CA1066652A - Electroforming nickel iron alloys - Google Patents
Electroforming nickel iron alloysInfo
- Publication number
- CA1066652A CA1066652A CA248,165A CA248165A CA1066652A CA 1066652 A CA1066652 A CA 1066652A CA 248165 A CA248165 A CA 248165A CA 1066652 A CA1066652 A CA 1066652A
- Authority
- CA
- Canada
- Prior art keywords
- nickel
- alloy
- iron
- electrolyte
- article
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
A process is disclosed for the electrodeposition of nickel iron alloy products in which the composition of the alloy ranges from 40% to 50% nickel with the balance iron and the product is in mesh form ranging from 0 to 1,500 lines per inch with the process comprising the use of sulfate baths, an alloy anode, and control of the pH, the temperature and current density during the plating cycle.
A process is disclosed for the electrodeposition of nickel iron alloy products in which the composition of the alloy ranges from 40% to 50% nickel with the balance iron and the product is in mesh form ranging from 0 to 1,500 lines per inch with the process comprising the use of sulfate baths, an alloy anode, and control of the pH, the temperature and current density during the plating cycle.
Description
~066652 Background of the Invention Field of the Invention. This invention relates generally to electrodeposition and, more specifically, to ~- -electrodeposition or electroforming of nickel iron alloys having a composition ranging from about 40% to 50% nickel with the balance iron. The concept of electroforming or electrodeposition of alloys and more specifically, electro-deposition of nickel iron alloys is old and well known in the art. However, the electrodeposition of nickel iron alloys has been fraught with difficulties as evidenced by numerous patents and numerous articles related to the electrodeposition of nickel iron alloys. For example, an article by E. M. Levy in the August, 1969 issue of "Plating"
titled "Nickel-Iron alloys Electrodeposited from a Sulfate-Chloride Electrolyte" suggests that a typical plating bath for forming a nickel iron alloy should contain a sulfate-chloride electrolyte in addition to a stress reducing agent such as the sodium salt of 1, 3, 6 - napthalenetrisulfonic acid. The composition of the electrolyte solution suggested by Levy was as follows: NiS04 6H2O, 32 grams per liter;
NiC12 6H20, 20 grams per liter; FeSo4 7H20, 18 grams per liter; H3B03, 30 grams per liter.
Another prior art teaching is found in the Barrett patent 3,817,843 which teaches electrodeposition of iron foil alloys but which states that, while it is possible to produce foil by electrodeposition with an electrolyte temp-erature below 92 C., it is not likely to be of commercial interest because of the low current density. In addition, Barrett suggests a pH of the electrolyte between .3 and l.4.
The Angel patent 2,622,063 teaches the electrode-position of iron alloyed with other materials such as manganese, molybdenum and tungsten by using anodes of nickel, : ~ :
~(~666~'Z
iron or nickel iron and adding other metals in the form of oxides so as to produce an iron alloy of desired properties.
The Donroe patent 2,418,970 teaches the electro- -deposition of iron and nickel iron alloys that are smooth and free of pitting by the addition of zinc hyposulfite to the electrolyte.
The Russell patent 1,906,029 shows how to make an alloy of 79% nickel and the balance iron with the use - -of an electrolyte that contains magnesium salt.
The Burns patent 1,837,355 teaches the making of an alloy approximately 79% nickel and the balance iron by the use of two anodes, a first anode of nickel and a second anode of iron.
At the other end of the alloy composition, the Crowder patent 2,131,427 teaches the electrodeposition of an alloy which does not exceed 5% nickel. Crowder electro-deposits his article by electrodepositing through a heated solution of iron and nickel salts of ferrous sulfate and nickel sulfate in which the solution also contains hydro-~ fluorlc acld and sodlum floride.
From a review of some of the prior art patents and literature, it is apparent that there have been many methods and compositions which have been employed to electrodeposit ` nickel iron alloys. However, no clear teaching has emerged as to how to deposit an alloy of a specific composition as what may work well for electrodeposition of an alloy of a particular composition may be exactly wrong for electro-deposition of an alloy of a different composition. With ; 30 this uncertainty of prior art information, the applicant now discloses a process for produc~ng-an alloy having the .~: range of 40% to 50% nickel with the balance iron. The alloy is in foil form and may have 0 to as high as 1,500 lines inch.-- :
- - , ~
- ., ~06665Z
- Brief Summary of the Invention Briefly, the process of the present invention teaches the electrodeposition of a nickel iron alloy by using a sulfate bath prepared from nickel sulfate and ferrous sulfate, use of an alloy anode which is about 40% nickel with balance iron, control of the electrolyte temperature and pH within certain ranges, and use of a constant voltage power source.
According to the broadest aspect of the invention there is provided a method of electrodeposition of a nickel iron foil wherein the alloy has a final composition ranging from about 40% to sa~ nickel with the balance iron comprising the steps:
a. preparing an electrolyte bath compr~sed of nickel sulfate and ferrous sulfate;
b. placing an alloy anode comprised of nickel and iron in said electrolyte bath;
c. maintaining the pH of said electrolyte bath at about
titled "Nickel-Iron alloys Electrodeposited from a Sulfate-Chloride Electrolyte" suggests that a typical plating bath for forming a nickel iron alloy should contain a sulfate-chloride electrolyte in addition to a stress reducing agent such as the sodium salt of 1, 3, 6 - napthalenetrisulfonic acid. The composition of the electrolyte solution suggested by Levy was as follows: NiS04 6H2O, 32 grams per liter;
NiC12 6H20, 20 grams per liter; FeSo4 7H20, 18 grams per liter; H3B03, 30 grams per liter.
Another prior art teaching is found in the Barrett patent 3,817,843 which teaches electrodeposition of iron foil alloys but which states that, while it is possible to produce foil by electrodeposition with an electrolyte temp-erature below 92 C., it is not likely to be of commercial interest because of the low current density. In addition, Barrett suggests a pH of the electrolyte between .3 and l.4.
The Angel patent 2,622,063 teaches the electrode-position of iron alloyed with other materials such as manganese, molybdenum and tungsten by using anodes of nickel, : ~ :
~(~666~'Z
iron or nickel iron and adding other metals in the form of oxides so as to produce an iron alloy of desired properties.
The Donroe patent 2,418,970 teaches the electro- -deposition of iron and nickel iron alloys that are smooth and free of pitting by the addition of zinc hyposulfite to the electrolyte.
The Russell patent 1,906,029 shows how to make an alloy of 79% nickel and the balance iron with the use - -of an electrolyte that contains magnesium salt.
The Burns patent 1,837,355 teaches the making of an alloy approximately 79% nickel and the balance iron by the use of two anodes, a first anode of nickel and a second anode of iron.
At the other end of the alloy composition, the Crowder patent 2,131,427 teaches the electrodeposition of an alloy which does not exceed 5% nickel. Crowder electro-deposits his article by electrodepositing through a heated solution of iron and nickel salts of ferrous sulfate and nickel sulfate in which the solution also contains hydro-~ fluorlc acld and sodlum floride.
From a review of some of the prior art patents and literature, it is apparent that there have been many methods and compositions which have been employed to electrodeposit ` nickel iron alloys. However, no clear teaching has emerged as to how to deposit an alloy of a specific composition as what may work well for electrodeposition of an alloy of a particular composition may be exactly wrong for electro-deposition of an alloy of a different composition. With ; 30 this uncertainty of prior art information, the applicant now discloses a process for produc~ng-an alloy having the .~: range of 40% to 50% nickel with the balance iron. The alloy is in foil form and may have 0 to as high as 1,500 lines inch.-- :
- - , ~
- ., ~06665Z
- Brief Summary of the Invention Briefly, the process of the present invention teaches the electrodeposition of a nickel iron alloy by using a sulfate bath prepared from nickel sulfate and ferrous sulfate, use of an alloy anode which is about 40% nickel with balance iron, control of the electrolyte temperature and pH within certain ranges, and use of a constant voltage power source.
According to the broadest aspect of the invention there is provided a method of electrodeposition of a nickel iron foil wherein the alloy has a final composition ranging from about 40% to sa~ nickel with the balance iron comprising the steps:
a. preparing an electrolyte bath compr~sed of nickel sulfate and ferrous sulfate;
b. placing an alloy anode comprised of nickel and iron in said electrolyte bath;
c. maintaining the pH of said electrolyte bath at about
2.3;
d. maintaining the ratio of nickel sulfate to ferrous sulfate about 1 to 1;
e. adding a wetting agent to the electrolyte bath to reduce the surface tension to less than forty dyne-centimeters;
f. placing an article to be plated in said electrolyte then applying a source of power to provide a constant current density to tAe article being electrodeposited. ~ -Description of the-Preferred Embodiment In order to electrodeposit an alloy having 40% to 50%
nickel with the balance iron, a sulfate bath was prepared from nickel sulfate NiS04 6H20 and ferrous sulfate FeS04 7H20 and water with the ratio of nickel to iron in the electrolyte , .
1 -4- ~
~', .: . : .. . . . . ..
,. : - , -~ 1066652 bath being about 1 and the amount of each of the nickel and --the iron in the bath being about 30 grams per liter. To this electrolyte bath, a wetting agent was added to reduce the surface tension of the liquid electrolyte. Any number of suitable wetting agents including alcohols or soaps, can be used; however, in the present process, it is preferred to use FC-170 wetting agent (trade name of 3M Co.). Generally, sufficient wetting agent to reduce the surface tension below ; approximately forty dyne-centimeters is preferred.
m e article was cleaned for electroforming by first - rinsing in hot tap water for 15 minutes. The article was then soaked in a cleaning solution; the article was rinsed again ~-and finally, the article was soaked in distilled water. The article was then immersed into the electrolyte bath and shaken to remove any hydrogen gas or air bubbles which may have formed -on the surface of the article. An alloy anode which comprises about 40% nickel with the balance iron was placed in a woven polypropylene bag and suKpended in thc .
.. ! 'i -4a-'. .
,, . ,: . .. , : . - , .. . . .
i ~066652 electrolyte bath. Plating was begun by applying a voltage across the cathode article and the alloy anode. The use of the woven polypropylene bag prevents any scaling or flakes from the anode from eroding into the electrolyte by prevent-ing those particles from passing through the woven sides of the bag. The electrolyte bath temperature was about 80 C.
and the pH of the solution was about 2.3.
The electroforming is carried out using a constant voltage source, either a continuous dc or pulse power supply. Generally, the electroformed alloy composition is dependant upon the current density and temperature during plating. As the current density increases, the percent composition of nickel decreases and increasing the temper-ature causes an increase in the percent composition of nickel. By using a constant current device to electroform an article whose surface area continuously increases, such ;; as electroformed mesh on a conductive grid, the current density would continuously decrease, thereby resulting in ~
an alloy whose composition varied with time. The applicants ;
have avoided this variation of composition with time by using a constant voltage source. This allows the current density to be maintained at a constant level thus virtually elim-inating the variation of the alloy composition with time.
In order to obtain the alloy of 40% to 50% nickel with the balance iron, it has been found that certain conditions should be maintained. First, the article must be cleaned so that there is a clean base to electroform on.
Second, the ratio of nickel and iron in the sulfate bath should be about 1 to 1 and the anode should be an alloy of iron and nickel. An alloy of about 40% nickel with the balance iron is preferable. However, other nickel iron alloys are also suitable. By controlling the operating -,. : . .: , :
. . .
. . . . . . . . ..
1~6665Z
conditions such as temperature, pH, and current, one canconsistently produce an alloy having 40% to 50% nickel with the balance iron. If the pH of the electrolyte solution is maintained at about 2.3 and the temperature of this electrolyte solution is at least 80 CO~ consistent results can be obtained. The present process can be used to electroform either foil or fine alloy mesh. If alloy mesh is electroplated, the electroforming is performed on a conductive grid.
`' :' ', ,, ..
.'~' '
d. maintaining the ratio of nickel sulfate to ferrous sulfate about 1 to 1;
e. adding a wetting agent to the electrolyte bath to reduce the surface tension to less than forty dyne-centimeters;
f. placing an article to be plated in said electrolyte then applying a source of power to provide a constant current density to tAe article being electrodeposited. ~ -Description of the-Preferred Embodiment In order to electrodeposit an alloy having 40% to 50%
nickel with the balance iron, a sulfate bath was prepared from nickel sulfate NiS04 6H20 and ferrous sulfate FeS04 7H20 and water with the ratio of nickel to iron in the electrolyte , .
1 -4- ~
~', .: . : .. . . . . ..
,. : - , -~ 1066652 bath being about 1 and the amount of each of the nickel and --the iron in the bath being about 30 grams per liter. To this electrolyte bath, a wetting agent was added to reduce the surface tension of the liquid electrolyte. Any number of suitable wetting agents including alcohols or soaps, can be used; however, in the present process, it is preferred to use FC-170 wetting agent (trade name of 3M Co.). Generally, sufficient wetting agent to reduce the surface tension below ; approximately forty dyne-centimeters is preferred.
m e article was cleaned for electroforming by first - rinsing in hot tap water for 15 minutes. The article was then soaked in a cleaning solution; the article was rinsed again ~-and finally, the article was soaked in distilled water. The article was then immersed into the electrolyte bath and shaken to remove any hydrogen gas or air bubbles which may have formed -on the surface of the article. An alloy anode which comprises about 40% nickel with the balance iron was placed in a woven polypropylene bag and suKpended in thc .
.. ! 'i -4a-'. .
,, . ,: . .. , : . - , .. . . .
i ~066652 electrolyte bath. Plating was begun by applying a voltage across the cathode article and the alloy anode. The use of the woven polypropylene bag prevents any scaling or flakes from the anode from eroding into the electrolyte by prevent-ing those particles from passing through the woven sides of the bag. The electrolyte bath temperature was about 80 C.
and the pH of the solution was about 2.3.
The electroforming is carried out using a constant voltage source, either a continuous dc or pulse power supply. Generally, the electroformed alloy composition is dependant upon the current density and temperature during plating. As the current density increases, the percent composition of nickel decreases and increasing the temper-ature causes an increase in the percent composition of nickel. By using a constant current device to electroform an article whose surface area continuously increases, such ;; as electroformed mesh on a conductive grid, the current density would continuously decrease, thereby resulting in ~
an alloy whose composition varied with time. The applicants ;
have avoided this variation of composition with time by using a constant voltage source. This allows the current density to be maintained at a constant level thus virtually elim-inating the variation of the alloy composition with time.
In order to obtain the alloy of 40% to 50% nickel with the balance iron, it has been found that certain conditions should be maintained. First, the article must be cleaned so that there is a clean base to electroform on.
Second, the ratio of nickel and iron in the sulfate bath should be about 1 to 1 and the anode should be an alloy of iron and nickel. An alloy of about 40% nickel with the balance iron is preferable. However, other nickel iron alloys are also suitable. By controlling the operating -,. : . .: , :
. . .
. . . . . . . . ..
1~6665Z
conditions such as temperature, pH, and current, one canconsistently produce an alloy having 40% to 50% nickel with the balance iron. If the pH of the electrolyte solution is maintained at about 2.3 and the temperature of this electrolyte solution is at least 80 CO~ consistent results can be obtained. The present process can be used to electroform either foil or fine alloy mesh. If alloy mesh is electroplated, the electroforming is performed on a conductive grid.
`' :' ', ,, ..
.'~' '
Claims (5)
1. A method of electrodeposition of a nickel iron foil wherein the alloy has a final composition ranging from about 40% to 50% nickel with the balance iron comprising the steps:
a. preparing an electrolyte bath comprised of nickel sulfate and ferrous sulfate;
b. placing an alloy anode comprised of nickel and iron in said electrolyte bath;
c. maintaining the pH of said electrolyte bath at about 2.3;
d. maintaining the ratio of nickel sulfate to ferrous sulfate about 1 to 1;
e. adding a wetting agent to the eletrolyte bath to reduce the surface tension to less than forty dyne-centimeters;
f. placing an article to be plated in said electrolyte then applying a source of power to pro-vide a constant current density to the article being electrodeposited.
a. preparing an electrolyte bath comprised of nickel sulfate and ferrous sulfate;
b. placing an alloy anode comprised of nickel and iron in said electrolyte bath;
c. maintaining the pH of said electrolyte bath at about 2.3;
d. maintaining the ratio of nickel sulfate to ferrous sulfate about 1 to 1;
e. adding a wetting agent to the eletrolyte bath to reduce the surface tension to less than forty dyne-centimeters;
f. placing an article to be plated in said electrolyte then applying a source of power to pro-vide a constant current density to the article being electrodeposited.
2. The invention of claim 1, wherein the source of power across said article and said cathode is a constant voltage signal to perform the electrodeposition of a nickel iron alloy.
3. The method of claim 1 wherein said alloy anode is suspended in a porous container to prevent large particles of the alloy anode from entering the electrolyte.
4. The method of claim 1 wherein said alloy anode has approximately 40% nickel with the balance iron.
5. The method of claim 2 wherein said source of constant voltage comprises a pulse direct current signal.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US60326675A | 1975-08-11 | 1975-08-11 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1066652A true CA1066652A (en) | 1979-11-20 |
Family
ID=24414705
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA248,165A Expired CA1066652A (en) | 1975-08-11 | 1976-03-18 | Electroforming nickel iron alloys |
Country Status (8)
| Country | Link |
|---|---|
| JP (1) | JPS5221227A (en) |
| BE (1) | BE842077A (en) |
| CA (1) | CA1066652A (en) |
| DE (1) | DE2616164A1 (en) |
| FR (1) | FR2320997A1 (en) |
| GB (1) | GB1528526A (en) |
| IT (1) | IT1061049B (en) |
| NL (1) | NL7603421A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0599215A (en) * | 1992-02-26 | 1993-04-20 | Koyo Fastener Kk | Assembling method for rivet |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3141837A (en) * | 1961-11-28 | 1964-07-21 | Rca Corp | Method for electrodepositing nickel-iron alloys |
| FR1397417A (en) * | 1964-03-09 | 1965-04-30 | Ibm France | New improvements to the electrolytic deposition of a magnetic layer |
| FR2202953A1 (en) * | 1973-01-20 | 1974-05-10 | Ibm | Electrodeposition of nickel-iron alloys - for use in transducers, plating soln. contains thiocyanate ions to increase nickel-iron ratio |
-
1976
- 1976-03-18 CA CA248,165A patent/CA1066652A/en not_active Expired
- 1976-04-01 NL NL7603421A patent/NL7603421A/en not_active Application Discontinuation
- 1976-04-13 DE DE19762616164 patent/DE2616164A1/en not_active Withdrawn
- 1976-04-22 FR FR7611901A patent/FR2320997A1/en active Granted
- 1976-05-17 IT IT2333976A patent/IT1061049B/en active
- 1976-05-21 BE BE167214A patent/BE842077A/en unknown
- 1976-06-05 JP JP6601876A patent/JPS5221227A/en active Pending
- 1976-06-09 GB GB2379476A patent/GB1528526A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| DE2616164A1 (en) | 1977-03-03 |
| FR2320997B1 (en) | 1979-02-02 |
| BE842077A (en) | 1976-09-16 |
| NL7603421A (en) | 1977-02-15 |
| FR2320997A1 (en) | 1977-03-11 |
| IT1061049B (en) | 1982-10-20 |
| JPS5221227A (en) | 1977-02-17 |
| GB1528526A (en) | 1978-10-11 |
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