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L, 1 laden
5-5/1" M’ UNETED' STATES PATENT OFFECE
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2,119,488
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ALLOYS AND PROCESS or minus SAME
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Henry N. l'adowicz, Bloom?eld, N. 3., assignor to
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Sirian Wire and Contact Company, Newark.
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N. 1., a corporation of Delaware
No Drawing. Application July 31, 1936,
Serial ‘No. 93,733
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15 Claims. (Cl. 75-136)
.1
The present invention relates to the production
,
of hard metal alloys, and it particularly relates
xiii)?" ‘_ to the production of alloys which may be uti-
dium. or it may be utilized in the amount of
between 1% and 5%‘.
It has been iound desirable to combine these
r
I
is’! I lized for making various types of cutting tools,
’ l
carbides with substantial amounts of cobalt, iron
wear-resisting implements. and so forth.
It has been proposed to make ‘hard metal
and/or nickel. and this may be done by adding‘,r 5
the ?nely divided carbide mixture to a solu- .
bodies from combinations of tungsten carbide
and cobalt which are sintercd together at temperatures between 1500' C. and 1600‘ C. It has
10 been found. however. that the hard metal alloys
tion, slurry or liquid dispersion of the water
soluble. organic cobalt or nickel‘compound. This
method-of combining nickel and cobalt with the
carbides is more fully described and setAortlf1m'~~~-.__
produced according to these processes. although
in co-pending.applioatloniserialljlgf??ili. ?led‘ -
quite
Julyalst. 1936.
expensive and
di?icult ‘to'manuiacture.
nevertheless are not fully satisfactory in their
; .
1-
'
hardness and wearing
‘ -
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In the-preferred procedure.
-
,
intzsaid'.
co-pendin: applleatton.-;the pulvedged and; __ii1_1ely_v
15 i It is among the objects of t 5 present inven—
divided :carblde
added ‘I to a' "colleen-31s
>_ iiou to prepare an improved 'haruv'iiéwilioy‘“tluirdrsolutionkoiialwbuitgsalkslhelpm;_
,
__“_
»—éitii?miiandzoi1iligiiuillyli?ils_p?ct10.
‘cobalt-acetate.
cobglirsalt mine‘-
In iieu‘jz'cf'
- - '
strenntli',"hardness and density, which. may, be opartp?gll?o - 'e‘icoff tqacetate'itrwposslblertopr-r-w-u
made of uniform quality from
‘to batch. use other solublcf?lts'isucnas cobaltsulphatc.
go and which will have a ‘sullicient degree of tough-
cobalt chloride; or, cobaltnitrate. and preferably ' 20
bass and density toenable its-wide utilization _, the cobalt-gsaltjisusednin the :i‘onn ota concen-v
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5E " aE
in connection with 'wl‘ EE
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'r E
' 5
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g
saturated
cutting tools,'and so forth.‘
' _
e
-
- -- -
and even carry
Other objects will be obvious and will appear
9;, during the course‘ of the ‘following speci?cation.
pension.
In accomplishing the objects of the present
I
-
;
~ ~ In lieu of some or all
V
.
_
g.
‘
the cobalt-‘compound
invention it has been found most suitable to
prepare a mixture of ?nely divided carbides of
or compounds above mentioned it is'posslble to
include the corresponding iron ‘or nickel com
rel'ractory
pounds.
metals, _said_ mixture
preferably iu-
39 eluding two or more of the iollowing carbides: >
-
particles of the cobaltv
salt or‘ even insoluble cobalteompounds in sus
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..
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.e
._
-
The propog?ouing ‘Q1 the refractory metapor' 3o
titanium carbide. tungsten carbide. tantalum of the additional metal such as cobalt. nlekclior
carbide. vanadium carbide. thorium carbide. mo-‘ item or “the who“. is preferably such mag
lybdenum carbide, uranium carbide, cglumbium - the ?nal refractory mem‘wm constitute between
carbide, and chromiumcarbide,v These carbides 50% to 30% of the aJ1oy,__or.ln seine instances
'2.‘ are usually best prepar
by obtaining the ?nely
betwcenaboutasqtito ,sosagor the ailjoyzjajmle 35
divided metal in pure condition, the metal being
the additional _mega1
, constitute ;___b_ety¢m -
most preferably prepared by reduction in a hy~v about 10%: and-141% ,_~,9I._the* alloy."
drogen atmosphere in anclectric furnace. '
. _
These ?nely divided refractory metals arcpreiw carbon wm'cons‘umtéhp owl-2%
49 erably carburized' by heating
?nely alloy. and
b°_-1o%' tools
‘divided carbon, preferably:- ot- the t-gpehknowi: instances:
l v _
'_
as sugar carbon, in a _:‘e u ng'a
insvsonie
mm-m¢m:m;_25%.9km¢ an”.
esp cm
In
3g:
‘ n
-
méauoif?tini'the car
_
an deem‘: furnace’ fvmch “and”; atmosphere ture alnd solution of the‘cobalfacetate'the'?nely'
may desirably include hydrocarbon gases sue
divided carbides .ar-e mixcdwr mined together
4:. as acetylene. ethylene, methane. and so forth.
These
~
finely
.- s“ divided
s,‘ 1“; carbides
.1
“Aveare ‘then
'
migced
Han
an, are- m” _ 1,159.,‘aw‘; thq¢éamwacéatc 4
505mm .
égg?éég?is
v ‘é‘gporziéd
v
_ of
‘way
a
f?'ictf?lrlli
“L33”?
v?iffiiiiaiflipigdiil- stirring
until a ‘dry solidsma'ss isground
obtained.
This '
‘w “WW
m w‘ - “WW” ___________ W
solid mass m'aythen be
and sub
H—n
?nal lmr'd metal alloy.
_
_
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‘13:19:11?
P the ng'cfgrrcd propel-liens _ are bgt‘veen
‘
if; in carbide:
19';- ef iitanimn.
vanadium
chro
mium
hetwocn 60%
‘.10 '35 and/or
of tungsten
carbi?c: and bets-‘sen 10% to 25% of tantalum
cai'b'zde. Where chromium carbide is also includcd, it may replace the titanium or vanaI
in CH
_
_
_
.
!
bar
Jected
furnacet0in
rcductlon.
hydrogen
mostatmosphere.
desu'ably in an’
After
0 8Cthis
‘a...’
reduction OWN-tier! has been comi-‘l‘l’l-ed the T‘?
sultant mass ‘may be formed or pressed to de
sired shapes and then sintered to form the ?n
lshed article readyi for commercial use in cut- 65
2
2,119,488
ting tools, drawing dies, wear-resisting parts,
and so forth.
0
The following are several typical examples of
carblde mixtures which may be prepared for
incorporation with the cobalt or nickel salt solu—
tion, said carbides being preferably produced by
reduction or carburizat-ion in a hydrogen atmos
phere;
'
Example 1.-—In parts by weight: 5 of titanium
10 carbide, 63 of tungsten carbide, 20 of tantalum
carbide, and 2 of vanadium carbide.
-
Example 2.—In parts by weight: 4 of titanium
carbide, l of chromium carbide, and 84 of tung
sten carbide.
Example 3.--In parts by weight: 2 of chromium
carbide, 35 of tungsten carbide, and 53 of tan
talum carbide.
15
Example 4.—In parts by weight: 38 of titanium
carbide, 4'10 of tungsten carbide, 150 of tantalum
20 carbide, and 15 of vanadium carbide.
Example 5.-—In parts by weight: 30 of tungsten
carbide and 60 of tantalum carbide.
_
Example 6.-In parts by weight: 3 of chro
mium carbide, 5 of titanium carbide, 5 of thorium
25 carbide, 10 of molybdenum carbide, 20 of tung
sten carbide, and 20 of tantalum carbide.
_ ‘
Example ?.—-In parts by weight: 30 of titanium
carbide, B of chromium carbide, and 636 of tungé
v‘sten carbide.
Example 8.—-In parts by weight: 15 of chromi
30
um carbide, 260 of tungsten carbide, and 400 of
tantalum carbide.
,
In each case these carbides have been prefer—
ably prepared by carburizing the ?nely divided,
35 pure metal with sugar carbon in a hydrogen at
miesnhemprtiro .nqnsatatammrawlie 0.21.290’
C. £0,169? C. ‘ The metal sfié?ders?may he sepa
rately carburized or they may be mixed together
before carburization. 'These metal powders after
40 carburization are milled for a couple of days.
preferably without balls,‘ to give a ?nely divided
mixture having a ?neness exceeding 180 mesh.
According toone desirable process of combina
pendent upon the size of the pieces. The tubes
are then pushed into the cooler and when cold
they are withdrawn.
Although the high temperature treatments,
namely the carburizing, the reduction, and the
sintering, are carried out in reducing atmos
pheres, it has been found most suitable to carry
out the carburizing in a hydrocarbon atmosphere,
while the reduction and sintering operations are
carried out in a reducing atmosphere, preferably
of hydrogen.
The present application is particularly directed
to the combination of mixtures of refractory
metal carbides with cobalt or nickel, with the
cobalt or nickel being in the form of a water sol
15
uble organic salt compound. The process of
combining a refractory metal carbide witha solu
tion of cobalt acetate or other cobalt or nickel
salts is more fully described and claimed in co~
pending application Serial No. 931734, ?led July 20
31st, 1936.
It is also possible to combine ?nely
divided refractory metal powder with the metallic
carbides before such metallic carbides are com
bined with the cobalt acetate solution.
Processes in which the tungsten or other re
fractory metal is combined in finely divided form
with the cobalt or nickel salt, are more fully de
scribed and claimed in, co-pending application
Serial No. 93,171, ?led July 29, 1936.
Many other changes could be effected in the 30
particular features of process treatment 'dis~
closed, and in speci?c details thereof, without
substantially departing from the invention in
tended to be de?ned in the claims, the speci?c de
scription herein merely serving to illustrate cer 35
tain elements by which, in one embodiment, the
spirit of'th'é’ invent-1011' may ‘be eliectuated.
What I desire to claim is:
'
>
1. A process of preparing hard metal alloys
which comprises combining a ?nelyclivided mix
ture of refractory metal carbides and then com
bining this mixture with a water solution of an '
organic salt of an additional metal selected from
and then sprinkled into a solution of 370 parts by
weight of crystallized cobalt acetate in 1,000 parts
the group consisting, of iron, nickel and cobalt,
said water solution being concentrated and being 45
evaporated down‘ to dryness while continually
stirring, the dry material being pulverized" and
by weight of water.
sifted and then reduced in a reducing atmos
tion, the milled carbide mixture of Examples 4, 7,
or, 8 is sieved through a 180 mesh screen or sieve
'
Of course the cobalt may be replaced in part or
whole by equivalent quantities of nickel or iron
salts. The solution containing the cobalt ace
tate is then evaporated to dryness with constant
stirring and the residue is dried forabout ten
hours and then thoroughly pulverized so that it
may be bolted through a 180 mesh screen.
This powder is then loaded into nickel boats
phere.
_
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v
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,
2. A process of preparing refractory metal al-'
loys which comprises combining a mixture of
?nely divided carbides of refractory metals with a
water solution of an organicacid salt of cobalt,
said water solution being. concentrated and'being
evaporated down to dryness. while continually 55
stirring, the dry material being pulverized and
and reduced in 'a hydrogen atmosphere in an
sifted and then reduced in..a reducing atmos-v
electric , furnace
phere.
schedule:
according
to
the
following
,
60
Held ‘A hour at 20 volts
Held 1% hours at 50 volts
Held 1A hour at 70 volts
Held 1A hour at 100 volts
Held 1%; hours at 130 volts
65
The temperature then reaches about 600‘? C.,
which is maintained until reduction is complete.
The boats are then pushed into the cooler and
allowed approximately ?fteen minutes to cool.
The ?nal product, which is in the form of a very
fine powder, is then formed under pressure to the
desired shape. The formed pieces are then
placed in carbon tubes and heated in a hydrogen
atmosphere in an electric furnace to approxi
mately 1450° C. for thirty minutes or longer, de
'
'
3. A process of preparing hard metal alloys"
which comprises combining a mixture of tungsten 60
and tantalum carbides with a water solution of
an organic acid salt of cobalt, said water solu
tion being concentrated and being evaporated
down to dryness while continually stirring, the
dry material being pulverized and sifted and then
reduced in a reducing atmosphere. ‘I
" ‘i. A process of preparing hard metal alloys
which comprises combining a mixture. of tung—
sten and tantalum carbides with a water solution
of an organic acid salt of nickel, said water solu
tion being concentrated and being evaporated
down to dryness wniie continually stirring, the
dry material being pulverized and sifted and then
reduced in a reducing atmosphere.
5. A process of preparing hard metal alloys
2,119,488
which comprises carburizing a mixture of at least
two refractory metals, and then combining the
mixture with a water solution of an organic acid
salt of cobalt, said water solution being concen
' trated and being evaporated down to dryness
while continually stirring, the dry material being
pulverized and sifted and then reduced in a re~
ducing atmosphere;
6. A process of preparing hard metal alloys
10 which comprises carburizing tungsten and tan
talum with sugar carbon, milling the carbides,
sifting the carbides through a 180 mesh screen,
and combining the carbides with a water solution
of an organic acid salt of cobalt, said water solu
15 tlon being concentrated and being evaporated
down to dryness while continually stirring, the
dry material being pulverized and sifted and then
reduced in a reducing atmosphere.
7. A process of preparing hard metal alloys
20 which comprises milling together carbides of
tungsten and tantalum, sifting the carbides
through a 180 mesh screen, and combining the _
carbides with cobalt, said combination being ef—
fected by sprinkling the sifted carbides into a
concentrated solution of cobalt acetate, evapo
rating to dryness with agitation, reducing the
dried mixture and sintering.
8. A method of making hard metal alloys
which comprises combining together at least two
30 ?nely divided refractory metal carbides selected
from the group consisting of titanium, tantalum,
tungsten,
chromium,
uranium,
molybdenum,
thorium and vanadium, and combining said car
bides with a Water solution of an organic acid
35 salt of cobalt, said water solution being concen
trated and being evaporated down to dryness
while continually stirring, the dry material be
ing pulverized and sifted and then reduced in
a reducing atmosphere.
9. A method of making hard metal alloys
40 which comprises combining together at least two
?nely divided refractory metal carbides selected
from the group consisting of titanium, tantalum,
tungsten, chromium, uranium, molybdenum,
thorium, vanadium, and sprinkling said carbides
into a concentrated cobalt acetate solution, evap
orating said solution to dryness with agitation,
powdering, reducing the powder in a hydrogen
atmosphere, forming the reduced powder, and
sintering.
10. A process of producing refractory metal al
loys which comprises combining together ?nely
divided refractory metal carbides and the ?nely
divided refractory metals, and then combining
55
this mixture with a water solution of an organic
3
acid salt of cobalt, said water solution being con
centrated and being evaporated down to dryness
while continually stirring, the dry material being
pulverized and sifted and then reduced in a re~
ducing atmosphere.
11. A hard metal alloycomprising about 90%
of a mixture of tantalum and tungsten carbides,
and about 10% of a mixture of nickel and cobalt,
the particles of the carbide being each encased
in and cemented together by a coating of nickel 10
and cobalt, said alloy being prepared by mixing
the carbides with a salt solution of the encasing
metal, followed by evaporating, drying, pulveriz
ing, reducing, compressing and sintering.
12. A hard metal alloy comprising about 90%
of a mixture of tantalum and tungsten carbides,
and about 10% of cobalt, the carbide particles
being each encased in and cemented together by
a cobalt coating, said alloy being prepared by
mixing the carbides with a salt solution of the
encasing metal followed by evaporating, drying,
pulverizing, reducing, compressing and sintering.
13, A process of ,producing a hard metal alloy
which comprises evaporating a slurry containing
and reducing the resultant mixture of ?nely di
vided cobalt acetate, tungsten carbide and tan
talum carbide, forming, and sintering, the car
bide particles being each encased by cobalt ace
tate before reduction.
14. A hard metal alloy consisting of finely di 30
vided tungsten and tantalum carbides, the par
ticles of which are each encased in, and cemented
together by, a coating of an additional metal
selected from the group consisting of iron, cobalt
and nickel, said alloy being prepared by mixing
the finely divided tungsten and tantalunncare
bides with a solution of a water soluble salt of
the additional metal to form a slurry followed
by reduction to dryness with constant agitation,
reduction of the dried mixture in hydrogen and 40
sintering.
15. A hard metal alloy consisting of finely di
vided tungsten and tantalum carbides, the par
ticles of which are each encased in. and cemented
together by, a coating of an additional metal
selected from the group consisting of iron, cobalt
and nickel, said alloy being prepared by mixing
the finely divided tungsten and tantalum car
bides with a solution of a water soluble salt of
the additional metal to form a slurry followed by
reduction to dryness with constant agitation, re
duction of the dried mixture in hydrogen and
sintering, said tungsten carbide being utilized in
greater proportion than the tantalum carbide.
HENRY N. PADOWICZ.
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