EP0134474A1 - Process for preparing nickel film - Google Patents
Process for preparing nickel film Download PDFInfo
- Publication number
- EP0134474A1 EP0134474A1 EP84107809A EP84107809A EP0134474A1 EP 0134474 A1 EP0134474 A1 EP 0134474A1 EP 84107809 A EP84107809 A EP 84107809A EP 84107809 A EP84107809 A EP 84107809A EP 0134474 A1 EP0134474 A1 EP 0134474A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- reducing agent
- nickel
- magnetic
- film
- hypophosphite
- 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.)
- Withdrawn
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 23
- 230000005291 magnetic effect Effects 0.000 claims abstract description 16
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052796 boron Inorganic materials 0.000 claims abstract description 8
- 239000011574 phosphorus Substances 0.000 claims abstract description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 150000002816 nickel compounds Chemical class 0.000 claims abstract description 5
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 229910000085 borane Inorganic materials 0.000 claims description 6
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- 239000000696 magnetic material Substances 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical group FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical group [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- -1 amine borane compound Chemical class 0.000 claims 1
- 239000010408 film Substances 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000001464 adherent effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
Definitions
- This invention relates to a process for preparing nickel film.
- it is concerned with a process for preparing a nickel film which has increased stability and is non magnetic.
- Nickel has been prepared by reducing an aqueous solution of a salt.
- Nickel has been prepared by reducing an aqueous solution of a nickel compound with a hypophosphite reducing agent.
- Nickel has also been prepared by reducing an aqueous solution of a nickel compound with an amine borane reducing agent.
- Nickel, produced by either of these processes, has a metastable non-crystalline form, ie it has a tendency to lose its amorphous state and crystallise when heated.
- Crystallisation is associated with three changes in properties which may be harmful. Firstly, the volume generally contracts. This promotes cracking and loss of adhesion. Secondly, precipitation of second phases is harmful in that it increases the susceptibility of the metal to galvanic corrosion. Thirdly, the remaining crystalline metal matrix becomes ferromagnetic.
- the invention seeks to provide a nickel film which retains its non-magnetic, amorphous state when heated to high temperatures.
- US-A-3,567,525 discloses use of a mixture of two reducing agents, one a phosphorus containing agent and one a boron containing agent, for the reduction of nickel.
- the conditions are such, however, that the process produces a material, which is strongly ferrogmagnetic and in powder form.
- a process for preparing a continuous film of nickel is characterised, according to the invention, by reducing an aqueous solution of a nickel compound in the substantial absence of any magnetic material with a mixture of a phosphorus containing reducing agent and a boron containing reducing agent in amounts so that the film retains its amorphous non-magnetic state when heated to a temperature of 300°C.
- the resulting nickel film has a greater stability than that obtained when only a single reducing agent is used.
- the rate of deposition of the nickel film is also increased.
- the film retains its amorphous, non-magnetic state when heated to a high temperature.
- the non-magnetic property is very important and desirable when the nickel is used as an undercoat on a substrate for a thin film magnetic record disk.
- hypophosphite reducing agent and the amine borane reducing agent in a ratio of about 10 equivalents to 1 equivalent.
- the preferred hypophosphite reducing agent is sodium hypophosphite
- the preferred amine borane reducing agent is dimethylamine borane.
- the relative amounts of the phosphorus containing reducing agent and the boron containing reducing agent should be such that the final product is a non-magnetic nickel containing from 10% to 15% by weight phosphorus and from 0.1% to 1% by weight boron. It is only within these critical ranges that the nickel films maintain their low level of stress and their non-magnetic character when heated.
- the present invention yields nickel deposits which are continuous films, and not layers of powder as is obtained in much of the prior art. These continuous films are also adherent to the substrate.
- the object is to form a non-magnetic film
- the reduction should be carried out in the substantial absence of any magnetic materials, ie the process and composition limits would be greatly affected by the presence of more than trace amounts of magnetic materials such as iron, cobalt and manganese.
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
An amorphous, non-magnetic film of nickel is prepared by reducing an aqueous solution of a nickel compound simultaneously with a mixture of a phosphorus containing reducing agent and a boron containing reducing agent. The film is exceptionally stable and retains its amorphous, non-magnetic state when heated to a temperature of 300°C.
Description
- This invention relates to a process for preparing nickel film. In particular, it is concerned with a process for preparing a nickel film which has increased stability and is non magnetic.
- In the past many metals have been prepared by reducing an aqueous solution of a salt. Nickel has been prepared by reducing an aqueous solution of a nickel compound with a hypophosphite reducing agent. Nickel has also been prepared by reducing an aqueous solution of a nickel compound with an amine borane reducing agent. Nickel, produced by either of these processes, has a metastable non-crystalline form, ie it has a tendency to lose its amorphous state and crystallise when heated.
- Crystallisation is associated with three changes in properties which may be harmful. Firstly, the volume generally contracts. This promotes cracking and loss of adhesion. Secondly, precipitation of second phases is harmful in that it increases the susceptibility of the metal to galvanic corrosion. Thirdly, the remaining crystalline metal matrix becomes ferromagnetic.
- The invention seeks to provide a nickel film which retains its non-magnetic, amorphous state when heated to high temperatures.
- US-A-3,567,525 discloses use of a mixture of two reducing agents, one a phosphorus containing agent and one a boron containing agent, for the reduction of nickel. The conditions are such, however, that the process produces a material, which is strongly ferrogmagnetic and in powder form.
- A process for preparing a continuous film of nickel, is characterised, according to the invention, by reducing an aqueous solution of a nickel compound in the substantial absence of any magnetic material with a mixture of a phosphorus containing reducing agent and a boron containing reducing agent in amounts so that the film retains its amorphous non-magnetic state when heated to a temperature of 300°C.
- When a mixture of reducing agents is used according to the present invention, the resulting nickel film has a greater stability than that obtained when only a single reducing agent is used. The rate of deposition of the nickel film is also increased. The film retains its amorphous, non-magnetic state when heated to a high temperature.
- The increased ability of the nickel to withstand high temperature and still be amorphous and non-magnetic greatly increases its usefulness in a wide variety of end uses. For example, the non-magnetic property is very important and desirable when the nickel is used as an undercoat on a substrate for a thin film magnetic record disk.
- In carrying out the process of the present invention, it is advantageous to use the hypophosphite reducing agent and the amine borane reducing agent in a ratio of about 10 equivalents to 1 equivalent. The preferred hypophosphite reducing agent is sodium hypophosphite, and the preferred amine borane reducing agent is dimethylamine borane.
- The relative amounts of the phosphorus containing reducing agent and the boron containing reducing agent should be such that the final product is a non-magnetic nickel containing from 10% to 15% by weight phosphorus and from 0.1% to 1% by weight boron. It is only within these critical ranges that the nickel films maintain their low level of stress and their non-magnetic character when heated.
- It should be emphasised that the present invention yields nickel deposits which are continuous films, and not layers of powder as is obtained in much of the prior art. These continuous films are also adherent to the substrate.
- Since the object is to form a non-magnetic film, the reduction should be carried out in the substantial absence of any magnetic materials, ie the process and composition limits would be greatly affected by the presence of more than trace amounts of magnetic materials such as iron, cobalt and manganese.
- An aqueous solution of nickel sulfate containing 7.0 grams of nickel per litre was prepared. The pH was 4.5. Sodium hypophosphite in an amount of 45 grams per litre and dimethylamine borane in an amount of 2.15 grams per litre were added at a temperature of 91°C. A continuous adherent film of nickel which contained 12% phosphorus and 0.5% boron was precipitated out. This nickel film remains amorphous and non-magnetic when heated to much higher temperatures than those sufficient to crystallise nickel made by a similar process in which only one of the reducing agents is used. Samples prepared according to the present invention can be heated to 300°C and still not become magnetic.
Claims (5)
1. A process for preparing a continuous film of nickel, the process being characterised by reducing an aqueous solution of a nickel compound in the substantial absence of any magnetic material with a mixture of a phosphorus containing reducing agent and a boron containing reducing agent in amounts so that the film retains its amorphous non-magnetic state when heated to a temperature of 300°C.
2. A process as claimed in claim 1, in which the reducing agents are an amine borane compound and a hypophosphite.
3. A process as claimed in claim 2, in which the ratio of hypophosphite reducing agent to amine borane reducing agent is about 10 equivalents to 1 equivalent.
4. A process as claimed in claim 2 or claim 3, in which the hypophosphite reducing agent is sodium hypophosphite and the amine borane reducing agent is dimethylamine borane.
5. An amorphous, non-magnetic nickel film containing from 10% to 15% by weight phosphorus and from 0.1% to 1% by weight boron when prepared by a process as claimed in any preceding claim.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US52803083A | 1983-08-31 | 1983-08-31 | |
| US528030 | 1983-08-31 | ||
| US58456184A | 1984-02-28 | 1984-02-28 | |
| US584561 | 1984-02-28 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP0134474A1 true EP0134474A1 (en) | 1985-03-20 |
Family
ID=27062593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP84107809A Withdrawn EP0134474A1 (en) | 1983-08-31 | 1984-07-05 | Process for preparing nickel film |
Country Status (1)
| Country | Link |
|---|---|
| EP (1) | EP0134474A1 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2028950A1 (en) * | 1970-06-12 | 1971-12-16 | Shipley Co | Aqueous solution for the electroless deposition of nickel or cobalt |
| US4152164A (en) * | 1976-04-26 | 1979-05-01 | Michael Gulla | Electroless nickel plating |
| SU681111A2 (en) * | 1976-03-01 | 1979-08-25 | Ордена Трудового Красного Знамени Институт Химии И Химической Технологии Ан Литовской Сср | Solution for chemical nickel plating |
| JPS57120664A (en) * | 1981-01-19 | 1982-07-27 | Matsushita Electric Ind Co Ltd | Formation of nickel film |
-
1984
- 1984-07-05 EP EP84107809A patent/EP0134474A1/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2028950A1 (en) * | 1970-06-12 | 1971-12-16 | Shipley Co | Aqueous solution for the electroless deposition of nickel or cobalt |
| SU681111A2 (en) * | 1976-03-01 | 1979-08-25 | Ордена Трудового Красного Знамени Институт Химии И Химической Технологии Ан Литовской Сср | Solution for chemical nickel plating |
| US4152164A (en) * | 1976-04-26 | 1979-05-01 | Michael Gulla | Electroless nickel plating |
| JPS57120664A (en) * | 1981-01-19 | 1982-07-27 | Matsushita Electric Ind Co Ltd | Formation of nickel film |
Non-Patent Citations (2)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN, unexamined applications, field C, vol. 6, no. 214, october 27, 1982 THE PATENT OFFICE JAPANESE GOVERNMENT page 164 (C-131); & JP-A-57 120 664 (MATSUSHITA DENKI SANGYO K.K.) * |
| SOVIET INVENTIONS ILLUSTRATED, section Ch, week C 17, June 4, 1980 DERWENT PUBLICATIONS LTD., London M 13; & SU-A-681111 (AS LITH CHEM TECHN) * |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| AK | Designated contracting states |
Designated state(s): DE FR GB |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 19851121 |
|
| RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: PHIPPS, PETER BEVERLY POWELL Inventor name: DOSS, SAAD KAMEL |