U.S. patent number 3,889,019 [Application Number 05/171,292] was granted by the patent office on 1975-06-10 for vapor randomization in vacuum deposition of coatings.
This patent grant is currently assigned to United Aircraft Corporation. Invention is credited to Mitchell J. Bala, Sol S. Blecherman, Dennis J. Evans, Nicholas E. Ulion.
United States Patent |
3,889,019 |
Blecherman , et al. |
June 10, 1975 |
Vapor randomization in vacuum deposition of coatings
Abstract
In the processes for forming protective coatings on metal
substrates, particularly the nickel-base and cobalt-base
superalloys, by deposition in vacuum, an inert gas leak adjacent
the substrate is utilized to randomize the coating vapor cloud and
cause non line-of-sight deposition.
Inventors: |
Blecherman; Sol S. (Newington,
CT), Bala; Mitchell J. (Hazardville, CT), Evans; Dennis
J. (Rocky Hill, CT), Ulion; Nicholas E. (Vernon,
CT) |
Assignee: |
United Aircraft Corporation
(East Hartford, CT)
|
Family
ID: |
26866927 |
Appl.
No.: |
05/171,292 |
Filed: |
August 12, 1971 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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806873 |
Mar 13, 1969 |
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Current U.S.
Class: |
427/251;
118/726 |
Current CPC
Class: |
C23C
14/24 (20130101) |
Current International
Class: |
C23C
14/24 (20060101); C23c 013/02 (); C23c
013/04 () |
Field of
Search: |
;117/106,107,119,93.1GD,93.1DH,93.2,93,93.3 ;118/49.5,50.1
;204/192 |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
Holland, L., Vacuum Deposition of Thin Films, Wiley & Sons,
Inc., New York, 1956, pp. 4-6. .
Lentz, J. J., Vacuum Evaporation Procedure, IBM Tech. Disc. Bul.,
Vol. 5, No. 1, 6-1962, p. 21. .
DaSilva et al., Fabrication of Al.sub.2 O.sub.3 Films, IBM Tech.
Disc. Bul., Vol. 4, No. 6, 12-1961, pp. 6-7..
|
Primary Examiner: Van Horn; Charles E.
Assistant Examiner: Massie; Jerome W.
Attorney, Agent or Firm: Del Ponti; John D.
Parent Case Text
This application is a continuation of Ser. No. 806,873, filed Mar.
13, 1969, now abandoned.
Claims
What is claimed is:
1. A process of vacuum vapor depositing a protective metal coating
on a metallic substrate comprising:
positioning a source of material to be vaporized within an
evacuated enclosure;
positioning the substrate within the enclosure above said source in
direct line-of-sight thereof such that vapor particles produced by
heating said source material impinge on and coat line-of-sight
portions of said substrate;
heating said source material to produce a vapor cloud of coating
material moving generally line-of-sight from said source to said
substrate and coating line-of-sight portions of the substrate;
introducing at low velocity an inert gas to increase the pressure
in the enclosure to at least 2.0 .times. 10.sup.-.sup.4 mm Hg to
decrease the mean free collision path of vapor cloud atoms to
randomize their direction and cause coating of non-line-of-sight
portions of said substrate, said pressure being sufficiently low to
prevent sustaining a gas plasma discharge.
2. The method of claim 1 wherein the inert gas is helium.
Description
BACKGROUND OF THE INVENTION
The present invention relates in general to metal coating processes
and apparatus therefor and, more particularly, to vacuum deposition
processes.
It is well known that the conventional nickel-base and cobalt-base
superalloys do not in and of themselves exhibit sufficient
oxidation-erosion resistance to provide component operating lives
of reasonable duration in the dynamic oxidizing environments such
as those associated with the operation of gas turbine engines.
Accordingly, it has been the usual practice to provide these alloys
with a protective coating in such applications.
Although the aluminide coatings, such as that described in the U.S.
Pat. No. to Joseph, No. 3,102,044, have in the past displayed
satisfactory performance, it is well known that these coatings,
because of their dependence upon the availability of substrate
elements, often are characterized by a composition less than
optimum. Furthermore, these coatings are often achieved only at the
expense of some mechanical property less in substrate strength.
Many of the more advanced coatings developed for the next
generation of jet engines depend in the first instance on the
deposition of a high melting point coating alloy with a concurrent
or subsequent reaction with the substrate to attain the desired end
composition, microstructure or adherence. These new alloys
generally demand the application of special coating techniques to
provide the right species in the right amounts at the surfaces to
be protected.
Several coating compositions of current interest are described in
detail in copending applications of the present assignee. Among
these compositions is that hereinafter referred to as the FeCrAlY
coating at a nominal composition of, by weight, 30 percent
chromium, 15 percent aluminum, 0.5 percent yttrium, balance iron,
as discussed in the copending application of Frank P. Talboom, Jr.,
et al entitled "Iron Base Coating for the Superalloys," Ser. No.
731,650 filed May 23, 1968. Another such composition is the CoCrAlY
composition at about, by weight, 21 percent chromium, 15 percent
aluminum, 0.7 percent yttrium, balance cobalt.
The basic problems associated with the deposition of these coating
alloys relates to their high melting points and the difficulty of
providing the right amount of all of the alloy species in the
coating as applied. Satisfactory results have been attained through
the use of vacuum vapor deposition techniques, such as that
suggested in the U.S. Pat. No. to Steigerwald 2,746,420. These
processes, which have in the past been primarily directed toward
the application of relatively low temperature materials of
relatively simple composition, are in the present instance
characterized by extreme sensitivity to variations in the process
parameters and, accordingly, reproducibility as well as processing
expense is a problem.
The vacuum vapor deposition of electron beam melted metals in
existing low evaporation rate, production-type systems, such as
high cyclic speed or strip line coaters, has essentially been
limited to line-of-sight coating from the source (molten pool of
coating metal) to rotating or linearly moving substrates. Recently,
several techniques have been developed to improve the versatility
of the basic process through collimation or densification of the
vapor cloud. In one such method, a gas cascade or multi-orificed
nozzle surrounding the pool of molten coating material is utilized
to introduce a high velocity inert gas inwardly at an angle to the
vapor cloud to densify the direction of the metal vapor atoms thus
permitting increased coating rates of line-of-sight areas. In
another such method, a high mass, high temperature reflector is
utilized to the same end.
SUMMARY OF THE INVENTION
The present invention contemplates a vacuum deposition process
which utilizes controlled inert gas impingement on the vapor cloud
to randomize and redirect the coating material vapor cloud. For
this purpose, a low velocity, inert gas leak is admitted, to a
chamber pressure sufficiently low to prevent sustaining a gas
plasma but sufficiently high to substantially decrease the mean
free collision path of the metal vapor atoms in the vicinity of the
surface to be coated, to randomize the direction of the metal vapor
atoms and, in essence, to cause coating of non line-of-sight
areas.
BRIEF DESCRIPTION OF THE DRAWING
An understanding of the invention will become more apparent to
those skilled in the art by reference to the following detailed
description when viewed in light of the accompanying drawing,
wherein is shown a schematic illustration, partially in section, of
vacuum vapor coating apparatus in accordance with this
invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In one particular embodiment as illustrated in the drawing, there
is shown a vacuum chamber 10 having an exit port 12 leading to a
suitable high vacuum pump, preferably of the diffusion type, for
the rapid and continuous evacuation of the chamber. Located inside
the chamber, there is shown an electron gun 14 for generating a
beam of charged particles to impinge upon and vaporize an ingot of
source metal 16. It will be appreciated by those skilled in the art
that the electron beam is suitably directed by conventional
magnetic deflection pole pieces 18. Of course, the arrangement of
the electron beam gun within the vacuum chamber is a function of
design. A 30 kilowatt electron beam unit has provided satisfactory
deposition rates with a two inch diameter ingot of a FeCrAlY
coating material the depth of the molten pool usually being 1/4 -
1/2 inch.
The ingot 16 is made movable and is slidably received at its upper
end by an annular water cooled crucible 20. The ingot is normally
continuously fed upwardly into the crucible through a heat
resistant vacuum seal 22 in the chamber wall at a controlled rate
by a chuck 24 to maintain a constant pool height.
It is important that the pool elevation be maintained constant not
only because the coating efficiency, composition and uniformity are
very susceptible to pool height changes, but also so that the
focused electron beam will impinge only on the desired pool surface
area.
The substrate to be coated is disposed within the vacuum chamber 10
vertically above the ingot 16 and is illustrated as a gas turbine
blade 26 having an airfoil section 28 and a shroud section 30.
Since the coating process is fundamentally line-of-sight, the part
is typically mounted to effect rotation about its longitudinal
axis, that is, the longitudinal axis of the airfoil 28, usually
utilizing a pass-through (not shown) through the vacuum chamber to
an external drive system. Of course, more than one part may be
coated at a time. In such a case, in order to minimize
non-uniformity of coating between each of the plurality of parts,
each part is normally mounted in a plane of vapor isodensity or
roughly along an arc defining a zone of constant vapor
concentration, the parts closest to the vertical passing through
the center of the molten pool being located slightly farther from
the pool surface than those positioned at an angle with respect to
the said vertical. Whether coating a single part or a plurality of
parts however, each substrate is further positioned as close as
possible to the surface of the molten source pool for maximum
coating efficiency but far enough removed therefrom to prevent
coating contamination by splash from the pool. The substrate height
varies with each system but for a 2 inch diameter pool and a
deposition rate of about 0.3 mils per minute with a FeCrAlY coating
material, a mean height of about 10 inches has been found
satisfactory.
As mentioned previously, the vacuum vapor coating process is
essentially line-of-sight. Although axial rotation of the part is
successful in effecting deposition along its entire length, it does
not alleviate the problem of coating the remaining end portions.
This is particularly unsatisfactory in a substrate having an
enlarged end portion such as the shroud 30 of the turbine blade 26.
In accordance with the present invention, there is provided an
inert gas line 32 adjacent the outer surface of shroud. The line 32
admits an inert gas, preferably helium, at a low velocity from a
location generally above and outwardly from the shroud in a
direction generally downwardly and inwardly theretoward. The inert
gas leak is controlled to a chamber pressure sufficiently low to
prevent sustaining a gas plasma yet sufficiently high to
substantially decrease the mean free collision path of the metal
vapor atoms in the vicinity of the shroud. It is to be noted that
the inert gas should not be of such impurity as to cause occluded
impurities in the coating. An inert gas having an oxygen and
moisture content each less than one ppm has been found
satisfactory. In essence, the inert gas leak randomizes the
direction of the metal vapor atoms and thus causes them to impinge
on and coat an area not line-of-sight with respect to the
source.
A number of tests were conducted with various coating materials and
various substrate alloys. In one series of tests, argon and helium
gas was introduced at a pressure of 17 psi through a 0.250 inch
stainless steel line having an inside diameter of 0.190 inches. The
line end was oriented at an angle of approximately 45.degree. and
spaced a distance of 2 to 3 inches with respect to the shroud of a
TF 30 turbine blade. The blade was preheated at 1,750.degree. to
1,825.degree.F by resistively heated filaments of tantalum alloy
(Ta + 10W). When metallographic examinations were made,
corresponding specimens coated with and without the admission of
inert gas showed substantial increases of coating thicknesses on
the shroud. The results of a number of tests are summarized in the
following table.
TABLE I
__________________________________________________________________________
RANDOMIZATION OF VAPOR CLOUD Chamber Pressure Coating Thickness
(Inches) Coating Time Test Specimen Coating* (Torr) Airfoil Shroud
(Min.)
__________________________________________________________________________
1 CoCrAlY 5.0 .times. 10.sup..sup.-5 .00360 0-.000125 16.0 2
CoCrAlY Ar, 7.2 .times. 10.sup..sup.-4 .00325 .00125 18.0 3 CoCrAlY
He, 2.0 .times. 10.sup..sup.-4 .00338 .00063 15.0 4 CoCrAlY He, 6.5
.times. 10.sup..sup.-4 .00375 .00100 13.0 5 CoCrAlY He, 1.5 .times.
10.sup..sup.-3 .00288 .00113 15.0 6 CoCrAlY He, 4.5 .times.
10.sup..sup.-4 .00425 .00175 15.0 7 CoCrAlY He, 1.1 .times.
10.sup..sup.-3 .00450 .00225 15.0
__________________________________________________________________________
*Ingot Material: Air Melt CoCrAlY
It is to be noted in referring to Table I that tests 2 through 7
were run utilizing the inert gas leak of the present invention and
thus should be compared with Test 1 which was run without vapor
cloud randomization. It will also be noted that in Test 7 the outer
shroud surface, which ordinarily receives no coating was coated to
approximately 50 percent of the airfoil coating thickness.
The typical coating procedure has utilized a power setting of the
electron beam gun at 21 kilowatts for the CoCrAlY material and at
15.5 kilowatts for the FeCrAlY coating.
What has been set forth above is intended primarily as exemplary to
enable those skilled in the art in the practice of the invention
and it should therefore be understood that, within the scope of the
appended claims, the invention may be practiced in other ways than
as specifically described.
* * * * *