U.S. patent number 3,635,801 [Application Number 04/804,593] was granted by the patent office on 1972-01-18 for nickel electrodeposition process for improving high-temperature ductility.
This patent grant is currently assigned to The United States of America as represented by the Secretary of the Navy. Invention is credited to Charles A. Bruch.
United States Patent |
3,635,801 |
Bruch |
January 18, 1972 |
NICKEL ELECTRODEPOSITION PROCESS FOR IMPROVING HIGH-TEMPERATURE
DUCTILITY
Abstract
A process of electroplating nickel using an electrolyte
containing a sulfte. The process is conducted at a temperature of
27.degree. C. or lower. The electrolyte may be used in either an
acid or an alkaline bath.
Inventors: |
Bruch; Charles A. (Cincinnati,
OH) |
Assignee: |
The United States of America as
represented by the Secretary of the Navy (N/A)
|
Family
ID: |
25189358 |
Appl.
No.: |
04/804,593 |
Filed: |
March 5, 1969 |
Current U.S.
Class: |
205/273;
204/192.1; 205/213; 205/170 |
Current CPC
Class: |
C25D
5/003 (20130101); C25D 5/00 (20130101); C25D
3/12 (20130101) |
Current International
Class: |
C25D
5/00 (20060101); C23b 005/08 () |
Field of
Search: |
;204/38B,38R,192,49 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Garvin; Patrick P.
Claims
What is claimed is:
1. In the process of electrodepositing nickel using an electrolyte
containing a sulfamate, the improvement which comprises conducting
said electroplating at a temperature no higher than 27.degree. C.
Description
STATEMENT OF GOVERNMENT INTEREST
The invention defined herein may be manufactured and used by or for
the Government of the United States of America for governmental
purposes without the payment of any royalties thereon or
therefor.
CROSS-REFERENCE TO RELATED APPLICATIONS
The process described in this application is closely related to an
application Ser. No. 829,215 now U.S. Pat. No. 3,582,480, filed
June 2, 1969 for Heat Treating Process for Improving High
Temperature Ductility of Electrodeposited Nickel and Nickel Alloys
in the name of Juan Chorne.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to the field of electroplating and, more
particularly, to the electrodeposition of nickel at low
temperatures.
2. Description of the Prior Art
A process known as the Barrett Sulfamate Nickel-Plating Bath and
described in U.S. Pat. No. 2,318,592 to Martin E. Cunery is used to
deposit nickel or nickel alloy. It consists of an electrolyte
containing a sulfamate, which may be used in either an acid or an
alkaline bath. An example bath would be made of sulfamic acid and
nickel carbonate. It has been found that when the finished product
is heated to temperatures above 450.degree. C. a severe
embrittlement occurs. This embrittlement is a serious defect. The
cause of this embrittlement is hydrogen which is deposited with the
nickel. U.S. Pat. No. 2,534,911 recognizes this problem and
attempts to remedy it.
SUMMARY OF THE INVENTION
The invention using a well-known process and altering the steps of
this process is eliminating the embrittlement found in present
whisker-reinforced composites at high temperatures and has
increased the specific strength (strength-to-density) ratio.
The object of the invention is to change the present process of
preparing whisker-reinforced composites by controlling the
temperature to develop whisker-reinforced composites having high
strength-to-weight ratios at elevated temperatures.
It is another object of the present invention to present a process
similar to that of the known Barrett Sulfamate process but by
carrying out the new process at low temperatures to produce a
product that will be free of embrittlement when used at high
temperatures.
It is a further object of this invention to provide a process for
the electrodeposition of nickel so that the finished product will
be ductile at high temperatures as well as normal working
temperatures.
It is a further object of the present invention to provide a
process for the electrodeposition of nickel, the process to be
carried out at low temperatures to prevent the codeposition of
hydrogen along with the nickel.
It is a still further object of the present invention to provide a
process for the deposition of nickel at which the process is
carried out at temperatures lower than 27.degree. C.
Other objects, advantages and novel features of the present
invention will become apparent from the following detailed
description of the invention when considered in conjunction with
the accompanying drawing.
DESCRIPTION OF THE DRAWING
FIG. 1 is a graph showing minimum percent elongation in room
temperature with relation to current density; and
FIG. 2 is a graph showing minimum percent elongation at room
temperature relative to plating both temperature.
DESCRIPTION OF PREFERRED EMBODIMENTS
It is expected to achieve a specific strength of 600,000
(strength-to-density ratio) inches at 2,000.degree. F. in a
conventional tensile test. The development of a technique for
preparing whisker reinforced high-temperature metals, such as
nickel or nickel alloys which reproducibly exhibit strength greater
than 200,000 inches at 1,800.degree. F. The feasibility of
reinforcing metals with high strength whiskers was demonstrated
previously using what may be considered a model system of A1.sub.2
O.sub.3 whiskers in a silver matrix. Composites prepared by
infiltering the A1.sub.2 O.sub.3 whiskers with molten silver
exhibited strength-to-density values as high as 725,000 inches at
room temperature with 24 volume percent whiskers and 320,000 inches
at 1,600.degree. F. with 45 volume percent whiskers.
Later a more refractory matrix metal was selected in order to meet
the elevated temperature criteria. The matrix selected was nickel,
since it is the base for many of the high temperature, oxidation
resistant alloys. It was found that molten nickel dissolved all
metallic coatings applied to the whiskers resulting in dewetting,
poor penetration and poor bonding. Several potential methods for
fabricating nickel and nickel alloy matrix composites were explored
and on the basis of these studies, it was concluded that the
achievement of higher strength-to-density ratios at temperatures
close to 2,000.degree. F. are feasible since small composites
prepared by an electroforming technique exhibited specific strength
values as high as 320,000 at 1,850.degree. F. However, these high
strength values could not be achieved in larger electroformed
specimens due to incomplete penetration of the whisker bundle of
the electroplated nickel. Voids and other matrix irregularities
resulted which greatly reduced the effective cohesive strength of
the matrix and limited the transfer of stresses to the fibers at
elevated temperatures. To heal these various matrix defects
incurred during electroplating, an additional step, pressure
bonding, was introduced.
Referring to FIG. 1 the minimum percent elongation in room
temperature is shown relative to changes in current density
expressed in amperes per square foot. Results are shown for a
plating temperature of 58.degree. C., 41.degree. C. and 27.degree.
C.
FIG. 2 illustrates the improvement in ductility with reduction of
the plating bath temperature. While actual tests have not been
conducted, as yet, below a 27.degree. C. temperature, calculations
indicate the curve will follow the course shown in dashed
lines.
With the electroplating pressure bonding process the results were
marred by the embrittlement of the electroplated nickel matrix
during exposures to the high temperatures used in the bonding
process. The nature of the matrix embrittlement was concluded to be
caused by a deposition of hydrogen along with the nickel during the
electroplating process. The steps taken to avoid this embrittlement
form the basis for the invention.
The making of high-strength composites by incorporating A1.sub.2
O.sub.3 whiskers in a nickel matrix employs an electroplating
process followed by pressure bonding.
The following steps are the basic steps in this process:
1. The A1.sub.2 O.sub.3 whiskers are first given a thin metallic
coating by a cathodic sputtering process using a variety of metals
including W, Ti, Mo and others.
2. The coated whiskers are formed into an oriented mat.
3. The coated whisker mats are then given an additional coating of
nickel by an electroplating process carried out at a temperature
not exceeding 27.degree. C. and with a critical electric current
density which is increased with a decrease in temperature to form a
"prepreg" which is partially consolidated.
4. The "prepregs" are placed in a suitable die and heated to
elevated temperatures in the range of 1,000.degree. to
1,400.degree. C. and then pressed in the die for final
consolidation.
5. The resulting composites are tested in the temperature range
ultimately intended for their use, 900.degree. to 1,100.degree. C.
A "prepeg," as noted above, is an art term meaning preimpregnated
and refers in this instance to the composite, whisker and nickel
coating previous to the bonding step.
The electroplating of nickel without the addition of the whisker
produces like results with regard to embrittlement.
While this is a comparatively small change, the results are that
the ductility of the composite is greatly improved, the
embrittlement of the nickel is almost eliminated and a useful
composite is produced.
Obviously many modifications and variations of the present
invention are possible in the light of the above teachings.
* * * * *