US3119753A - Method of preparing thin magnetic films - Google Patents
Method of preparing thin magnetic films Download PDFInfo
- Publication number
- US3119753A US3119753A US60735A US6073560A US3119753A US 3119753 A US3119753 A US 3119753A US 60735 A US60735 A US 60735A US 6073560 A US6073560 A US 6073560A US 3119753 A US3119753 A US 3119753A
- Authority
- US
- United States
- Prior art keywords
- films
- plating
- hypophosphite
- nickel
- iron
- 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 - Lifetime
Links
- 238000000034 method Methods 0.000 title claims description 20
- 230000005291 magnetic effect Effects 0.000 title description 10
- 238000007747 plating Methods 0.000 claims description 24
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 6
- 238000009713 electroplating Methods 0.000 claims description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 159000000014 iron salts Chemical class 0.000 claims description 3
- 239000010408 film Substances 0.000 description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 229910052759 nickel Inorganic materials 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 3
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- 239000011790 ferrous sulphate Substances 0.000 description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- -1 alkali metal hypophosphites Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002739 metals 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
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 1
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/65—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition
- G11B5/653—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent characterised by its composition containing Fe or Ni
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/14—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/24—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates from liquids
- H01F41/26—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates from liquids using electric currents, e.g. electroplating
Definitions
- Thin ferromagnetic films of nickel-iron alloys are used extensively for computer information storage and in switching applications. in use, it is desirable that the films have relatively square hysteresis loops and low coercive forces.
- Various methods have been used, such as vacuum deposition of vapors of the metals and the like. It has also been proposed to prepare the thin films by electrodeposition from suitable plating solutions. The latter method has advantages, but the films produced often leave something to be desired in their properties.
- the present invention constitutes an improved electroplating method for the formation of thin nickel-iron films.
- the most important characteristic of the present invention is the presence of the small amount of a hypophosphite. This permits a very precise control and results in films of lower coercivity, H and B and in the hard direction the hysteresis loop opens up to a much lower degree as will be shown in the drawings. An even more important property is switching time.
- the films of the present invention have much lower switching times under the same operating conditions than do films of the same character prepared without hypophosphite.
- the range of hypophosphite in grams per liter is from about 0.95 to 0.4. Optimum results are obtained with hypophosphite concentrations from 0.08 to 023 g./l.
- the pH should be maintained in the range from 1.7 to 2.8, poorer results being obtained when the pH is outside of this range. Within the range of pHs, BH properties are excellent and are uniformly reproducible.
- Film thickness while not as critical as hypophosphite content and pH, is, nevertheless, of importance. Good results are obtained with thicknesses from 800 to 1600' A.
- hypophosphite is not especially critical so long as it is not a platable metal.
- sodium hypophosphite is preferred although, of course, the same results can be obtained with other alkali metal hypophosphites, such as potassium hypophosphite.
- alkali metal hypophosphites such as potassium hypophosphite.
- the plating procedure is otherwise normal, and does not present any particular problems.
- the temperature is not especially critical, and room temperature may be used. There is no appreciable difference between the BH properties of films plated at room temperature and those plated at higher plating temperatures, for example in the range of 50 to 52 C. The relative insensitivity to small temperature changes makes control of the process of the present invention simple and is a desirable practical operating characteristic.
- the nature of the substrate does not differ significantly from general plating practice by other methods.
- a smooth conducting surface is desirable which, for example, can either be polished metal or glass metallized so that it has the necessary conductivity for electroplating.
- the latter type of substrate has some advantages and will be described in connection with specific examples, though, of course, the invention is not in any sense limited to the particular type of substrate used.
- the proportions of nickel and iron in the final film can be varied over wide ranges by control of the various proportions of nickel and iron salts in the plating bath. Optimum results are obtained when the proportion of iron to nickel in the bath is between 1.5 to 98.5 to 3 to 97. This results in percentages of iron in the film from slightly below 14 to about 23%. It is an advantage of the present invention that the films produced have excellent properties over a considerable range of iron to nickel proportions so that in this respect no extremely critical control of plating bath composition is necessary.
- FIG. 1 is a series of curves of reciprocal switching times for two different films
- FIG. 2 is a pair of BH loops for a film prepared with hypophosphite
- FIG. 3 is a similar pair for a film prepared without phosphite.
- Substrates were made from circular pieces of glass 9 mm. in diameter plated first with a film about a A. of chromium followed by 100 A. film of gold. Coating was by vacuum vapor deposition. The substrates were then plated in the bath in the conventional manner at room temperature using 4 to 6 volts and maintaining the current density at 6 ma./cm. pH of the various baths was varied from 1.5 to 3.4. Time of plating varied from approximately 60 seconds to about 2 minutes in order to produce films from 800 to 1600 A.
- FIG. 1 shows curves of reciprocal switching times vs. drive for two films prepared as above, one with .3 g./l. hypophosphite and one without. It will be seen that the curves of the film prepared with the hypophosphite are much steeper than those of the other film. This permits faster switching times under any given set of drive conditions. This is of great importance in practical applications in computers and constitutes the most important advantage of films prepared by the process of the present invention.
- FIGS. 2 and 3 illustrate hysteresis loops of the two films described above. It will be noted that in FIG. 2, which illustrates films prepared by the present invention, the loops are squarer and in the hard direction there is little or no opening of the loop. There is also a much lower coercive force shown in FIG. 2 which will be expressed in figures in following examples.
- EXAMPLE 2 Plating was effected under conditions described in Example 1 in a series of baths having 0.3 g./l. of hypophosphite and varied amounts of ferrous sulfate. The following tabulation gives the composition of the films with change in ferrous sulfate concentration.
- EXAMPLE 3 A series of platings were made with fixed thickness, current density, bath composition and hypophosphite content. The pHs varied from 1.5 to 3.4. The composition of the bath, film thickness and resulting film properties are as follows:
- EXAMPLE 4 A series of platings was efiected with different amounts of sodium hypophosphite. The plating data and characteristics were as follows:
- hypophosphite markedly reduces coercivity and improves other characteristics.
- the nickel-iron composition ranges from between about 77% and 86% nickel, balance iron
- the method comprises plating on a conducting substrate from a plating bath comprising nickel and iron salts, the improvement comprising adding from 0.05 to 0.4 g./l. of an alkali metal hypophosphite to the bath and maintaining the pH of the plating bath below 3.
- alkali metal hypophosphite concentration is from 0.08 to 0.3 g./l. of hypophosphite.
- a solution for use in electroplating nickel-iron magnetic films comprising approximately 218 g./l. of nickel sulfate, approximately 3.6-6.0 g./l. of ferrous sulfate and approximately 0.4 g./l. of sodium hypophosphite.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Chemically Coating (AREA)
- Thin Magnetic Films (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Electroplating Methods And Accessories (AREA)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NL269912D NL269912A (de) | 1960-10-05 | ||
US60735A US3119753A (en) | 1960-10-05 | 1960-10-05 | Method of preparing thin magnetic films |
GB34704/61A GB950342A (en) | 1960-10-05 | 1961-09-27 | Method of preparing thin magnetic films |
DES76109A DE1147817B (de) | 1960-10-05 | 1961-09-30 | Verfahren zum galvanischen Abscheiden eines Nickel-Eisen-UEberzuges |
CH1154261A CH425393A (it) | 1960-10-05 | 1961-10-04 | Procedimento per la preparazione di pellicole magnetiche sottili |
FR875096A FR1302747A (fr) | 1960-10-05 | 1961-10-05 | Procédé de préparation de pellicules magnétiques minces |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US60735A US3119753A (en) | 1960-10-05 | 1960-10-05 | Method of preparing thin magnetic films |
Publications (1)
Publication Number | Publication Date |
---|---|
US3119753A true US3119753A (en) | 1964-01-28 |
Family
ID=22031429
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US60735A Expired - Lifetime US3119753A (en) | 1960-10-05 | 1960-10-05 | Method of preparing thin magnetic films |
Country Status (5)
Country | Link |
---|---|
US (1) | US3119753A (de) |
CH (1) | CH425393A (de) |
DE (1) | DE1147817B (de) |
GB (1) | GB950342A (de) |
NL (1) | NL269912A (de) |
Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3255033A (en) * | 1961-12-28 | 1966-06-07 | Ibm | Electroless plating of a substrate with nickel-iron alloys and the coated substrate |
US3297418A (en) * | 1964-04-24 | 1967-01-10 | Firestone Stanley | Magnetic thin film element and method of manufacture |
US3350180A (en) * | 1967-10-31 | Magnetic device with alternating lami- na of magnetic material and non-mag- netic metal on a substrate | ||
US3354059A (en) * | 1964-08-12 | 1967-11-21 | Ibm | Electrodeposition of nickel-iron magnetic alloy films |
US3353986A (en) * | 1963-11-20 | 1967-11-21 | Sperry Rand Corp | Electroless deposition of cobalt-ironphosphorous magnetic material |
US3393982A (en) * | 1962-11-08 | 1968-07-23 | Ncr Co | Ferromagnetic storage devices having uniaxial anisotropy |
US3442774A (en) * | 1964-03-09 | 1969-05-06 | Ibm | Method of electrodepositing a magnetic coating on a chain-like memory element |
US3549508A (en) * | 1965-11-19 | 1970-12-22 | Toko Inc | Process for producing magnetic thin film wire by multiple-layer electrodeposition |
US3699553A (en) * | 1971-02-12 | 1972-10-17 | Us Navy | Nondestructive readout thin film memory device and method therefor |
US5576099A (en) * | 1990-02-09 | 1996-11-19 | International Business Machines Corporation | Inductive head lamination with layer of magnetic quenching material |
CN102409375A (zh) * | 2011-12-01 | 2012-04-11 | 广州市海珠区金穗达表面技术发展中心 | 一种镍磷合金电镀液及其使用方法 |
CN106381510A (zh) * | 2016-12-06 | 2017-02-08 | 刘志红 | 一种Ni‑Fe‑P合金基复合镀层的制备工艺 |
CN106757287A (zh) * | 2016-12-06 | 2017-05-31 | 刘志红 | 一种Fe‑Ni‑P基复合镀层的制备工艺 |
CN104451829B (zh) * | 2014-11-20 | 2017-06-27 | 长沙理工大学 | 一种镍‑铁‑磷/纳米v8c7复合电镀液 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1965399A (en) * | 1929-06-25 | 1934-07-03 | Western Electric Co | Method of and apparatus for electro-chemically producing articles |
US2643221A (en) * | 1950-11-30 | 1953-06-23 | Us Army | Electrodeposition of phosphorusnickel and phosphorus-cobalt alloys |
US2644787A (en) * | 1950-01-05 | 1953-07-07 | Eckert Mauchly Comp Corp | Electrodeposition of a magnetic coating |
US2945217A (en) * | 1958-10-01 | 1960-07-12 | Ncr Co | Magnetic data storage devices |
-
0
- NL NL269912D patent/NL269912A/xx unknown
-
1960
- 1960-10-05 US US60735A patent/US3119753A/en not_active Expired - Lifetime
-
1961
- 1961-09-27 GB GB34704/61A patent/GB950342A/en not_active Expired
- 1961-09-30 DE DES76109A patent/DE1147817B/de active Pending
- 1961-10-04 CH CH1154261A patent/CH425393A/it unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1965399A (en) * | 1929-06-25 | 1934-07-03 | Western Electric Co | Method of and apparatus for electro-chemically producing articles |
US2644787A (en) * | 1950-01-05 | 1953-07-07 | Eckert Mauchly Comp Corp | Electrodeposition of a magnetic coating |
US2643221A (en) * | 1950-11-30 | 1953-06-23 | Us Army | Electrodeposition of phosphorusnickel and phosphorus-cobalt alloys |
US2945217A (en) * | 1958-10-01 | 1960-07-12 | Ncr Co | Magnetic data storage devices |
Cited By (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3350180A (en) * | 1967-10-31 | Magnetic device with alternating lami- na of magnetic material and non-mag- netic metal on a substrate | ||
US3255033A (en) * | 1961-12-28 | 1966-06-07 | Ibm | Electroless plating of a substrate with nickel-iron alloys and the coated substrate |
US3393982A (en) * | 1962-11-08 | 1968-07-23 | Ncr Co | Ferromagnetic storage devices having uniaxial anisotropy |
US3353986A (en) * | 1963-11-20 | 1967-11-21 | Sperry Rand Corp | Electroless deposition of cobalt-ironphosphorous magnetic material |
US3442774A (en) * | 1964-03-09 | 1969-05-06 | Ibm | Method of electrodepositing a magnetic coating on a chain-like memory element |
US3297418A (en) * | 1964-04-24 | 1967-01-10 | Firestone Stanley | Magnetic thin film element and method of manufacture |
US3354059A (en) * | 1964-08-12 | 1967-11-21 | Ibm | Electrodeposition of nickel-iron magnetic alloy films |
US3549508A (en) * | 1965-11-19 | 1970-12-22 | Toko Inc | Process for producing magnetic thin film wire by multiple-layer electrodeposition |
US3699553A (en) * | 1971-02-12 | 1972-10-17 | Us Navy | Nondestructive readout thin film memory device and method therefor |
US5576099A (en) * | 1990-02-09 | 1996-11-19 | International Business Machines Corporation | Inductive head lamination with layer of magnetic quenching material |
CN102409375A (zh) * | 2011-12-01 | 2012-04-11 | 广州市海珠区金穗达表面技术发展中心 | 一种镍磷合金电镀液及其使用方法 |
CN104451829B (zh) * | 2014-11-20 | 2017-06-27 | 长沙理工大学 | 一种镍‑铁‑磷/纳米v8c7复合电镀液 |
CN106381510A (zh) * | 2016-12-06 | 2017-02-08 | 刘志红 | 一种Ni‑Fe‑P合金基复合镀层的制备工艺 |
CN106757287A (zh) * | 2016-12-06 | 2017-05-31 | 刘志红 | 一种Fe‑Ni‑P基复合镀层的制备工艺 |
Also Published As
Publication number | Publication date |
---|---|
NL269912A (de) | |
GB950342A (en) | 1964-02-26 |
DE1147817B (de) | 1963-04-25 |
CH425393A (it) | 1966-11-30 |
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