US3607390A - Single crystal ferrimagnetic films - Google Patents

Single crystal ferrimagnetic films Download PDF

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Publication number
US3607390A
US3607390A US862080A US3607390DA US3607390A US 3607390 A US3607390 A US 3607390A US 862080 A US862080 A US 862080A US 3607390D A US3607390D A US 3607390DA US 3607390 A US3607390 A US 3607390A
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orientation
substrate
dysprosium
film
terbium
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US862080A
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Richard L Comstock
Daniel A Nepela
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International Business Machines Corp
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International Business Machines Corp
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    • 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
    • H01F10/18—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being compounds
    • H01F10/20—Ferrites
    • H01F10/24—Garnets
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/901—Levitation, reduced gravity, microgravity, space
    • Y10S117/902—Specified orientation, shape, crystallography, or size of seed or substrate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S117/00—Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10S117/906—Special atmosphere other than vacuum or inert

Definitions

  • the present invention relates to a process for making single crystal films and more particularly to a process for making thin single crystal garnet films having ferrimagnetic properties and the advantage of simultaneously combining square hysteresis loops, controllable coercivity, and compensation temperatures near room temperature.
  • the preparation of such films is very important, since the films are useful as modulators for light beams, as couplers or modulators in microwave systems, and as the active memory elements in beam addressable memory systems such as magnetothermal recording with magneto-optical readout.
  • the present application differs from the prior one in that a portion of the gadolinium must be replaced by either terbium or dysprosium.
  • the substrate besides being yttrium aluminum garnet, may also be rare earth aluminum garnet.
  • the substrate orientation may also be [100] as well as [l 1 1].
  • the substrate orientations are indicated according to standard crystallographic practice. See, for example, the textbook, STRUCTURE OF METALS, by Barrett, McGraw Hill Book Company, Inc., Second Edition, 1952, pages 8-9.
  • the garnet substrate has either [100] or [1 1 1] orientation, and the formula R -,A1,,O wherein R is yttrium or a rare earth.
  • the film has the composition Gd ,M I Fe O wherein M is terbium or dysprosium and x is within the range of about from 0.1 to 0.6 when M is terbium and the orientation is [111], within the range of about from 1 to 2.7 when M is terbium and the orientation is [100], within the range of about 0.1 to 1.7 when M is dysprosium and the orientation is [11 1], and within the range of about 0.27 to 1.7 when M is dysprosium and the orientation is [100].
  • the deposition of the film on the substrate can be accomplished by any of several methods.
  • Useful methods include spinning from an aqueous system of the proper composition and subsequent conversion to a crystalline state, and also include reactively sputtering the appropriate composition wherein the composition to be deposited constitutes the cathode of the sputtering system.
  • the technique of sputtering with two cathodes can also be used, as described in copending application Ser. No. 818,588, filed Apr. 23, 1969, by Eric Kay and Erich Sawatzky.
  • a concentrated stock solution containing gadolinium and iron ions and also those of either terbium or dysprosium (preferably all as nitrates) is first diluted with, for example, ethyl alcohol. A few drops of the diluted solution are applied to the prepared substrate held horizontally on a photoresist spinner. The solution is dis tributed into a uniform film by spinning. After 15-20 seconds of spinning, the film is sufficiently dry to remain quiescent on the substrate surface. Further drying on a hot plate at 3005O 0 C.
  • the dry product is an amorphous solid which has the desired composition according to the formula Gd ,,M
  • the crystalline garnet is obtained by heating in the presence of oxygen, for example, in the ambient atmosphere.
  • a temperature of about 650 C. to 800 C. is suitable for crystallization.
  • films having useful properties may be obtained by careful selection of the proper amount of terbium or dysprosium substituted for some of the gadolinium. It is essential that the proper amount of substituent be used.
  • the proper amount is different for terbium from that for dysprosium, and it also depends upon the orientation of the substrate.
  • the value ofx in the formula Gd M Fe O is between 0.1 and 0.6.
  • the upper limit is exceeded, the hysteresis loop is no longer square.
  • coercivity may be too high.
  • the substrate orientation is the value of x is between 1 and 2.7.
  • the hysteresis loop When the content is below this limit, the hysteresis loop is no longer square. On the other hand, when it is above the limit, the compensation temperature is too low.
  • the value of x should be between 0.1 and 1.7 when the orientation of the substrate is [111].
  • the dysprosium content is too low, it does not exert sufficient influence on the coercivity.
  • the compensation temperature becomes too low.
  • the orientation is 100] the value ofx should be between 0.27 and 1.7.
  • the hysteresis loop When the dysprosium level is below this limit, the hysteresis loop is no longer square and when the dysprosium content is above this limit, the compensation temperature drops too low.
  • the present invention provides a method of obtaining thin ferrimagnetic films having square hysteresis loops, compensation temperatures in the most desirable range near ambient temperatures, and also coercivities which may be regulated within a wide range of useful values. These three physical properties are simultaneously determined according to the present invention by the proper selection of the amount of terbium or dysprosium.
  • Example 1 Gd -,Tb Fe O, on [1 1 l oriented yttrium aluminum garnet yields a coercivity of 250 0c at compensation temperature plus 30 C., and an Mr/Ms l .0.
  • Example 111 Gd Tb Fe O on [100] oriented yttrium aluminum garnet yields a coercivity of 520 oe at compensation temperature plus 30 C. and an Mr/Ms Z 0.95.
  • Example V Gd Dy Je O on [100] oriented yttrium aluminum garnet would yield a coercivity of 520 at compensation temperature plus 30 C. and an Mr/Ms Z 0.95.
  • Example VI In a manner like that shown in the above examples, in place of yttrium aluminum garnet substrate, rare earth aluminum garnet substrate may be employed and similar results obtained.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Power Engineering (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Thin Magnetic Films (AREA)

Abstract

A process for preparing single crystal ferrimagnetic films having square hysteresis loops, a regulated coercivity, and a compensation temperature above 250* K. A film of gadolinium iron garnet wherein a carefully selected amount of terbium or dysprosium replaces part of the gadolinium is deposited on a tytrium or rare earth aluminum garnet substrate having (111) or (100) orientation and heated until crystallization occurs.

Description

United States Patent Richard L. Comstock San Jose;
Daniel A. Nepela, Saratoga, both of Calif. 862,080
Sept. 29, 1969 Sept. 21, 1971 International Business Machines Corporation Armonk, N.Y.
Inventors Appl. No. Filed Patented Assignee SINGLE CRYSTAL FERRIMAGNETIC FILMS 5 Claims, No Drawings u.s.c| 117/237,
117/235 Int. Cl n01: 10/02 FieldolSearch 117/235,
Primary Examiner-William D. Martin Assistant Examiner- Bernard D. Pianalto AnorneysHanifin and Jancin and Joseph G. Walsh ABSTRACT: A process for preparing single crystal ferrimagnetic films having square hysteresis loops, a regulated coercivity, and a compensation temperature above 250 K. A film of gadolinium iron garnet wherein a carefully selected amount of terbium or dysprosium replaces part of the gadolinium is deposited on a tytrium or rare earth aluminum garnet substrate having [111] or [100] orientation and heated until crystallization occurs,
SINGLE CRYSTAL FERRIMAGNETIC FILMS FIELD OF THE INVENTION The present invention relates to a process for making single crystal films and more particularly to a process for making thin single crystal garnet films having ferrimagnetic properties and the advantage of simultaneously combining square hysteresis loops, controllable coercivity, and compensation temperatures near room temperature. The preparation of such films is very important, since the films are useful as modulators for light beams, as couplers or modulators in microwave systems, and as the active memory elements in beam addressable memory systems such as magnetothermal recording with magneto-optical readout.
PRIOR ART Pending application Ser. No. 766,698, filed Oct. 1 l, 1968, by Eric Kay and Erich Sawatzky, and assigned to the assignee of the present application, discloses a process for forming single crystal garnet films. According to that application, gadolinium iron garnet is deposited on a substrate of yttrium aluminum garnet in the [1 1 l] orientation.
SUMMARY OF THE INVENTION The present application differs from the prior one in that a portion of the gadolinium must be replaced by either terbium or dysprosium. The substrate, besides being yttrium aluminum garnet, may also be rare earth aluminum garnet. Furthermore, the substrate orientation may also be [100] as well as [l 1 1]. The substrate orientations are indicated according to standard crystallographic practice. See, for example, the textbook, STRUCTURE OF METALS, by Barrett, McGraw Hill Book Company, Inc., Second Edition, 1952, pages 8-9. According to the present invention, the garnet substrate has either [100] or [1 1 1] orientation, and the formula R -,A1,,O wherein R is yttrium or a rare earth. The film has the composition Gd ,M I Fe O wherein M is terbium or dysprosium and x is within the range of about from 0.1 to 0.6 when M is terbium and the orientation is [111], within the range of about from 1 to 2.7 when M is terbium and the orientation is [100], within the range of about 0.1 to 1.7 when M is dysprosium and the orientation is [11 1], and within the range of about 0.27 to 1.7 when M is dysprosium and the orientation is [100].
In carrying out the process of the present invention, the deposition of the film on the substrate can be accomplished by any of several methods. Useful methods include spinning from an aqueous system of the proper composition and subsequent conversion to a crystalline state, and also include reactively sputtering the appropriate composition wherein the composition to be deposited constitutes the cathode of the sputtering system. The technique of sputtering with two cathodes can also be used, as described in copending application Ser. No. 818,588, filed Apr. 23, 1969, by Eric Kay and Erich Sawatzky.
The techniques employed for the steps of the present invention are the same as those which have been previously described in the literature. The chemical method of spinning is preferred because of the ease in changing composition and because the resulting films have particularly good optical quality. According to this technique, a concentrated stock solution containing gadolinium and iron ions and also those of either terbium or dysprosium (preferably all as nitrates) is first diluted with, for example, ethyl alcohol. A few drops of the diluted solution are applied to the prepared substrate held horizontally on a photoresist spinner. The solution is dis tributed into a uniform film by spinning. After 15-20 seconds of spinning, the film is sufficiently dry to remain quiescent on the substrate surface. Further drying on a hot plate at 3005O 0 C. decomposes the nitrates to oxides and converts the film to a glassy state which makes the film insoluble in a spinning solution. The spin dry process may then be repeated to achieve the desired final thickness. Single coat thicknesses are about 1,000 A.The dry product is an amorphous solid which has the desired composition according to the formula Gd ,,M
,Fe O given above, and wherein the amount of gadolinium, iron, terbium, or dysprosium is in accordance with the relative amounts present in the original solutions. The crystalline garnet is obtained by heating in the presence of oxygen, for example, in the ambient atmosphere. A temperature of about 650 C. to 800 C. is suitable for crystallization.
We have discovered that films having useful properties may be obtained by careful selection of the proper amount of terbium or dysprosium substituted for some of the gadolinium. It is essential that the proper amount of substituent be used. The proper amount is different for terbium from that for dysprosium, and it also depends upon the orientation of the substrate. When terbium is used and the substrate has the 1 1 l] orientation, the value ofx in the formula Gd M Fe O is between 0.1 and 0.6. When the upper limit is exceeded, the hysteresis loop is no longer square. On the other hand, when the amount of terbium is below this limit, coercivity may be too high. When the substrate orientation is the value of x is between 1 and 2.7. When the content is below this limit, the hysteresis loop is no longer square. On the other hand, when it is above the limit, the compensation temperature is too low. When the substituent is dysprosium the value of x should be between 0.1 and 1.7 when the orientation of the substrate is [111]. When the dysprosium content is too low, it does not exert sufficient influence on the coercivity. When the dys prosium content is too high, the compensation temperature becomes too low. When the orientation is 100] the value ofx should be between 0.27 and 1.7. When the dysprosium level is below this limit, the hysteresis loop is no longer square and when the dysprosium content is above this limit, the compensation temperature drops too low.
The present invention provides a method of obtaining thin ferrimagnetic films having square hysteresis loops, compensation temperatures in the most desirable range near ambient temperatures, and also coercivities which may be regulated within a wide range of useful values. These three physical properties are simultaneously determined according to the present invention by the proper selection of the amount of terbium or dysprosium.
PREFERRED EMBODIMENTS The general nature of the invention having been set forth, the following examples are now presented as to the specific preparation of preferred embodiments of the invention. The specific details presented are for purposes of illustration and not limitation.
Example 1 Gd -,Tb Fe O, on [1 1 l oriented yttrium aluminum garnet yields a coercivity of 250 0c at compensation temperature plus 30 C., and an Mr/Ms=l .0.
Example 11 Gd Tb Fe O, on [11 1] oriented yttrium aluminum garnet yields a coercivity of oe at compensation temperature plus 30 C. and an Mr/Ms=1.0.
Example 111 Gd Tb Fe O on [100] oriented yttrium aluminum garnet yields a coercivity of 520 oe at compensation temperature plus 30 C. and an Mr/Ms Z 0.95.
Example IV Gd Dy,Fe O, on [111] oriented yttrium aluminum garnet yields a coercivity of 1,140 oe at compensation temperature plus 30 C. and an Mr/Ms=l .0.
Example V Gd Dy Je O on [100] oriented yttrium aluminum garnet would yield a coercivity of 520 at compensation temperature plus 30 C. and an Mr/Ms Z 0.95.
Example VI In a manner like that shown in the above examples, in place of yttrium aluminum garnet substrate, rare earth aluminum garnet substrate may be employed and similar results obtained.
All of the above films were prepared at a thickness of l.0p.i0.2.
While the invention has been shown and described with reference to preferred embodiments thereof, it will be ap preciated by those skilled in the art that variations in form may be made therein without departing from the spirit and scope of the invention.
What is claimed is:
l. A process for preparing a single crystal ferrimagnetic film having a square hysteresis loop, a regulated coercivity, and a compensation temperature above 250 K., said process comprising:
a. depositing on a garnet substrate having [111] or [100] orientation, and having the formula R Al O wherein R is yttrium or a rare earth, a film having the composition Gd -,,,M,Fe .,0,, wherein M is terbium or dysprosium and x is within the range from 0.1 to 0.6 when M is terbium and the orientation is [l l l within the range of l to 2.7
when M is terbium and the orientation is [I00], within the range 0.1 to 1.7 when M is dysprosium and the orientation is [l l 1], and within the range 0.27 to 1.7 when M is dysprosium and the orientation is and b. heating in an oxygen-containing atmosphere until crystallization occurs.
2. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having [111] orientation and the film has the formula Gd ,,Tb,Fe O wherein x is within the range from 0.1 to 0.6.
3. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having [100] orientation and the film has the formula Gd Tb,Fe O wherein x is within the range from 1 to 2.7.
4. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having [111] orientation and the film has the formula Gd Dy,Fe O,, wherein x is within the range from 0.1 to 1.7.
5. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having [100] orientation and the film has the formula Gd ,,Dy ,Fe -,O, wherein x is within the range from 0.27 to 1.7.

Claims (4)

  1. 2. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having (111) orientation and the film has the formula Gd3 xTbxFe5O12 wherein x is within the range from 0.1 to 0.6.
  2. 3. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having (100) orientation and the film has the formula Gd3 xTbxFe5O12 wherein x is within the range from 1 to 2.7.
  3. 4. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having (111) orientation and the film has the formula Gd3 xDyxFe5O12 wherein x is within the range from 0.1 to 1.7.
  4. 5. A process as claimed in claim 1 wherein the substrate is yttrium aluminum garnet having (100) orientation and the film has the formula Gd3 xDyxFe5O12 wherein X is within the range from 0.27 to 1.7.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2349348A1 (en) * 1972-10-07 1974-04-11 Philips Nv MAGNETIC DEVICE WITH A MAGNETO-OPTICAL MEDIUM AND METHOD FOR MANUFACTURING IT
US3837911A (en) * 1971-04-12 1974-09-24 Bell Telephone Labor Inc Magnetic devices utilizing garnet epitaxial materials and method of production
US3849193A (en) * 1971-05-25 1974-11-19 Commissariat Energie Atomique Method of preparation of single crystal films
US4827218A (en) * 1985-05-30 1989-05-02 Thomson-Csf Linear magnetoresistance-effect sensor with semiconductor and ferrimagnetic layers and its application in a magnetic-domain detector
EP0410627A1 (en) * 1989-07-27 1991-01-30 Kabushiki Kaisha Toshiba Oxide film with preferred crystal orientation, method of manufacturing the same, and magneto-optical recording medium
US5607781A (en) * 1989-07-27 1997-03-04 Kabushiki Kaisha Toshiba Oxide film with preferred crystal orientation, method of manufacturing the same, and magneto-optical recording medium
US5851284A (en) * 1995-11-21 1998-12-22 Nippon Telegraph And Telephone Corporation Process for producing garnet single crystal

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS623022A (en) * 1985-06-27 1987-01-09 Nec Corp Magneto-optical garnet

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3429740A (en) * 1965-09-24 1969-02-25 North American Rockwell Growing garnet on non-garnet single crystal
US3437577A (en) * 1967-06-26 1969-04-08 Ibm Method of fabricating uniform rare earth iron garnet thin films by sputtering
US3486937A (en) * 1967-03-24 1969-12-30 Perkin Elmer Corp Method of growing a single crystal film of a ferrimagnetic material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3429740A (en) * 1965-09-24 1969-02-25 North American Rockwell Growing garnet on non-garnet single crystal
US3486937A (en) * 1967-03-24 1969-12-30 Perkin Elmer Corp Method of growing a single crystal film of a ferrimagnetic material
US3437577A (en) * 1967-06-26 1969-04-08 Ibm Method of fabricating uniform rare earth iron garnet thin films by sputtering

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3837911A (en) * 1971-04-12 1974-09-24 Bell Telephone Labor Inc Magnetic devices utilizing garnet epitaxial materials and method of production
US3849193A (en) * 1971-05-25 1974-11-19 Commissariat Energie Atomique Method of preparation of single crystal films
DE2349348A1 (en) * 1972-10-07 1974-04-11 Philips Nv MAGNETIC DEVICE WITH A MAGNETO-OPTICAL MEDIUM AND METHOD FOR MANUFACTURING IT
US4827218A (en) * 1985-05-30 1989-05-02 Thomson-Csf Linear magnetoresistance-effect sensor with semiconductor and ferrimagnetic layers and its application in a magnetic-domain detector
EP0410627A1 (en) * 1989-07-27 1991-01-30 Kabushiki Kaisha Toshiba Oxide film with preferred crystal orientation, method of manufacturing the same, and magneto-optical recording medium
US5607781A (en) * 1989-07-27 1997-03-04 Kabushiki Kaisha Toshiba Oxide film with preferred crystal orientation, method of manufacturing the same, and magneto-optical recording medium
US5851284A (en) * 1995-11-21 1998-12-22 Nippon Telegraph And Telephone Corporation Process for producing garnet single crystal

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JPS4932597B1 (en) 1974-08-31
DE2041847C3 (en) 1978-09-28
DE2041847B2 (en) 1978-01-26
DE2041847A1 (en) 1971-04-08
GB1268029A (en) 1972-03-22
FR2060934A5 (en) 1971-06-18
CA943439A (en) 1974-03-12

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