U.S. patent number 3,725,521 [Application Number 05/085,240] was granted by the patent office on 1973-04-03 for method of making steel powder particles of select electrical resistivity.
This patent grant is currently assigned to A. O. Smith Corporation. Invention is credited to Hilmer F. Ebling.
United States Patent |
3,725,521 |
Ebling |
April 3, 1973 |
METHOD OF MAKING STEEL POWDER PARTICLES OF SELECT ELECTRICAL
RESISTIVITY
Abstract
A method of making a compressed steel powder article having high
resistivity to be used as an electrical component. Steel powder
having a particle size finer than 28 mesh is treated with a
non-aqueous solution of an organic thermosetting resin to coat the
particles with the resin. After evaporation of the solvent and
curing of the resin, the coated particles are compressed to form a
non-sintered, compressed steel powder article having high
electrical resistivity. The compressed article can be subsequently
heated to an elevated temperature to stress relieve the article and
stabilize the resistivity.
Inventors: |
Ebling; Hilmer F. (Milwaukee,
WI) |
Assignee: |
A. O. Smith Corporation
(Milwaukee, WI)
|
Family
ID: |
22190346 |
Appl.
No.: |
05/085,240 |
Filed: |
October 29, 1970 |
Current U.S.
Class: |
264/104; 419/1;
419/35; 419/10 |
Current CPC
Class: |
B22F
1/0059 (20130101); C22C 33/02 (20130101) |
Current International
Class: |
C22C
33/02 (20060101); B22F 1/00 (20060101); B22f
009/00 () |
Field of
Search: |
;264/111,104 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: White; Robert F.
Assistant Examiner: Hall, Jr.; J. R.
Claims
I claim:
1. A method of preparing a compressed steel powder article having a
predetermined electrical resistivity to be used in electrical
apparatus, comprising the steps of:
a. dissolving an uncured thermosetting resin in an organic
non-aqueous solvent to provide a treating solution,
b. blending the solution with a quantity of steel particles having
a particle size finer than 28 mesh and a carbon content in the
range of 0.001 to 0.10 percent by weight to coat said particles,
said resin on a solids basis being present in an amount of 0.06 to
1.0 percent by weight of the steel particles,
c. evaporating the solvent,
d. curing the resin to provide a flowable mass of coated particles,
and
e. compressing the coated particles at a pressure in the range of
30 to 100 tsi to mechanically interlock the steel particles and
form a compressed steel article having a density greater than 90
percent of the theoretical density of pure iron and having an
electrical resistivity in the range of 15 to 100,000 microhm
cm.
2. The method of claim 1, wherein the compressing is done at a
temperature below the sintering temperature of the steel
particles.
3. The method of claim 1, wherein the compressing is done at room
temperature.
4. A method of preparing a compressed steel powder article having a
predetermined electrical resistivity to be used in an electrical
apparatus comprising the steps of:
a. dissolving an uncured thermosetting resin having a decomposition
temperature in the range of 500.degree. to 1,200.degree.F in an
organic non-aqueous solvent to provide a treating solution,
b. blending the solution with a quantity of steel particles having
a particle size finer than 28 mesh and a carbon content in the
range of 0.001 to 0.10 percent by weight to coat said particles,
said resin on a solids basis being present in an amount of 0.06 to
1.0 percent by weight of the steel particles,
c. evaporating the solvent,
d. curing said resin to provide a flowable mass of coated
particles,
e. compressing the coated particles at a pressure in the range of
30 to 100 tsi to mechanically interlock the steel particles and
form a compressed steel article having a density g greater than 90
percent of the theoretical density of pure iron and having an
electrical resistivity in the range of 15 to 100,000 microhm cm.,
and
f. heating the compressed article to a temperature in the range of
500.degree. to 1,200.degree.F and below the decomposition
temperature of the resin to stress relieve the article and
stabilize the resistivity.
5. The method of claim 4, wherein said resin is selected from the
group consisting of silicone resins and polyimide resins.
Description
BACKGROUND OF THE INVENTION
This invention relates to a method of making a compressed steel
powder article having a select electrical resistivity.
Rotors, stators, and other magenetic cores, for use in electrical
equipment are usually not formed of single piece wrought materials
due to high eddy current losses developed in the low resistivity
wrought iron. The conventional practice in forming rotors, stators
and magnetic cores is to use a laminated structure formed from a
stack of thin rolled ferrous sheets. More recently, compressed
steel powder has been utilized to form high resistivity electrical
components by a process in which the steel particles are initially
coated with an electrically insulate coating prior to compressing
into the desired shape. U.S. Pat. No. 3,245,841 describes a process
of producing high electrical resistivity steel powder by treating
the steel powder with a phosphoric acid and chromic acid aqueous
solution to provide a surface coating on the steel particles,
consisting principally of iron phosphate and chromium
compounds.
It has been found that on a commercial scale the water used in the
treating solution, such as that disclosed in the aforementioned
patent, cannot be evaporated from a large mass of steel powder
without oxidation of the steel due to the difficulty in aerating
the powder mass. Oxidation of the steel particles results in a loss
of mechanical properties in the compressed part and lowers the
density of the compressed part.
It has also been found that when preparing electrical components
from steel powder that some compressed parts should be stress
relieved in order to obtain stability of resistivity under
operating conditions, which can be up to 300.degree.F, although
this may not be necessary in all applications. Thus, any
electrically insulating coating applied to the particles must be
capable of withstanding stress relieving without decomposing or
reacting with the steel, if the part is to be subjected to a stress
relieving treatment.
SUMMARY OF THE INVENTION
The invention is directed to a method of making a compressed steel
powder article having a select electrical resistivity which can be
used in a wide variety of electrical components. In accordance with
the invention, steel powder having a particle size finer than about
28 mesh is initially treated with a non-aqueous solution of an
uncured organic thermosetting resin to coat the individual
particles of steel powder. After evaporation of the solvent, the
coated particles are compressed to form a non-sintered compressed
powder article. In the compressed part, the cured resin should be
capable of maintaining its high electrical resistivity without
decomposing or reacting with the base metal at temperatures above
250.degree.F and up to 1,200.degree.F. To stabilize the resistivity
of the article at operation conditions, the compressed article can
be stress relieved at temperatures up to 1,200.degree.F.
The resulting heat treated, compressed steel powder part has a high
stabilized resistivity and can be operated at elevated temperatures
without substantial variation in resistivity.
As the coating is applied to the steel particles by use of a
non-aqueous solution, oxidation of the individual steel particles
will be prevented during the treating operation. The insures that
the mechanical properties of the compressed part will be maintained
and provides improved uniformity from part-to-part.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The steel powder to be employed can be prepared by the method shown
in the U.S. Pat. No. 3,325,277 to Huseby, in which a stream of
molten steel is atomized by a sheet of high pressure water to form
irregularly shaped particles which are subsequently heat treated to
soften the particles and reduce the carbon and residual oxygen
content.
The steel powder has a carbon content generally in the range of
0.001 to 0.1 percent and preferably less than 0.05 percent. In
addition, the steel may contain alloying additions such as nickel,
silicon aluminum, and the like, up to about 5 percent by weight,
depending upon the magnetic characteristics desired.
The size of the steel powder is not particularly critical and the
powder generally has a size finer than about 28 mesh (590 microns).
There is no limit to the fineness of the steel powder, but from a
practical standpoint, if the particle size is finer than 100 mesh,
the cost of the powder and the mechanical strength of the article
are diminished.
The steel particles are individually coated with an uncured organic
thermosetting resin. Silicone resins have proven very satisfactory
as the coating material. Polyorgano-siloxanes are characterized by
a molecular backbone of alternate atoms of silicon and oxygen with
organic groups attached to the silicon atoms. The type of organic
groups and the extent of crosslinking determine whether the
silicone will be fluid, elastomeric or resinous. The basic
polydimethylsiloxane structure is as follows: ##SPC1##
where X is an integer of at least 5.
More specifically, the following silicone resin can be employed:
##SPC2##
where both n and m are integers having a value in the range of 200
to 500.
In addition, polyimide resins of the type described in U.S. Pat.
Nos. 3,179,614 and 3,179,634 can also be utilized as the coating
material.
The amount of the resin to be used is important in carrying out the
invention, and generally, the resin is employed in an amount from
0.06 to 1.0 percent by weight of the steel powder, with
approximately 0.25 to 0.50 percent being preferred.
The resin is applied in the uncured state to the individual dual
steel particles by means of a non-aqueous treating solution. The
solvent to be employed in the solution can be any volatile organic
solvent, capable of dissolving the resin to be used. In general,
solvents such as toluene, xylene, benzene, and the like, may be
employed. As the solvent is subsequently evaporated and is not
present in the final product, the particular nature of the solvent
is not critical and any volatile readily available organic solvent
may be employed.
The concentration of the treating solution is not critical and the
solution can have any degree of dilution which will facilitate
mixing with the steel powder. It has been found that a
concentration in which 1 gram of the resin is dissolved in 160 to
240 ml of the solvent is satisfactory.
It is contemplated that a finely divided inert filler can be
incorporated with the resin. The filler should have a substantially
smaller particle size than the steel powder, and preferably has a
particle size finer than 10 microns. The filler may take the form
of quartz, diamotaceous earth, kaolin, talc, aluminum silicate,
calcium carbonate, and the like. The amount of filler, if used, is
not critical and the resin may contain from 0.01 to 3 parts by
weight of filler to one part resin. When a filler is utilized, the
combined weight of the filler and resin should be from 0.06 to 1.0
percent by weight of the steel powder.
As the filler will not be dissolved by the solvent, the particles
of filler will be dispersed or suspended in the treating solution.
In this case, when the treating solution is mixed with steel
powder, the resin and the filler will coat the steel particles.
The steel powder and the treating solution can be mixed together by
use of conventional blending equipment such as a rotating drum. It
is not necessary to heat the materials and the materials are
generally mixed together at room temperature. During the mixing
operation, the treating solution will tend to completely coat or
encapsulate the individual steel particles.
After the mixing operation, the solvent is evaporated. While
heating is not necessary for evaporation of the solvent, under
normal conditions, heating is utilized in order to accelerate the
evaporation. Following evaporation of the solvent, the resin is
cured. While the resin will crosslink or cure at room temperature,
heat is preferred to accelerate the cure. In practice, it has been
found that heating the coated particles to a temperature in the
range of about 150.degree. to 250.degree.F for a period of 15 to 60
minutes will not only evaporate the solvent during the initial
stage of the heating treatment, but will also cure the resin in the
latter state of this heat treatment.
The thickness of the cured coating is not critical, but it is
believed that the coating, in most cases, is continuous to
virtually encapsulate the individual steel particles and is
generally less than 1 micron in thickness. Due to the very thin
nature of the coating, the particles after curing of the resin,
will not adhere together, but the powder mass will still be
flowable although the rate of flow will not be as great as the
uncoated particles.
After curing of the coating, the coated particles are compressed
into the shape of the desired component or article. The compressing
is preferably carried out at room temperature, although
temperatures up to the decomposition temperature of the resin can
be used. The coated powder is compressed preferably with a pressure
in excess of 50 tsi and generally in the range of about 30 to 100
tsi. During the compression, the coating will flow and squeeze
between the particles. As the compression is normally done without
heating there will be no sintering of the steel particles and the
particles will be held together primarily by the mechanical
interlock between the irregular particles and the adhesive nature
of the coating.
In the compressed part, the cured resin is characterized by the
ability to maintain its high electrical resistance without
decomposing or reacting with the steel when heated to a temperature
in the range of 250.degree. to 1,200.degree.F
Following compression, the compressed part can be stress relieved
by heating to a temperature in the range from about 500.degree. to
1,200 .degree.F and below the decomposition temperature of the
resin coating. The heat treatment serves a multiple function in
that it removes stress from the compressed part, stabilizes the
resistivity so that the resistivity will be less likely to change
during service, and increases the mechanical strength of the
compressed part. If the compressed part is to be stress relieved,
the resin to be used as the coating should have a decomposition
temperature in the upper portion of the 250.degree.F to
1,200.degree.F so that the part can be heated to the stress
relieving temperature without decomposition of the resin. If the
part is not to be stress relieved, then a resin having a lower
decomposition temperature can be used.
After stress relieving treatment the part is cooled to room
temperature.
It has been found that improved properties are obtained if the
resin is fully cured prior to compression, rather than curing the
resin during the stress relieving treatment and following
compression. It is believed that fully curing the resin prior to
compression volatizes all of the solvent, so that there is no
residual solvent present in the particle mass which would adversely
affect the compression.
The compressed part has a density of at least 90 percent of
theoretical density of iron and generally the treated powder has a
compressibility greater than 7.4 grams/cc at a compaction pressure
of 60 tsi.
The compressed iron powder article of the method of the invention
can be used for a wide variety of electrical components such as
rotors, stators, transformer cores, chokes, and the like. The
electrical resistivity of the compressed part can vary between 15
to 100,000 microhm cm. with the particular resistivity depending on
the ultimate function and use of the electrical component.
The use of the silicone resin as the coating material has the added
advantage that it serves as a lubricant during the compression
step. By using the silicone resin it is not necessary to lubricate
the die with a separate lubricant during the compression step.
The following examples illustrate the process of the invention.
EXAMPLE I
908 grams of steel powder having a carbon content of 0.005 percent
and having a particle size in the range of 28 to 100 mesh were
mixed with 50 ml of a 0.25 percent by weight toluene solution of
silicone resin GE-RTV 102. After thorough mixing of the ingredients
the resulting coated powder was heated in a circulating oven at a
temperature of 250.degree.F to evaporate the toluene and cure the
resin.
Following the heating the coated particles were compressed at room
temperature at 60 tsi into a part having the dimensions 1 1/4
.times. 1/2 .times. 1/4 inches. Subsequently the compressed part
was heated to a temperature of 800.degree.F for a period of 1 hour
to stress relieve the part and stabilize the resistivity.
The resulting heat treated steel powder part had a density of 7.41
grams/cc. The part had a resistivity of 15,000 microhm cm., as
pressed, and a resistivity of 1,800 microhm cm. after stress
relieving.
The compressed part had a transverse rupture strength of 4,830 psi,
as pressed, and 8,590 psi after the stress relieving treatment.
EXAMPLE II
908 grams of steel powder having a carbon content of 0.005 percent
and a particle size finer than 28 mesh were mixed with 170 ml of a
0.25 percent toluene solution of silicone resin GE RTV-106.
After thorough mixing of the ingredients to coat the particles the
mixture was heated in a circulating oven to a temperature of
250.degree.F to evaporate the solvent and cure the resin. The
coated particles were then compressed at room temperature and at a
pressure of 60 tsi into an article having the dimensions 1 1/4
.times. 1/2 .times. 1/4 - inches.
The compressed part was then stress relieved at a temperature of
800.degree.F for a period of 1 hour.
The resulting stress relieved part had a density of 7.40 grams/cc,
and a resistivity, as pressed, of 7,300 microhm cm. and a
resistivity, after stress relieving, of 1,300 microhm cm.
EXAMPLE III
A compressed steel powder part was prepared in a manner similar to
that of Example I, except the treating solution contained 0.06
percent of silicone resin GE RTV-102.
The resulting compressed and stress relieved part had a density of
7.43 grams/cc and the compressed powder part had a resistivity of
16,500 microhm cm., as pressed, and a resistivity of 1,200 microhm
cm. after stress relieving.
The compressed article had a transverse rupture strength of 5,800
psi, as pressed, and 10,000 psi after stress relieving.
Various modes of carrying out the invention are contemplated as
being within the scope of the following claims particularly
pointing out and distinctly claiming the subject matter which is
regarded as the invention.
* * * * *