriate TS level and higher uniformity can be
given to high carbon steel wire rod.9~ Hot rolled
wire rod is continuously put into the hot water kept
at boiling point and pulled up at about 400 °C. Fig. 14. Mec hanical properties of ED and EDC rod.
Though EDC has the most simple function of the new
process, this new one includes some additional
improvements compared with the other existing EDC
processes.
Figure 14 shows the mechanical properties of the
wire rod treated by EDC process in comparison with
that by old ED process and it reveals the higher
uniformity and ductility. Figure 15 shows the
variation in TS within a coil and a ring.

2. High Tensile Patented Rod


High tensile patented rod was manufactured by
the new cooling process with the new coolant ex-
plained in the previous section and the mechanical
properties were equivalent to those by lead patenting
process.
Figure 16 shows an example of mechanical prop-
Fig. 15. Variation in TS for EDC rod.

Fig. 13. Flow speed distribution of coolant in cross section

of processing tank. Fig. 16. Mechanical properties of patented rod.


Transactions ISIJ, Vol. 27, 1987 (49)

Table 2. Estimation concerning intensity of influence


of factors on tensile strength.

Fig. 17. Mechanical properties of PC wire.

where, TS : Tensile strength (kgf/mm2)


l w: Temperature of inlet coolant (°C)
T f : Temperature of rod at finishing roll
(°C)
TT,: Temperature of rod at laying head
(°C).
Concerning to the variables picked up in Eq. (1),
they are quality controlled in the actual operation
within such narrow ranges as shown in Table 2. The
variation in TS can be estimated by applying control
Fig. 18. Mechanical properties of AP rod.
range R to Eq. (1). Table 2 informs that the intensity
of influence on TS is ranked in the following ascending
order: finishing temperature, impurity element Cr%
and C%.

3. Air CooledRod
The high carbon steel wire rod mainly used for
tire cord is properly and uniformly cooled through
air cooling line in order to obtain especially high
drawability. This line is also applied for low alloy
steel and Fig. 18 shows the mechanical properties of
Si-Cr steel wire rod (equivalent to SAE 9254) for
valve springs and reveals its appropriate strength and
ductility to satisfy the cutting ability and cold
Fig . 19. Mechanical properties of DA rod.
drawability.

4. Direct AnnealedRod stainless steel is easily attained.


Though this process does not involve annealing in Table 3 shows the mechanical properties of a
the strict meaning but simple slow cooling treatment, quenched rod of 0.15 % C low alloy steel for rein-
sufficient heat treatment can be made in most cases. forcing member and it shows the considerably high
For the slower cooling, wire rods are piled thickly in TS and ductility.
the form of nonconcentric spirals and travels slowly Several kinds of heat treatment provided by the
through the tunnel covered by isolation plates. new process have been mentioned and the summary
Figure 19 shows the mechanical properties of wire of their mechanical properties are shown in Table 3.
rod for CO2 welding wire and it reveals that the rod
is softened enough to satisfy the considerably higher V. Summary
drawability. The cooling behavior of wire rod through boiling
In the case of manufacturing the high tensile phenomena in water was precisely observed and in-
quenched and tempered wire, hydrogen included in vestigated and the factors which affect the cooling be-
wire rods delicately affects the ageing phenomena just havior and the mechanical properties were made clear.
after tempering and the delayed failure during using. (1) The oxidative gas-water mixed fluid has
This problem is solved by this treatment. substantially different characteristics from those of
simple water and it can be taken as a new coolant
5. Direct QuenchedRod for patenting and all the problems for manufacture
Direct quenched rod is able to be manufactured by has been solved.
the appropriate combination of the chemical com- (2) The new multi-function direct heat treatment
position of steel and the cooling ability. For this equipment has been developed. Its principal tech-
purpose gas-water mixed fluid or water is used as nology is the new coolant and the new cooling method.
a coolant and the solution treatment for austenitic The equipment covers the very wide range of cooling
(50) Transactions ISIJ, Vol. 27, 1987

Table 3. Mechanical properties of rods treated by new process.

speeds 2 100°C/s. Therefore, each wire rod is DE Patent No. 1942731, (1980).
able to be subjected to the appropriate heat treatment 3) A. Tendler: Wire J., 14 (1981), 84.
according to the steel grade, uses and rod diameter. 4) H. Yada, T. Mori, M. Murakami, J. Tominaga and M.
Ochiai: Seitetsu Kenkyu, (1982), No. 310, 264.
(3) All the wire rods treated by the new process 5) K. Wakimoto, T. Inoue, K. Matsuoka, J. Tominaga and
have very high uniformity in mechanical properties K. Ito: Tetsu-to-Hagane, 69 (1983), 5570.
and metallurgical structure. 6) K. Nashimoto, K. Goto, Z. Tsutsumi, H. Kaneda, T.
Ninomiya, K. Azuma, K. Kawabata, T. Suzuki and M.
REFERENCES Omori : Tetsu-to-Hagane, 68 (1982), 51308.
1) K. Takeo, K. Maeda, T. Kamise, H. Iwata, Y. Satomi 7) M. Tagaya and I. Tamura: J. Japan Inst. Metals, B-15
and H. Nakata : Tetsu-to-Hagane, 60 (1974), 2135. (1951), 538.
2) Japanese Patent Publication No. 45-8536, (1970) and No. 8) K. Nishikawa, 0. Hasegawa, H. Honda, S. Sakaguchi:
46-8089, (1971). Trans. Japan Soc. Mech. Eng., 34 (1968), 134.
U.S. Patent No. 3669762, (1970). 9) G. Lessel and E. Grethen: Rev. Met., 76 (1979), 661.

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