JPS58147538A - Sputtered amorphous magnetic material and its manufacture - Google Patents
Sputtered amorphous magnetic material and its manufactureInfo
- Publication number
- JPS58147538A JPS58147538A JP57028064A JP2806482A JPS58147538A JP S58147538 A JPS58147538 A JP S58147538A JP 57028064 A JP57028064 A JP 57028064A JP 2806482 A JP2806482 A JP 2806482A JP S58147538 A JPS58147538 A JP S58147538A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic material
- amorphous magnetic
- niobium
- amorphous
- sputtered
- 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.)
- Pending
Links
- 239000000696 magnetic material Substances 0.000 title claims abstract description 152
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 45
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 239000010955 niobium Substances 0.000 claims description 50
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 44
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 24
- 229910017052 cobalt Inorganic materials 0.000 claims description 20
- 239000010941 cobalt Substances 0.000 claims description 20
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 20
- 229910052742 iron Inorganic materials 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 11
- 239000011572 manganese Substances 0.000 claims description 10
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052735 hafnium Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052715 tantalum Inorganic materials 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052785 arsenic Inorganic materials 0.000 claims description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 239000004859 Copal Substances 0.000 claims description 3
- 241000782205 Guibourtia conjugata Species 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004071 soot Substances 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 241000894007 species Species 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 41
- 230000004907 flux Effects 0.000 abstract description 32
- 238000002425 crystallisation Methods 0.000 abstract description 11
- 230000008025 crystallization Effects 0.000 abstract description 11
- 239000000758 substrate Substances 0.000 abstract description 11
- 238000004544 sputter deposition Methods 0.000 abstract description 7
- 239000000470 constituent Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 22
- 238000000034 method Methods 0.000 description 16
- 230000005415 magnetization Effects 0.000 description 15
- 238000005260 corrosion Methods 0.000 description 14
- 230000007797 corrosion Effects 0.000 description 14
- 230000005389 magnetism Effects 0.000 description 8
- 229910052721 tungsten Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- -1 panazicum Chemical compound 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 229910052752 metalloid Inorganic materials 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910002056 binary alloy Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910020517 Co—Ti Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000007545 Vickers hardness test Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910020515 Co—W Inorganic materials 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 235000003976 Ruta Nutrition 0.000 description 1
- 240000005746 Ruta graveolens Species 0.000 description 1
- 241000269821 Scombridae Species 0.000 description 1
- 241000270666 Testudines Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 235000020640 mackerel Nutrition 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 235000005806 ruta Nutrition 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15358—Making agglomerates therefrom, e.g. by pressing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Soft Magnetic Materials (AREA)
- Thin Magnetic Films (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はスパッタ非晶質磁性材料及び七ＯＩｌ造方法に
関するものであ如、４１１に飽和磁束一度か大きく、保
臓力及び磁歪が小さい軟磁気特性が優れ九スパッタ非蟲
質磁性材料及びそＯＩｍ造方法に関する４のである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sputtered amorphous magnetic material and a method for producing 7OIl. Part 4 relates to magnetic magnetic materials and their OI manufacturing method.
スパッタリング法を用いて得喪スパッタ非晶質磁性材料
が知られている。このようにして得られ九非晶質磁性材
料は、結晶磁性材料の如き規則的原子配＾をとることな
く長周期的構造を持たず。It is known that sputtered amorphous magnetic materials can be obtained using a sputtering method. The amorphous magnetic material obtained in this way does not have a regular atomic arrangement and does not have a long-period structure like crystalline magnetic materials.
原子配列が無秩序１に材料であること力・ら、結晶磁気
異方性かなく良好な軟磁気特性を示す材料である。Since the material has a disordered atomic arrangement, it has no crystal magnetic anisotropy and exhibits good soft magnetic properties.
またこのスパッタ非晶質磁性材料はガス状態の金属を凝
集させること、すなわち気体から直接固体を形成１せる
ような一種の凍結作用によって得られ九非晶質材料であ
るから、溶融状部にある磁性材料を射出し、これを高速
回転するドラムに接触させて急冷して、非晶質磁性材料
リボンを形成する超急冷法によって得られた４のに比べ
て極めて薄い膜を得ることがで勤る亀ど０４＋１黴点を
有している。更に上記Ｏ超急冷法において！Ｉｉ溶融状
態にある磁性材料に更にホウ素、シリコンなどの非磁性
元素を含有していない＠）非晶質磁性材料か形成されな
いＯＫ対し、スパッタリング法においてはかかる元素を
加えなくても非晶質磁性材％＆影形成ることができるこ
とから、両プロ竜スによって得られ良材料は本質的に興
なる材料であると言える。In addition, this sputtered amorphous magnetic material is obtained by agglomerating metal in a gaseous state, that is, by a kind of freezing effect that directly forms a solid from a gas. It is possible to obtain an extremely thin film compared to the ultra-quenching method obtained by the ultra-quenching method in which a magnetic material is injected and brought into contact with a high-speed rotating drum to form an amorphous magnetic material ribbon. It has a mildew point of 04+1. Furthermore, in the above O super-quenching method! Ii The magnetic material in the molten state does not contain any non-magnetic elements such as boron or silicon @) Amorphous magnetic material is not formed.In contrast, in the sputtering method, amorphous magnetic material is not formed even without adding such elements. Since it can form materials and shadows, it can be said that the good materials obtained by both professional dragons are essentially good materials.
本発明は新規なスパッタ非晶質磁性材料及びそＯＩＩ造
方法【提供せんとすることｔａ的とする。The present invention aims to provide a novel sputtered amorphous magnetic material and its OII manufacturing method.
本発明は、コバルトを主体とし、ニオブ［４Ｇ原子パー
セント以下會むことを特徴とするスパッタ非晶質磁性材
料であ）、更にコバルトを主体とし、ニオブを１ｏｌｌ
子パーセント以下含む非晶質磁性材料を結晶化温度以下
Ｏ温度で熱処理することを特徴とするスパッタ非晶質磁
性材料ｏｐ造方法である。The present invention is a sputtered amorphous magnetic material mainly composed of cobalt and niobium [which is characterized by a content of less than 4G atomic percent], and further mainly composed of cobalt and 1ol of niobium.
This is a sputtering method for producing an amorphous magnetic material by sputtering, which is characterized by heat-treating an amorphous magnetic material containing less than 1% of the total amount of amorphous material at a temperature below the crystallization temperature.
更に本実−０１’）ｔ）＠＠はコバルトを主体とし、ニ
オブを４０原子バー七ント以下含み、更にチタン、ジル
コニウム、ハフニウム、パナジクム、タンタル、銅、モ
リブデン、タングステンから成る詳から選ばれえ少なく
ともｌ１ｌＯ追加的元素を含むヒとを特徴とするスパッ
タ非晶質磁性材料であ如、又本発明ＯＩＩ１１０ＩＩｗ
Ｉｋはコパル）１主体とし、ニオブを４ａ鳳子パーセン
ト以下含み、］！にタロム、マンガン、ニッケル、鉄か
ら成る詳から選ばれた少なくとも１種Ｏ追加的元素を含
むことを特徴とするスパッタ非晶質磁性材料であ〕、本
発明Ｏ他Ｏｍｌ轡はコバルトを主体とし、ニオブｆ４２
原子パーセント以下含み、更にほう素、炭素、けい素、
リン、ゲルマニウム、すす、インジウム、ひ素、アンチ
毫ンから威る詳から選ばれえ少なくとも１種Ｏ追加的元
素を會むヒとを特徴とするスパッタ非晶質磁性材料であ
夛、更に本発明Ｏ他Ｏｍ＊ｒｉコバルトを主体とし、ニ
オブを４ａｌ［子Ｉ（−七ント以下含与％］！に鉄及び
マンガンから成る群から選ばれえ少くとも１種Ｏ追加的
兄素を含むととｔｒ＊徴とするスパッタ非晶質磁性材料
である。Furthermore, Honjitsu-01')t)@@ is mainly composed of cobalt, contains 40 atoms or less of niobium, and is further selected from the group consisting of titanium, zirconium, hafnium, panazicum, tantalum, copper, molybdenum, and tungsten. A sputtered amorphous magnetic material characterized in that it contains at least an additional element of l11O, and the present invention OII110IIw
Ik is copal) 1, contains niobium at less than 4a Foshi percent, ]! This is a sputtered amorphous magnetic material characterized by containing at least one additional element selected from the group consisting of talom, manganese, nickel, and iron. , niobium f42
Contains less than atomic percent of boron, carbon, silicon,
The present invention further comprises a sputtered amorphous magnetic material characterized by having at least one additional element selected from the group consisting of phosphorus, germanium, soot, indium, arsenic, and antipropylene. Om*ri mainly composed of cobalt, containing 4al of niobium [child I (-7% or less content]!) and at least one additional brother element selected from the group consisting of iron and manganese. This is a sputtered amorphous magnetic material with tr* characteristics.
次に本発明Ｏスパッタ非晶質磁性材料を製造する方法の
一例について第１図会参照して説明する。Next, an example of a method for manufacturing the O sputtered amorphous magnetic material of the present invention will be described with reference to FIG.
＠Ｉｌｌは本発明のスパッタ非晶質磁性材料を製造する
えめＯ装置ｖ−ｆｌｔ示す概略断面図である。＠Ill is a schematic cross-sectional view showing a v-flt apparatus for producing the sputtered amorphous magnetic material of the present invention.
第１１１において、容Ｉ！１１内には約１０−” ｔｏ
ｒｒｃｓｔｔｔｔ−ムｒガスが耐大されている。１１１
１へ０ＡｒｔＪスは例えば１ｏ−・テｏｒｒ ｆＣ予備
真空され九＊Ｋ １０−”テｏｒｒ ｔで真空にされる
。２及びｓ＃ｉｔ”れぞれタングステンフィラメント及
びステンレス板によって構成されているカノード及び７
ノードであ夛、これらＯ関には電源４によって約１０７
．４０Ａ＠度の電圧、電＃ｌか印加され容器１中にプラ
ズマを発生させる。ここでアノ−レジＳは水冷され更に
電源ＳＫよって１００７以下ｌ１１０＊＊正電圧が印加
されてもよい。４はターゲット電極÷あ）、少なくとも
コパルＦ及びニオブ【會む材料か１１１！質されておＬ
水冷されている。しめターゲット電極６には電源７によ
りてＯ〜１ｚ口０Ｙ１１度の負電圧が印加されている。In the 111th, Yong I! Approximately 10-” to 11
rrcstttt-mr gas is resistant. 111
1 to 0ArtJ, for example, is pre-evacuated to 1o-teorr fC and evacuated at 9*K10-"teorrt. 2 and s#it" are each constructed of a tungsten filament and a stainless steel plate. and 7
With a large number of nodes, these O ports have approximately 107
．． A voltage of 40 A@degrees is applied to generate plasma in the container 1. Here, the anorage S may be water-cooled and further a positive voltage of 1007 or less l110** may be applied by the power source SK. 4 is target electrode ÷ a), at least copal F and niobium [meeting material 111! L
It is water cooled. A negative voltage of 0 to 11 degrees is applied to the tightening target electrode 6 by a power source 7.
魯は本発明Ｏ非晶質磁性材料ｔデポジットするえめＯ基
板であって水冷され、１１！に電源！によって最大５ｏ
ｏｖ＠度Ｏ負電圧が印加されてもよい。The present invention is a substrate on which an amorphous magnetic material is deposited, which is water-cooled, and 11! Power to! up to 5o by
An ov@degree O negative voltage may be applied.
本実Ｔｌ１４ｔ）非晶質磁性材ｌＩ！は上記カンード２
及び７／−ＦｌとＯＱＫ約１＠マ、４０ＡＯ電圧電流を
印加しプラズマを発生させ、プラダ１中に斃生し良イオ
ンｉｔ−’ＩＫマ（最大約ＳＯＤ鵬ム）０強い電界で加
速し、ターゲット’ＷＬＩｈｈｋｘｚ＜ツメして構成原
子【放出させ、これを基板魯↓に付着、堆積させるとと
によって得られる。この−にしてＳ日間Ｏ連続スパッタ
によって厚さ約！００声鵬の非晶質磁性材料を得ること
ができえ。Honji Tl14t) Amorphous magnetic material lI! is the above cand 2
And 7/-Fl and OQK about 1 @ ma, 40 AO voltage and current are applied to generate plasma, and good ions are generated in Prada 1 and are accelerated by a strong electric field (maximum of about SOD). , the target'WLIhhkxz< is obtained by ejecting the constituent atoms and attaching and depositing them onto the substrate. The thickness is approx. by continuous O sputtering for -S days! It is possible to obtain an amorphous magnetic material of 0.00.
次にこＯ−にして作った本発明の非晶質磁性材料につい
て、実験した結果について第り表及び第２＠ｌに基いて
説−する。第１表及び第２表は上述０’ｍｌ製法によ）
基板上に非晶質磁性材料を付着させて、厚さａｌｍｓ、
直径４０−０円盤状試料及び外４％ Ｓ Ｏａｍ、内＠
２０ｍｌ０りンダ状試料をそれぞれ作威し、これらの磁
気分析、磁化―纏Ｏ欄定、示差熱分析、硬さ試験及び分
極−纏ＯＶａ定をそれぞれ行１に％Ａ、その試料Ｏ軟磁
気特性、熱的安定性。Next, the results of experiments conducted on the amorphous magnetic material of the present invention prepared using O- will be explained based on Table 1 and Section 2@l. Tables 1 and 2 are based on the 0'ml manufacturing method mentioned above)
Depositing an amorphous magnetic material on the substrate to a thickness of alms,
Diameter 40-0 disc-shaped sample and outer 4% S Oam, inner @
A 20 ml cylinder-like sample was prepared, and the magnetic analysis, magnetization-column O column, differential thermal analysis, hardness test, and polarization-column OVa column were measured in %A in row 1, and the soft magnetic properties of the sample were measured. , thermal stability.
機械的性質及び耐食性について調べ良結果を示す４ので
ある。No. 4 has been tested for mechanical properties and corrosion resistance and has shown good results.
なお、このようにして作成し良磁性材料が非晶質構造【
示すこと０４１１１定はターゲットとしてν・。Note that the good magnetic material created in this way has an amorphous structure [
Show that 04111 is constant ν· as the target.
Ｋｍ纏を用い、！曽闘折線を測定することによって行な
った。そＯ結果＄１表及び第２１１Ｋ示す試＊ＯＸｍＭ
折線ｄ２〜ＳＯ散慢ｔａ折Ｖｙ１０４を示し、結晶のよ
うな鋭いＩ折線を示さず、これらが非晶質構造となって
いることが明らかとなつ九。Using Km-mat! This was done by measuring the so-to-fold line. Test showing result $1 table and 211K *OXmM
It shows the fold line d2 to SO scattering ta fold Vy104, and does not show a sharp I fold line like a crystal, making it clear that these have an amorphous structure.
第１１１はコバルト及びニオブＯ組成を種々変化させて
作うえ本発明Ｏスパッタ非晶質磁性材料Ｏ室−における
飽和磁化、飽和磁束一度、磁歪、保磁力、硬さ、結晶化
温度及びキエーリ一点をそれぞれ示す。第１表において
飽和磁化及び飽和磁束豐度はニオブＯ含有率が低いＩＩ
（二元系にお−ではコバルトの含有率が＾いＩＩ）高い
値を示す。又、磁性材料として高い飽和磁束ＩＩｆと共
に優れえ軟磁性を示すえめには磁気ひず拳（磁歪）が小
さい事が必要であるが、本発明のスパッタ非晶質、磁性
材料は磁歪がいずれも負Ｏ比較的小さな値を示す。No. 111 is made by varying cobalt and niobium O compositions, and saturation magnetization, saturation magnetic flux, magnetostriction, coercive force, hardness, crystallization temperature, and Chieri point in the sputtered amorphous magnetic material according to the present invention. Each is shown below. In Table 1, the saturation magnetization and saturation magnetic flux intensity are II with low niobium O content.
(In a binary system, the content of cobalt is high II). In addition, as a magnetic material, it is necessary to have a small magnetostriction (magnetostriction) in order to exhibit excellent soft magnetism as well as a high saturation magnetic flux IIf. Negative O indicates a relatively small value.
本発明Ｏスパッタ非晶質磁性材料Ｏ大Ｉｔ特徴点０１つ
は磁歪が比較的小さな値を示し、更にそＯ値が負である
点にある。即ち、近年半金属元素を含まない００−系非
晶質磁性材料（Ｏｏ−テ１ｅＺｒ＊Ｈｆ、テ＆ Ｗ）
が優れえ軟磁性特性を示すことで注目され発表がなされ
ている。これらのうち０Ｏ−Ｔｉ系、Ｃｏ−Ｋｒ系及び
０ｏ−１ｆ 系非晶質磁性材料は磁歪が正Ｏ値を示す材
料であるから、ζＯ磁歪を実質的に零にする良めには例
えばｌＩｉ、Ｍｏ及びＯｒ を加えなければならないが
％このような元素は磁性材料Ｏ鉋和磁束書［を減少させ
てしまう。One characteristic point of the O sputtered amorphous magnetic material of the present invention is that the magnetostriction exhibits a relatively small value, and furthermore, the O value is negative. That is, in recent years, 00-based amorphous magnetic materials (Oo-Te1eZr*Hf, Te&W) that do not contain metalloid elements have been developed.
It has attracted attention and has been published as it exhibits excellent soft magnetic properties. Among these, 0O-Ti system, Co-Kr system, and 0o-1f system amorphous magnetic materials are materials whose magnetostriction exhibits a positive O value, so for example, lIi , Mo and Or must be added, but these elements reduce the magnetic flux of the magnetic material.
一方Ｇｏ−？ａ系及び０ｏ−Ｗ系非晶質磁性材料は磁歪
が負である仁とから例えばν・、 Ｍｕ を加えて磁
歪を実質的に零にすることができ、更にこれらの元素は
磁性材料の飽和磁束＊ｔを増加させるか少なくともｔｌ
とんと低下させないＯで喪好な非晶質磁性材料であると
言えるが、かかるＣｏ−Ｔｉ系及び００−Ｗ系非晶質磁
性材料においても本発明０Ｃｏ−１１ｂ系非晶質磁性材
料に比して低い飽和磁束書＆０４０か得られるに過ぎな
い。即ち本発明の非蟲質ｍｋ！！材料は例えば伊達する
第２表Ｏ試料胤１ ＠ （”８１５ Ｆ・４Ｌ５１”１
０）Ｋ示す如く磁歪が実質的に零で、１２乃至１ｓキＵ
ガウス以上の極めて大きな飽和磁束密ａｔ有する材料を
作成することができる。On the other hand, Go-? The magnetostriction of a-based and 0o-W-based amorphous magnetic materials can be reduced to substantially zero by adding, for example, ν·, Mu to the negative magnetostriction, and furthermore, these elements can reduce the saturation of the magnetic material. increase the magnetic flux *t or at least tl
Although it can be said that it is a good amorphous magnetic material because of O that does not drop significantly, such Co-Ti-based and 00-W-based amorphous magnetic materials also have a higher resistance compared to the 0Co-11b-based amorphous magnetic material of the present invention. Therefore, only a low saturation magnetic flux of &040 can be obtained. That is, the non-insect mk of the present invention! ! The material is, for example, Date Table 2 O Sample Seed 1 @ ("815 F・4L51" 1
0) As shown in K, magnetostriction is virtually zero, and 12 to 1 s
It is possible to create a material having an extremely large saturation magnetic flux density at of Gauss or higher.
従って本発明で最も好ましい非晶質磁性材料はコバルト
を主体とし、ニオブ１４０ｊ［子パー七ント含み、更に
鉄、マンガンの少なくともいずれか一方Ｏ追加的元素を
含むものであ）、こＯ追加的元素の量としては例えば（
Ｏｏｌ−ｘＭＩＳｘ）６５３１ｂ１５０組成の非晶質磁
性材料においてはＸがａ０４からＣＬ０４０値にあるこ
とがよく、又、００８五５−に？・８１１ｂ１４５
（）組成の非晶質磁性材料にあってｆｉｘがａｏｌから
ａａｉｏＨｃあることがよ−。Therefore, the most preferable amorphous magnetic material in the present invention is one containing cobalt as a main component, niobium 140j [containing niobium 140j] and at least one of iron and manganese as an additional element. For example, the amount of an element is (
Ool-x MIS・811b145
In the amorphous magnetic material having the composition (), the fix ranges from aol to aaioHc.
又、ホウ素などの半金属元素を添加し九ときＯ飽和磁束
１１度Ｏ低下及び磁ｊＯ変化を考慮すれば、本実１ｊＩ
Ｏ非晶質磁性材料にはこれら半金属元素【含まないこと
が好ましい。Moreover, if we add a metalloid element such as boron and take into consideration the decrease in O saturation magnetic flux by 11 degrees and the change in magnetic jO, the actual 1jI
The amorphous magnetic material preferably does not contain these metalloid elements.
本発明Ｏスパ゛／夕非晶質磁性材料に要求される軟磁性
の目安として保磁力は重畳な性質であ〉、こむ保磁力が
できる隈）小さいことが要求されるが、本実１１４のス
バクタ非晶質磁性材料＃１ＪＩＩＩＩＩＩに示す如く、
比較的ＫｊＬ好な値を示す。又ζＯ保畝力は第Ｓ’ｌＫ
示す如く適！！１に条件での加熱処理によ如更に小さく
することができる。即ち、ｔａｓ’ｔｓに示ｔ１ｍ ＜
、試料−３（００！ｌ！ＬＳＩＩｂ１Ｌ５）の組成にお
ける熱処理しない場合Ｏ保磁力は１８０１１０６０値を
示すが、第３表に示す各＠鮫で５０分熱処理することに
よって更に小さな保磁力となることが判る。例えば３６
０℃Ｏｍ１度で熱処理しえときは３５１１０＠、４０ｏ
ｃｃ＋ｉｉ＊で熱処理したときには３０ｍ０・ Ｏ極め
て低い値を示す。As a measure of the soft magnetism required for the amorphous magnetic material of the present invention, the coercive force is a superimposed property, and it is required that the coercive force be small. As shown in Subakta amorphous magnetic material #1 JIIIIII,
It shows a relatively good value of KjL. Also, ζO ridge force is No. S'lK
Suitable as shown! ! The size can be further reduced by heat treatment under conditions 1. That is, t1m <
, the O coercive force in the composition of Sample-3 (00!l!LSIIb1L5) without heat treatment shows a value of 18011060, but by heat treating each @Shark shown in Table 3 for 50 minutes, the coercive force becomes even smaller. I understand. For example 36
35110@, 40o when heat treatment can be done at 0℃Om1 degree
When heat treated at cc+ii*, it shows an extremely low value of 30m0·O.
本発明における熱処ｇｏ条件は少なくとも非晶質磁性材
料を結晶化温度以下０１１度で熱処理することが必要で
あるか、ニオブＯ組成比が高い場合には比較的低温の熱
処理で効果を生じるがニオブの組成比が低い場合には比
較的高温０熱処理を必要とする。即ちこの繰処理温ｔｔ
ｉ−オプの組成比が高い場合１５０℃乃至結晶化温度で
数時間乃至１分Ｉ１度、ニオブＯ＃Ｉ成比が低い場合に
は２５０℃乃至結晶化温度で数時間乃至１分ｓｆでよい
。The heat treatment conditions in the present invention require that at least the amorphous magnetic material be heat treated at 0.11 degrees below the crystallization temperature, or if the niobium O composition ratio is high, heat treatment at a relatively low temperature will produce an effect. When the composition ratio of niobium is low, relatively high temperature zero heat treatment is required. That is, this reprocessing temperature tt
If the composition ratio of i-op is high, it may be sf for several hours to 1 minute at 150°C to the crystallization temperature, and if the niobium O#I composition ratio is low, it may be sf for several hours to 1 minute at 250°C to the crystallization temperature. .
又、加熱した恢デ冷等によって２乃至５時間和度Ｏ除冷
を行なうむとが好ましい。この際、飽和磁化に必要な数
０・乃至数１０００・の磁界を与えることが轡に望まし
い。Further, it is preferable to perform slow cooling using heating and cooling for 2 to 5 hours. At this time, it is desirable to apply a magnetic field of several 0 to several 1000, which is necessary for saturation magnetization.
本発明のスパッタ非晶質磁性材料は上述した如く優れた
軟磁性を持つか、この他に材料学的特性として横槍的性
質が良好であ〉且つ耐食性が高いという特長【有してい
る。即ちｔｌＩ４ｓ表において一例として００−Ｍｌ）
２元系の非晶質磁性材料Ｏ硬さｔ示すが、本発明Ｏ非
晶質磁性材＠０硬さはビッカース硬さ試験法で５２０乃
至１０２３ ｂ／−０極めて高い横槍的強度を有し、Ｍ
Ｔｓ ｉｉＯ増加とともに増加する性質を有する。The sputtered amorphous magnetic material of the present invention not only has excellent soft magnetism as described above, but also has other material properties such as good transverse magnetic properties and high corrosion resistance. That is, in the tlI4s table, as an example, 00-Ml)
The binary amorphous magnetic material has a hardness of t, and the amorphous magnetic material of the present invention has an extremely high horizontal strength of 520 to 1023 b/-0 according to the Vickers hardness test method. ,M
It has the property of increasing as Ts iiO increases.
次に本発明Ｏ非晶質磁性材料Ｏ耐食性について第２図に
基いて説明する。第２図は前述Ｏ方法によりゼ形成した
ａ３乃至α４−００Ｏ−１１１）非晶質磁性材料【基板
から剥離し良材料【一方Ｏ電極とし。Next, the corrosion resistance of the amorphous magnetic material of the present invention will be explained based on FIG. 2. Figure 2 shows a3 to α4-00O-111) amorphous magnetic material [material that can be easily peeled off from the substrate] formed by the O method described above [on the other hand, used as an O electrode].
Ｈｇ２０ｊ＠を他方Ｏ電極として１規定Ｏ塩酸中に浸漬
させ１両電極間に電圧を印加し、両電極間に不均一電流
が流れる電位を測定した結果【示す。Hg20j@ was immersed in 1N O hydrochloric acid using the other O electrode, a voltage was applied between the two electrodes, and the potential at which a non-uniform current flows between the two electrodes was measured. The results are shown below.
以上Ｏ結果によ〉本発明Ｏ非晶質磁性材料は塩素イオン
Ｏ存在によって通常見られる局部腐食０典麺である孔食
が着しく抑制され、耐食性か極めて良好であることか判
る。From the above results, it can be seen that the presence of chlorine ions in the amorphous magnetic material of the present invention significantly suppresses pitting corrosion, which is usually seen as localized corrosion, and has extremely good corrosion resistance.
更に、一般に非晶質材料は一種の凍結された準安定状Ｉ
ＩＩＫあるため、特定の温度で結晶化してしまうことが
知られてお〕、この温度が高い１安定性が高く、又キエ
ーリ一点も高い和安定な磁気特性を得ることがで龜るが
、第１表に示す如く本発明Ｏ非晶質磁性材料はこれらの
温度が極めて高く安定して良好な磁気特性を得ることが
可能である。Furthermore, amorphous materials are generally a kind of frozen metastable state I
IIK, it is known that it crystallizes at a certain temperature], and the higher this temperature is, the higher the stability is, and the higher the Chieri point is, the more stable the magnetic properties can be obtained. As shown in Table 1, the amorphous magnetic material of the present invention has extremely high temperatures and is capable of stably obtaining good magnetic properties.
以上の説明においては主ｆｃ Ｇｏ−Ｍｂ を元系Ｏ非
晶質磁性材料にりいて述べ良が、本発明の非晶質磁性材
料ＫＦ１種々の第５元素を添加してもよい、こｔ）第５
元素の例としては例えば主に磁歪を変化させる元素とし
て〒ｉ、 Ｚｒｅ Ｈｌｍ Ｖａ テａ＃Ｏｕ
、Ｍｏ 及びＶａどかあシ、又主に飽和磁化を変化さ
せる元素としてＣτ、Ｍｎ、］Ｉｉ及び１・などがあ）
、更に主に非晶質構造【形成させること動春易とするえ
めＯ元素として、Ｂ、０，８１゜Ｆ ＊ Ｇｏ ＊ ａ
ｎ ＊ Ｘｎ ｅム一及び８’Ｆ などがあシ。In the above explanation, fc Go-Mb is mainly described as an element O amorphous magnetic material, but various fifth elements may be added to the amorphous magnetic material KF1 of the present invention. Fifth
Examples of elements that mainly change magnetostriction include 〒i, Zre Hlm Va Tea#Ou
, Mo and Va, and elements that mainly change the saturation magnetization include Cτ, Mn, ]Ii and 1)
, and mainly as an amorphous structure [O element that facilitates the formation of B, 0.81°F * Go * a
n*Xn em and 8'F etc. are available.
これらは単独にあるいは組合せて用いられる。本発明の
非晶質磁性材料が負の比較的小さな磁歪【示すことから
好ましくは磁歪【正の方向に変化させ且つ飽和磁束密ａ
ｔ低下させないν・、ＭｎＯ少なくともいずれか一方の
元素を含むもＯであることが量も好ましい。又、本発明
００ｏ−Ｍｂ系材料はＢ４０半金属元素を含有しなくと
４非晶質構造をと）得ることから、これらＯ元素を含有
しない材料とすることが好ましい。These may be used alone or in combination. Since the amorphous magnetic material of the present invention exhibits relatively small negative magnetostriction, it is preferable that the magnetostriction be changed in the positive direction and the saturation magnetic flux density a
It is preferable that the amount is O, which contains at least one of the elements ν· and MnO, which does not lower the t. Furthermore, since the 00o-Mb-based material of the present invention has an amorphous structure unless it contains the B40 metalloid element, it is preferable to use a material that does not contain these O elements.
本発明Ｏ非晶質磁性材料に上記の第１元素を添加した結
果について第２ＩＩＫ示す。ζＯ結果から第３元素【添
加した本発明０３元系非晶質蟲性材料Ｏ飽和磁化及び飽
和磁束＊度は上記した２元系非晶質磁性材料に比べて磁
気特性が羨化し、飽和磁束＊度が改善されている仁とが
判る。The results of adding the above-mentioned first element to the amorphous magnetic material of the present invention are shown in 2nd IIK. From the ζO results, the third element [added to the ternary amorphous material of the present invention] saturation magnetization and saturation magnetic flux *You can see that the level has improved.
以上第１１１及び第を表に示した結果に基づいて本発明
００ｏ−１１１系非晶質磁性材料はコノ（ルトを主体と
し、ニオブを最大４０ｊｌ子−含む４０であれば喪好な
軟磁性を示すことが判った。又、現在集用されているヘ
ッド材料として最高Ｏ飽和磁束密度を持つセンダス）０
飽和磁束密度がα！キロガウスであることから見て上記
Ｏ如くコノ（ルト【主体とし、ニオブを４０原子−以下
、特に好ましくは５０７［子−以下含む二元系非晶質磁
性材料は十分に実用化しうる材料でＴｏシ、更に第２表
に示す如くこれに第１元素を加えることによ）飽和磁束
書皺を大巾に改曹しうるＯで、上記のコバルトを主体と
し、ニオブ（４０原子−以下、４１に好壕しくはＳＯ＠
子慢以下含む非晶質磁性材料は容易に極めて高い磁束密
度のものを得る仁とが可能となる。Based on the results shown in Tables 111 and 111 above, the 00o-111 series amorphous magnetic material of the present invention is mainly composed of Kono(rut) and contains up to 40 g of niobium, exhibiting poor soft magnetism. It was found that Sendas)0 has the highest O saturation magnetic flux density among currently used head materials.
Saturation magnetic flux density is α! Considering that it is a kilogauss, the binary amorphous magnetic material containing 40 atoms or less of niobium, particularly preferably 507 atoms or less, as mentioned above, is a material that can be fully put to practical use. (by adding the first element to it as shown in Table 2), the saturation magnetic flux wrinkles can be greatly improved. O is mainly composed of the above cobalt, and niobium (40 atoms or less, 41 The best place to go is SO@
Amorphous magnetic materials containing less than 100% of the magnetic flux can easily have extremely high magnetic flux densities.
以上詳細に説明し九通シ、本発明は軟磁気特性か嵐く、
機械的、化学的性質が喪いＯで、例えば磁気ヘッド材料
、低周波及び高周波トランス、磁気増幅器及び磁気フィ
ルターとしてＯ実用性が大きく、ｌ！にその組成によ）
キエーリ一点が変化することから熱セン賃としても用い
ることが可能である。Having explained in detail above, the present invention has soft magnetic properties,
It has good mechanical and chemical properties, and has great practicality as, for example, magnetic head materials, low-frequency and high-frequency transformers, magnetic amplifiers, and magnetic filters. (depending on its composition)
Since Chieri's single point changes, it can also be used as a heat sensor.
鯖２表 ｉｐ2 tables of mackerel ip
第１１！！ｌは本実Ｉ１４のスパッタ非晶質磁性材料【
作成する装置Ｏ概略断面図、第ｚｇは本発明のスパッタ
非晶質材料Ｏ耐食性を示すグラフである。
第１９１１中、１は容器、！はカンード、Ｓは７ノ（ほ
か５名）
１Ｂ１図
さ
第 ２ 図
Ｎｂ （原３Ｉ−％）
手続補ＩＩ：、書
１Ｍ４Ｆｉｌ ５９ ｊＮ ５ 月＋＞６日ｌ 中性
の表小
＋１１（４１１５７４＃特許願第２８０６４ 月２
ヅこ明の名称
スノ々ツタ非晶質磁性材料及びその製造方法３、補正を
する者
小（１，との関係：特許出願人
代名藤ａ啓安
霞が関ヒル内郵便局 私書箱第４９号
７ 補正の対象
明 細 書
１、発明の名称
ス／４ツタ非晶質磁性材料及びその製造方法！４１１許
請求の範囲
１）′３ノζルトを主体とし、ニオブを４０原子・セー
セント以下含むことを特徴とするス・々ツタ非晶質磁性
材料。
２） コノでルトな主体とし、二オシを４０原子パーセ
ント以下含み、更にチタン、ジルコニウム、ハフニウム
、バナジウム、メンタル、鋼、モリブデン、タングステ
ンから成る群から選ばれた少なくともＬ種の追加的元素
を含むことＶ＊黴とする特許請求の範囲第１項記載？ス
パッタ非晶質磁性材。
科。
３）；パルトを主体とし、ニオブを４０原子ノ々−セン
ト以下含み、更にクロム、マンガン、ニッケル、鉄から
成る群から選ばれた少なくとも１種の追加的元素を含む
ことを特徴とする特許請求の範囲第１項記載のスＪツタ
非晶質磁性材料。
４） コノセルトを主体とし、二オシを４０原子、Ｒ−
セント以下含み、更にほう素、炭素、けい素、リン、ゲ
ルマニウム、すす、インジウム、ひ素、アンチ千ンから
成る群から選ばれた少くとも１１１の追加的元素を含む
ことを特徴とする特許請求の範囲Ｗ、１項記献のスパッ
タ非晶質磁性材料。
５）コノＺルトな主体とし、ニオブを４０１［子）（−
セント以下含み更に鉄及びマンガンからなる群から選ば
れた少くとも１種の追加的元素を含むことを特徴とする
特許請求の範囲第３項記載のスパッタ非晶質磁性材料。
６）コノ硬ルトを主体とし、ニオブを４０原子ノで一セ
ント以下含むスパッタ非晶質磁性材料を結晶化温度以下
の温度で熱処理することを特徴とするスパッタ非晶質磁
性材料の製造方法。
３、発明の詳細な説明
本発明はスパッタ非晶質磁性材料及びその製造方法に関
するものであり、特に飽和磁束密度が大きく、保磁力及
び磁歪が小さい軟磁気特性が優れたス・碇ツタ非晶質磁
性材料及びその製造方法に関するものである。
ス／々ツメリング法を用いて得たスパッタ非晶質磁性材
料が知られている。このようにして得られた非晶質磁性
材料は、結晶磁性材料の如き規則的原子配列なとること
なく長周期的構造を持たず。
原子配列が無秩序な材料であることから、結晶磁気異方
性がなく良好な軟磁気特性を示す材料である。
またこのスパッタ非晶質磁性材料はガス状態の金属を凝
集させること、すなわち気体から直接固体を形成させる
ような一種の凍結作用によって得られた非晶質材料であ
るから、ｉ！融状Ｉｌにある磁性材料を射出し、これを
高速回転するドラムＫｍ触させて急冷して、非晶質磁性
材料リボンを形成する超急冷法によつ【得られたものに
比べて極めて薄い腰を得ることができるなどのＩＩｆＩ
像点を有し【いる、更に上記の超急冷法においては＃Ｉ
−状態にあや磁性材料に更にホウ素、シリコンなどの非
磁性元素を含有していない限り非晶質磁性材料が形成さ
れないのに対し、スノツタリング法においてはかかる元
素を加えなくても非晶質磁性材料な形成することができ
ることから１両プロセスによって得られた材料は本質的
ＫＭなる材料であると言える。
本発明は新規なスパッタ非晶質磁性材料及びその製造方
法を提供せんとすることを目的とする。
本発明は、コノ２ルトを主体とし、ニオブを４０原子・
セーセント以下含むことを特徴とするスパッタ非晶質磁
性材料であり、更にコノ層ルトな主体とし、ニオブを４
０１−７−７々−セント以下含む非晶質磁性材料を結晶
化温度以下の温度で熱処理することを特徴とするスパッ
タ非晶質磁性材料の製造方法である。
更に本発明の１つの態様はコバルトを主体とし。
ニオブｖ４０原子ノーセント以下含み、更にチタン、ジ
ルコニウム、ハフニウム、パナジクム、タンタル、鋼、
モリブデン、タングステンから成る群から選ばれた少な
（ともｌｌｌの追加的元素を含むことを特徴とするスパ
ッタ非晶質磁性材料であり、又本発明の他の態様はコ、
１ルトを主体とし、二オシを４ＯＮ［子パーセント以下
含み、更にクロム、マンガン、ニッケル、鉄から威る群
から選ばれた少なくともｌｓの追加的元素を含むことな
特徴とするス・（ツタ非晶質磁性材料であり、本発明の
他のａＩＩＩｌはコバルトを主体とし、ニオブｖ４０原
子〕（−セント以下含み、更Ｋｆｉｊ素、炭素、けイ素
、リン、ゲルマニウム、すず、ベンジ９ム。
ひ素、アンチモンから成る群から選ばれた少なくとも１
種の追加的元素を含むことを特徴とするスパッタ非晶質
磁性材料であり、更に本実町の他のｉ＊＊はコバルトを
主体とし、ニオブを４０原子・セーセント以下含み、更
に鉄及びマンガンから成る群から選ばれた少くとも１種
の追加的元素を含むことを＊＊とするスパッタ非晶質磁
性材料である。
次に本発明のスパッタ非晶質磁性材料を製造する方法の
一例につい【第１図を参照して説明する。
第１図は本発明のスパッタ非晶質磁性材料を製造するた
めの装置の一例を示す概略断面図である。
第１図において、容器１内は約１０ Ｔｏｒｒの９
９．９９％Ａｒガス雰囲気に保たれている。容６１への
Ａｒ ガスの導入は例えば１０−”Ｔｏｒｒ Ｋ予備
排気された後に行なわれ１０−”Ｔｏｒｒの真空に保た
れる。２及び３はそれぞれタングステンフィラメント及
びステンレス板によって構成されているカソード及びア
ノード９であり、これらの間には電源４によって約１０
Ｖ、４０Ａ程度の電圧、電流が印加され容器１中にプラ
ズマを発生させる。ここでアノード３は水冷され更に電
源５により”ｔ” １００Ｖ以下程度の直流正電圧が印
加されてもよい、６はターゲット電極であり、少なくと
もコノ２ルト及びニオブを含む材料が設置されており、
水冷されている。このターゲット電極６には電源７によ
って０〜１５００Ｖ程度の負電圧が印加されている。
８は本発明の非晶質磁性材料をデゼジットするための基
板であって水冷され、更に電源９によって最大５００Ｖ
程度の負電圧が印加されてもよい。
本発明の非晶質磁性材料は上記カソード９２及び・７ノ
ード３との間に約ＩＱＶ、４０Ａの電圧電流を印加しプ
ラズマを発生させ、プラズマ中に発生したイオンを１〜
２ＫＶＣ最大約３００ｍム） の強い電界で加速し、タ
ーゲット電極６をスパッタして構成原子を放出させ、こ
れ１基板８上に付着。
堆積させることＫよって得られる。この様にして３日間
の連続スノ々ツタによって厚さ約２００μ肥の非晶質磁
性材料を得ることができた。
次にこのＩＩＫして作った本発明の非晶質磁性材料につ
いて、実験した結果について第１表及び第２表に基いて
説明する。第１表及び第２表は上述の如き製法により基
板上に非晶質磁性材料を付着させて、厚さ０．２ｍ、直
径４０謔の円盤状試料及び外径３０ｍ、内径２０■のリ
ング状試料をそれぞれ作成し、これらの磁気分析、磁化
曲線の測定、示差熱分析、硬さ試験及び分極曲線の測定
をそれぞれ行ない、その試料の軟磁気特性、熱的安定性
。
機械的性質及び耐食性について調べた結果を示すもので
ある。
なお、このようにして作成した磁性材料が非晶質構造を
示すことの判定はターゲットとし″ＣＦｅ。
Ｋａ線を用い、ｘ！１回折線を測定することによって行
なった。その結果第１表及び第２表に示す試料のＸ６回
折線は２〜３の散慢な回折リングのみシ示し、結晶のよ
うな鋭い回折線な示さず、これらが非晶質構造となって
いることが明らかとなった。
第１表はコｊルト及び二オシの組成を種々変化させて作
った本発明のスパッタ非晶質磁性材料の室温における飽
和磁化、ｆＩｓ和磁束密度、磁歪、保磁力、硬さ、結晶
化温度及びキューリ一点をそれぞれ示す、第１表におい
て飽和磁化及び飽和磁束密度はニオブの含有率が低い程
（二元系におい【はコバルトの含有率が高い程）高い値
を示す、又。
磁性材料として高い飽和磁束密度と共に優れた軟磁性を
示すためには磁気ひずみ（磁歪）が小さい事が必要であ
るが１本発明のスパッタ非晶質磁性材料は磁歪がいずれ
も負の比較的小さな値を示す。
本発明のスパッタ非晶質磁性材料の大きな特徴点の１つ
は磁歪が比較的小さな値を示し、更にその値が負である
点にある。即ち、近年半金属元素を含まない０〇−系非
晶質磁性材料（Ｃｏ−Ｔｉ、 Ｚｒ。
Ｈｆ、 Ｔａ、 Ｗ）が優れた軟磁性特性を示すこと
で注目され発表がなされている。これらのうちＯＯ−丁
１系、Ｇｏ−Ｚｒ系及びＣｏ−Ｈｆ系非晶質磁性材料は
磁歪が正の値を示す材料であるから、この磁歪な実質的
に零にするためには例えばＮ１．Ｍｏ及びＯｒを加えな
ければならないが、このような元素は磁性材料の飽和磁
束密度を減少させてしまう。
一方Ｃｏ−Ｔａ系及びＣｏ−Ｗ系非晶質磁性材料は磁歪
が負であることから例えばＦｅ、Ｍｎ ｋ加えて磁歪を
実質的に零にすることができ、更にこれらの元素は磁性
材料の飽和磁束密度を増加させるか少なくともはとんと
低下させないので良好な非晶質磁性材料であると言える
が、かかるＣｏ−Ｔａ系及びＧｏ−Ｗ系非晶質磁性材料
においても本発明のＣｏ−Ｎｂ系非晶質磁性材料に比し
て低い飽和磁束密度のものが得られるに過ぎない、即ち
本発明の非晶質磁性材料は例えば後述する第２表の試＠
ム１８ （ＯＯｕ、５Ｆｆ３４．５Ｎｂｔｏ ） Ｋ示
す如＜ａ歪が実質的に零で、１２乃至１３キロガウス以
上の極めて大きな飽和磁束密度を有する材料を作成する
ことができる。
従って本発明で最も好ましい非晶質磁性材料ゆコバルト
を主体とし、ニオブな４０原子／セーセント月下含み、
更に鉄、マンガンの少なくともいずれか一方の追加的元
素な磁歪が実質的に零となる量含むものであり、この追
加的元素の量は１例えば（Ｏｏｌ−エμｎｚ）８ｊＮｂ
１５の組成の非晶質磁性材料においてはＸが０．０２か
ら０．０６の値にあることがよく、又、（Ｇｏ、−ｘＦ
ｅｗ）ａｓＮｂｘｉあるいはＣＣＪ、１３−ＪｅＸ Ｎ
ｂ１ｇ、１６ノ組ｆｉｌｌ）非＆’ｌｉｍ性材料Ｋｍい
てはＸが０．０１から０．０３の値にあることがよ（１
゜
又、ホウ素などの非晶質構造を形成することを容易とす
るための元素を添加したときの飽和磁束密度の低下及び
磁歪の変化を考慮すれば１本発明の非晶質磁性材ＩＮＫ
はこれらの元素を含まないことが好ましい。
本発明のスーぞツタ非晶質磁性材料ＫＩＬ［求される軟
磁性の目安として保磁力は重要な性質であり。
この保磁力ができる限り小さいことが要求されるが、本
発明のスパッタ非晶質磁性材料は第１表に示す如く、比
較的に良好な値を示す、又この保磁力は第３表に示す如
く適当な条件での加熱処ｌＪＫより更に小さくすること
ができる。即ち、第３表に示す如く、試料４３ （ＣＯ
ｓｓ、５Ｎｂｔｔ、−の組成における熱処理しない場合
の保磁力は１８０ ｍ（ｌｅの値を示すが、＃！３表に
示す各温度で３０分熱処理することによって更に小さな
保磁力となることが判る０例えば３６０℃の温度で熱処
理したとｆ！１３５ ｍ０６．４００℃の温度で熱処理
したときＫは３０ ！ＤＯ・の極めて低い値な示す。
本発明における熱処理の条件は少なくとも非晶質磁性材
料を結晶化温度以下の温度で熱処理することが必要であ
るが、ニオブの組成比が高い場合には比較的低温の熱処
理で効果を生じるがニオブの組成比が低い場合には比較
的高温の熱処理を必要とする。即ちこの熱処理温度はニ
オブの組成比が高い場合１５０℃乃至結晶化温度で数時
間乃至１分根！、 ニオブの組成比が低い場合には２５
０℃乃至結晶化温度で数時間乃至１分根度でよい。
又、加熱した後炉冷等によって２乃至３時間程度の除冷
を行なうことが好ましい、このａ、飽和磁化に必要な数
Ｏｅ乃至＃ｊ１０００ｇの磁界を与えることが％に箇ま
しい。
本発明のスパッタ非晶質磁性材料は上述した如く督れた
軟磁性を持つが、この他に材料学的特性として機械的性
質が良好であり且つ耐食性が高いという特長を有してい
る。即ち第３表において一例としてＧｏ−Ｎ、ｂ ２元
系の非晶質磁性材料の硬さを示すが、本発明の非晶質磁
性材料の硬さはビッカース硬さ試験法で５２０乃至１０
２３％Ｃｌ ／ ｍ ”の極めて高い機械的強度を有し
、Ｎｂ量の増加とともに増加する性質を有する。
次に本発明の非晶質磁性材料の耐食性について第２図に
基いて説明する。第２図は前述の方法によって形成した
０、３乃至０，４ＲのＣｏ−Ｎｂ非晶質磁性材料な基板
から剥離した材料を一方の電極とし、ＨｇｘＣ４ｘ ｔ
’他方の電極としてｌ規定の塩酸中に浸漬させ１両電極
間に電圧を印加し、両電極間に不均一電流が流れる電位
を測定した結果を示す。
以上の結果により本発明の非晶質磁性材料は塩素イオン
の存在によって通常見られる局部腐食の典型である孔食
が著しく抑制され、耐食性が極め【良好であることが判
る。
更に、一般に非晶質材料は一種の凍結された準安定状態
にあるため、＊定の温度を結晶化してしまうことが知ら
れており、この温度が高い程安定性が高く、又キューリ
一点も高い程安定な磁気特性を得ることができるが、第
１表に示す如く本発明の非晶質磁性材料はこれらの温度
が極めて高く安定して良好な磁気特性を得ることが可能
である。
以上の説明においては主にＧｏ−Ｎｂ ２元系の非晶質
磁性材料について述べたが、本発明の非晶質磁性材料に
は種々の第３元素を添加してもよい。
この第３元素の例としては例えば主に磁歪な変化させる
元素としてＴｉ、Ｚｒ、ＨらＶ、ＴａｔＧｕ、Ｍ。
及びＷなどがあり、又主に飽和磁化を変化させる元素と
しＣＣｒ、ｂ
更に主に非晶質構造を形成させることを容易とすルタ１
６１’＞元素として、Ｂｏｏ、Ｓｔ、Ｐ、Ｇｏ、Ｓｏ。
Ｉｎ、ＡＩ及びＳｂなどがあり、これらは単独にあるい
は組合せて用いられる０本発明の非晶質磁性材料が自の
比較的小さな磁歪な示すことから好ましくは磁歪を正の
方向に変化させ且つ飽和磁束密度を低下させないｉ’ｅ
、Ｍｎの少なくともいずれか一方の元素を含むものであ
ることが最も好ましい。
同ＩＩＫ少量の添加で磁歪な正の方向に変化させること
ができるＺｒ、Ｉｆの少なくともいずれか一方の元素を
含むものも好ましい、又、本発明のＣ。
−Ｎｂ系材料はＢ等の非晶質構造を形成することを容易
とする元素を含有しなくとも非晶質構造をとり得ること
から、これらの元素を含有しない材料とすることが好ま
しい。
本発明の非晶質磁性材料に上記の第３元素を添左した結
果について第２表に示す、この結果から第３元素を添加
した本発明の３元系非晶質磁性材料の飽和磁化及び飽和
磁束密度は上記した２元系非晶質磁性材料に比べて磁気
特性が変化し、飽和磁束密度が改善されていることが判
る。
更Ｋｔｌ！、４ｆ？にオイテ、ＣＣ；ｏ１−ＩＭｘ）、
、Ｗｂｌ、ｒ＞Ｍ成の非晶質磁性材料の−としてＦｅ、
Ｍｎを用い、９！ＫＸｖ値を種々変化させた場合の飽和
磁化及び磁歪なそれぞれ示す。更にこの第４表にはＵと
してＮ１．Ｔｉ を用いた場合についても示している。
第４表の結果から明らかな如く、上記の組成の非晶質磁
性材料においてＵとしてＦｅ、Ｍｎを適当量加えるとと
Ｋよって飽和磁化及び磁歪な著しく改善することができ
る０例えば、それぞれ磁歪が極めて小さな値を示す試料
、４２６．３２．３７及び３８を比較すれば明らかな如
く、試料Ａ６２６．３２が大きな飽和磁化の値を示すこ
とがわかる。
このような３元系の非晶質磁性材料においても、上述し
た２元系の非晶質磁性材料と同様に加熱処理により保磁
力を更に小さくすることができる。
即ち、前述と同様和して各種の組成の非晶質磁性材料を
外径２５ｗａ＋φ、内径１５■φ、厚さ０．３簡のリン
グ状に形成した試料の飽和磁束密度及びこれを回転数３
５０回／分、１０００・の磁場の回転磁場中で４００℃
、３０分熱処理した後、除冷した時の熱処理前及び熱処
理後の保持力を第５表に示す、この表から明らかな如（
、これら各種り）非晶質磁性材料は熱処理によって保持
力が著しく改良されることが判る。
更にこの加熱処理においては、第３図に示す如（、加熱
処理温度が高くなるに従って保磁力が改良され、更にこ
の加熱を磁場の存在下で行なうことＫより、磁場の存在
しない条件下で加熱を行なう場合に比して更に著しく保
磁力が改良されることが判る。
次に前記と同様な手段によってサファイア単結晶基板（
８面）Ｋｌ［厚５．７００ＡのＣｏ□、−・２．。
Ｎｂ１＠、５の組成の非晶質磁性材料を形成したもの（
試料層４５）及び膜厚１１５０ ＧＡ ｔ＞ Ｇｏ、、
、、Ｆｅ、５Ｎｂ、。
の組成の非晶質磁性材料を形成したもの（試料ム４６）
な準備し、これｖ＃Ｉ定磁界（Ｈｍ ）を１００ ｅ
５５０Ｈ２の条件下でその磁気特性を測定した結果を第
６表に示す、この表から明らかな如（、その組成比によ
って大きくその磁気特性も変化し、この例では試料層４
５の組成の非晶質磁性材料が試料Ａ４６の非晶質磁性材
料よりも更に好ましい磁気特性を示している。
史に本発明の非晶質磁性材料はその結晶化温度以下の温
度で熱処理するととにより、前述の如く保磁力を改良で
きると共に異方性磁界（Ｈｋ）をも改良することができ
る。これを試料層４５の非晶質磁性材料を各種の温度で
熱処理した例を第７表に示す、この表から明らかなよう
に熱処理な行なうことによって異方性磁界を更に改良で
きることが明らかである。
以上第１表乃至第７表、及び第２図、第３図に示した結
果に基づいて本発明のＧｏ−Ｎｉ 系非晶質磁性材料は
コバルトを主体とし、ニオブを最大４０原子％を含むも
のであれば良好な軟磁性を示すことが判った。又、現在
実用されているヘッド材料として最高の飽和磁束密度な
持つセンダストの飽和磁束密度が０．９キロガウスであ
ることから！て上記の如くコノｔルトを主体とし、ニオ
ブを４ＯＮ子％以下、特に好ましくは３０原子シ以下含
む二元系非晶質磁性材料は十分に実用化しさる材料であ
り、更に第２表に示す如くこれに第３元素を加えること
Ｋより域領磁束密ｌｔす大巾に改梼し与るので、上記の
コバルトを主体とし、ニオノを４０原子シ以下、％に好
ましくは３０原子％以下含む非晶ｗ磁性材料は容易に極
めて高い磁束密ｉのものを得ることが可能となる。
以上鮮細に説明した通り１本発明は軟磁気特性が良＜、
ＷＡ械的、化学的性質が良いので、例えば磁気ヘット０
材料、低周波及び高周波トランス、磁気増幅器及び磁気
フィルターとしての実用性が大きく、更にその組成によ
りキエーリ一点が変化することから熱センサとしても用
いることが可能である。
第２表
第３１Ｉ
第４
第 ・ 表
第 １＊
４、図面の簡単な説明
第１１１は本発明のスパッタ非晶質磁性材料を作成する
装Ｎｆ１概略断画図、第２図は本発明のス２ツタ非晶質
材料の耐食性を示すグラフ、第ＢＷＪは本発明のスノ臂
ツタ非晶質材料の加熱処ｉｌ！による効果を示すグラフ
である。
亀１１１１１１１．０！容Ｉ１．２ｋｔｔｌ：／−￥、
３４１７／−ド、４，５，７．９は電源、６はターゲ
ット電番、８は基鈑である。
（嫌か３名） 学
１３Ｗｉ
熱廻理清膚Ｔａ（’Ｃ）11th! ! l is the sputtered amorphous magnetic material of Honjitsu I14 [
In the schematic cross-sectional view of the apparatus O to be produced, zg is a graph showing the corrosion resistance of the sputtered amorphous material O of the present invention. Of the 1911th, 1 is a container! is Kando, S is 7 (and 5 others) 1B1 Figure 2 Figure 2 Nb (Original 3I-%) Procedure Supplement II:, Book 1M4Fil 59 jN May + > 6th l Neutral table small + 11 (411574# Patent Application No. 28064/2
Name of Tsuko Akira: Suno Tsuta Amorphous Magnetic Material and Manufacturing Method 3, Person Making Amendment (1) Relationship with Patent Applicant Name: Fuji A Keiyasu Kasumigaseki Hill Post Office P.O. Box No. 49 No. 7 Amendment Description of the subject matter 1, Title of the invention S/4 Ivy amorphous magnetic material and method for producing the same!411 Claims 1) '3-north ζ-olt as a main component and containing niobium at 40 atoms secent or less Features: Amorphous magnetic material. 2) Contains not more than 40 atomic percent of nitrogen, and further contains at least L additional elements selected from the group consisting of titanium, zirconium, hafnium, vanadium, mental, steel, molybdenum, and tungsten. Is the claim 1 stating “V*mold”? Sputtered amorphous magnetic material. Department. 3); A patent claim characterized in that it is mainly composed of Palt, contains 40 or less atomic cents of niobium, and further contains at least one additional element selected from the group consisting of chromium, manganese, nickel, and iron. Scope of the invention The amorphous magnetic material according to item 1. 4) Mainly Conocerto, 40 Niosi atoms, R-
and at least 111 additional elements selected from the group consisting of boron, carbon, silicon, phosphorus, germanium, soot, indium, arsenic, and antisulfur. Range W, sputtered amorphous magnetic material described in item 1. 5) Let niobium be the main subject and 401 [child) (-
4. The sputtered amorphous magnetic material according to claim 3, further comprising at least one additional element selected from the group consisting of iron and manganese. 6) A method for producing a sputtered amorphous magnetic material, which comprises heat-treating a sputtered amorphous magnetic material which is mainly made of niobium and contains 40 atoms or less of niobium at a temperature below the crystallization temperature. 3. Detailed Description of the Invention The present invention relates to a sputtered amorphous magnetic material and a method for manufacturing the same, and in particular to sputtered amorphous magnetic materials, which have excellent soft magnetic properties such as high saturation magnetic flux density, low coercive force and small magnetostriction. The present invention relates to highly magnetic materials and methods of manufacturing the same. Sputtered amorphous magnetic materials obtained using the sputtering method are known. The amorphous magnetic material thus obtained does not have a regular atomic arrangement unlike a crystalline magnetic material and does not have a long periodic structure. Since it is a material with a disordered atomic arrangement, it has no crystal magnetic anisotropy and exhibits good soft magnetic properties. Moreover, since this sputtered amorphous magnetic material is an amorphous material obtained by agglomerating metal in a gaseous state, that is, by a kind of freezing effect that directly forms a solid from a gas, i! The magnetic material in the molten state is injected, brought into contact with a high-speed rotating drum Km, and rapidly cooled to form an amorphous magnetic material ribbon. IIfI can get waist
Furthermore, in the ultra-quenching method described above, #I
- While an amorphous magnetic material cannot be formed unless the magnetic material further contains non-magnetic elements such as boron or silicon, in the snottering method, an amorphous magnetic material can be formed even without the addition of such elements. It can be said that the material obtained by this process is essentially a KM material. An object of the present invention is to provide a novel sputtered amorphous magnetic material and a method for manufacturing the same. The present invention mainly consists of niobium, with 40 atoms of niobium.
It is a sputtered amorphous magnetic material characterized by containing less than 100% of niobium.
01-7-7 A method for producing a sputtered amorphous magnetic material characterized by heat-treating an amorphous magnetic material containing less than 7 cents at a temperature below the crystallization temperature. Further, one embodiment of the present invention mainly contains cobalt. Contains less than 40 atoms of niobium, as well as titanium, zirconium, hafnium, panazicum, tantalum, steel,
Another aspect of the present invention is a sputtered amorphous magnetic material characterized by containing a small amount of additional elements selected from the group consisting of molybdenum, tungsten,
It is characterized by containing 1 rut as the main ingredient, 4 on % or less of 2 nitrate, and further containing at least ls of additional elements selected from the group consisting of chromium, manganese, nickel, and iron. The other aIII of the present invention, which is a crystalline magnetic material, is mainly composed of cobalt, niobium v40 atoms] (including less than -cent, and further contains Kfij elements, carbon, silicon, phosphorus, germanium, tin, benzene9 atoms, arsenic , at least one selected from the group consisting of antimony
It is a sputtered amorphous magnetic material characterized by containing additional elements of species, and Honji Town's other i** is mainly composed of cobalt, contains less than 40 atoms/sec of niobium, and further contains iron and manganese. A sputtered amorphous magnetic material containing at least one additional element selected from the group consisting of **. Next, an example of a method for manufacturing the sputtered amorphous magnetic material of the present invention will be described with reference to FIG. FIG. 1 is a schematic cross-sectional view showing an example of an apparatus for producing the sputtered amorphous magnetic material of the present invention. In Figure 1, the inside of container 1 is approximately 10 Torr.
A 9.99% Ar gas atmosphere is maintained. The introduction of Ar gas into the chamber 61 is carried out after preliminary evacuation of, for example, 10-'' Torr, and the chamber 61 is maintained at a vacuum of 10-'' Torr. Reference numerals 2 and 3 denote a cathode and an anode 9, each composed of a tungsten filament and a stainless steel plate.
A voltage and current of approximately V and 40 A are applied to generate plasma in the container 1. Here, the anode 3 is water-cooled, and a direct current positive voltage of about 100 V or less "t" may be applied by a power source 5. 6 is a target electrode, and a material containing at least Conolite and niobium is installed.
It is water cooled. A negative voltage of about 0 to 1500 V is applied to this target electrode 6 by a power source 7. Reference numeral 8 denotes a substrate for digitizing the amorphous magnetic material of the present invention, which is water-cooled and is further supplied with a power supply of up to 500 V by a power source 9.
A relatively negative voltage may be applied. The amorphous magnetic material of the present invention generates plasma by applying a voltage current of approximately IQV and 40 A between the cathode 92 and the 7 node 3, and ions generated in the plasma are
The target electrode 6 is sputtered by accelerating with a strong electric field of 2 KVC (maximum approximately 300 mm) to emit constituent atoms, which adhere to a substrate 8. Obtained by depositing K. In this way, it was possible to obtain an amorphous magnetic material with a thickness of about 200 μm by continuously cultivating it for 3 days. Next, the results of experiments conducted on the amorphous magnetic material of the present invention produced by IIK will be explained based on Tables 1 and 2. Tables 1 and 2 show disk-shaped samples with a thickness of 0.2 m and a diameter of 40 cm, and ring-shaped samples with an outer diameter of 30 m and an inner diameter of 20 cm, prepared by depositing an amorphous magnetic material on a substrate using the manufacturing method described above. Each sample was prepared and subjected to magnetic analysis, magnetization curve measurement, differential thermal analysis, hardness test, and polarization curve measurement to determine the soft magnetic properties and thermal stability of the sample. This shows the results of an investigation into mechanical properties and corrosion resistance. The determination that the magnetic material produced in this way exhibits an amorphous structure was made by measuring the x!1 diffraction line using Ka radiation as a target of "CFe".The results are shown in Table 1 and The X6 diffraction line of the sample shown in Table 2 shows only 2 to 3 scattered diffraction rings and no sharp diffraction lines like crystals, making it clear that these have an amorphous structure. Table 1 shows the saturation magnetization, fIs sum magnetic flux density, magnetostriction, coercive force, hardness, and crystallinity at room temperature of the sputtered amorphous magnetic materials of the present invention made by varying the composition of Colt and Niosci. In Table 1, which shows the magnetization temperature and Curie point, respectively, the saturation magnetization and saturation magnetic flux density show higher values as the niobium content is lower (in a binary system [and the cobalt content is higher)]. In order for a material to exhibit high saturation magnetic flux density and excellent soft magnetism, it is necessary to have a small magnetostriction (magnetostriction).1 The sputtered amorphous magnetic material of the present invention has a relatively small magnetostriction that is negative in both cases. One of the major features of the sputtered amorphous magnetic material of the present invention is that the magnetostriction exhibits a relatively small value, and furthermore, this value is negative. 〇-based amorphous magnetic materials (Co-Ti, Zr, Hf, Ta, W) have attracted attention and have been published as exhibiting excellent soft magnetic properties. Among these, OO-T1-based and Go- Zr-based and Co-Hf-based amorphous magnetic materials are materials in which magnetostriction exhibits a positive value, so in order to make this magnetostriction substantially zero, it is necessary to add, for example, N1.Mo and Or. Such elements reduce the saturation magnetic flux density of the magnetic material.On the other hand, since the magnetostriction of Co-Ta and Co-W amorphous magnetic materials is negative, for example, Fe, Mnk may be added to substantially reduce the magnetostriction. Furthermore, these elements can be said to be good amorphous magnetic materials because they increase the saturation magnetic flux density of the magnetic material or at least do not significantly reduce it. Even in the case of the -W-based amorphous magnetic material, a saturation magnetic flux density lower than that of the Co--Nb-based amorphous magnetic material of the present invention can only be obtained. Tests in Table 2 below @
(OOu, 5Ff34.5Nbto) It is possible to create a material that has substantially zero strain and has an extremely large saturation magnetic flux density of 12 to 13 kilogauss or more. Therefore, the most preferred amorphous magnetic material in the present invention is mainly composed of cobalt and contains less than 40 atoms/scent of niobium,
Further, it contains at least one of iron and manganese in an amount such that the magnetostriction is substantially zero, and the amount of this additional element is 1, for example (Ool-Eμnz)8jNb
In the amorphous magnetic material having the composition No. 15, X often has a value of 0.02 to 0.06, and (Go, -xF
ew) asNbxi or CCJ, 13-JeX N
b1g, 16 sets fill) For non-&'lim material Km, X may have a value of 0.01 to 0.03 (1
゜Also, considering the decrease in saturation magnetic flux density and the change in magnetostriction when adding an element such as boron to facilitate the formation of an amorphous structure, the amorphous magnetic material INK of the present invention
preferably does not contain these elements. The smooth amorphous magnetic material KIL of the present invention [coercive force is an important property as a measure of the required soft magnetism. This coercive force is required to be as small as possible, and the sputtered amorphous magnetic material of the present invention shows relatively good values as shown in Table 1, and this coercive force is shown in Table 3. It can be made even smaller than that obtained by heat treatment under suitable conditions. That is, as shown in Table 3, sample 43 (CO
The coercive force without heat treatment in the composition of ss, 5Nbtt, - is 180 m (le value is shown, but it can be seen that the coercive force becomes even smaller by heat treatment for 30 minutes at each temperature shown in table #!3. For example, when heat treated at a temperature of 360°C, K shows an extremely low value of 30!DO· when heat treated at a temperature of 360°C. When the niobium composition ratio is high, heat treatment at a relatively low temperature produces an effect, but when the niobium composition ratio is low, a relatively high temperature heat treatment is required. In other words, the heat treatment temperature is 150°C to the crystallization temperature for several hours to 1 minute when the niobium composition ratio is high, and 25°C when the niobium composition ratio is low.
It may be incubated for several hours to one minute at 0°C to the crystallization temperature. Further, after heating, it is preferable to perform slow cooling for about 2 to 3 hours by furnace cooling or the like, and it is preferable to apply a magnetic field of several Oe to #j of 1000 g necessary for saturation magnetization. The sputtered amorphous magnetic material of the present invention has excellent soft magnetism as described above, but also has other material properties such as good mechanical properties and high corrosion resistance. That is, in Table 3, the hardness of the Go-N, b binary amorphous magnetic material is shown as an example, and the hardness of the amorphous magnetic material of the present invention is 520 to 10 according to the Vickers hardness test method.
It has an extremely high mechanical strength of 23%Cl/m'', and has the property of increasing as the amount of Nb increases.Next, the corrosion resistance of the amorphous magnetic material of the present invention will be explained based on FIG. 2. In Figure 2, one electrode is a material peeled from a 0,3 to 0,4R Co-Nb amorphous magnetic material substrate formed by the method described above, and HgxC4x t
``The other electrode is immersed in l-regulated hydrochloric acid, a voltage is applied between the two electrodes, and the potential of non-uniform current flowing between the two electrodes is measured.The results are shown below. The above results show that the presence of chlorine ions in the amorphous magnetic material of the present invention significantly suppresses pitting corrosion, which is typical of localized corrosion normally observed, and has extremely good corrosion resistance. Furthermore, since amorphous materials are generally in a kind of frozen metastable state, it is known that they crystallize at a certain temperature; The higher the temperature, the more stable the magnetic properties can be obtained, and as shown in Table 1, the amorphous magnetic material of the present invention can have these temperatures extremely high and stably obtain good magnetic properties. In the above description, the amorphous magnetic material of the Go--Nb binary system was mainly described, but various third elements may be added to the amorphous magnetic material of the present invention. Examples of the third element include Ti, Zr, H, V, TatGu, and M as elements that mainly change magnetostriction. and W, etc., and CCr, b, which is an element that mainly changes the saturation magnetization, and Ruta 1, which mainly facilitates the formation of an amorphous structure.
61'>Elements include Boo, St, P, Go, So. There are In, AI, Sb, etc., and these are used alone or in combination.Since the amorphous magnetic material of the present invention exhibits a relatively small magnetostriction, it is preferable to change the magnetostriction in a positive direction and to achieve saturation. i'e that does not reduce magnetic flux density
, Mn is most preferable. It is also preferable that IIK contains at least one of Zr and If, which can change the magnetostriction in a positive direction by adding a small amount, and C of the present invention. Since the -Nb-based material can have an amorphous structure without containing elements such as B that facilitate the formation of an amorphous structure, it is preferable to use a material that does not contain these elements. The results of adding the third element to the amorphous magnetic material of the present invention are shown in Table 2. From these results, the saturation magnetization and It can be seen that the saturation magnetic flux density is improved by changing the magnetic properties compared to the binary amorphous magnetic material described above. More Ktl! ,4f? Nioite, CC; o1-IMx),
, Wbl, Fe as - of the amorphous magnetic material with r>M composition,
Using Mn, 9! The saturation magnetization and magnetostriction are shown when the KXv value is varied. Furthermore, in this Table 4, N1. The case using Ti is also shown. As is clear from the results in Table 4, when appropriate amounts of Fe and Mn are added as U to an amorphous magnetic material having the above composition, K can significantly improve saturation magnetization and magnetostriction. As is clear from a comparison of samples 426.32.37 and 38, which show extremely small values, sample A626.32 shows a large saturation magnetization value. Even in such a ternary amorphous magnetic material, the coercive force can be further reduced by heat treatment, similar to the above-mentioned binary amorphous magnetic material. That is, the saturation magnetic flux density of a sample formed of amorphous magnetic materials of various compositions in the shape of a ring with an outer diameter of 25 wa + φ, an inner diameter of 15 φ, and a thickness of 0.3 mm, and the rotation speed of 3.
50 times/min, 400°C in a rotating magnetic field of 1000°
, Table 5 shows the holding power before and after heat treatment when slowly cooling after heat treatment for 30 minutes.
It can be seen that the coercivity of amorphous magnetic materials (of these various types) is significantly improved by heat treatment. Furthermore, in this heat treatment, as shown in Fig. 3, the coercive force is improved as the heat treatment temperature increases, and since this heating is performed in the presence of a magnetic field, it is possible to conduct heating in the absence of a magnetic field. It can be seen that the coercive force is further improved significantly compared to the case where the sapphire single crystal substrate (
8th side) Kl [Co□ with thickness 5.700A, -2. . An amorphous magnetic material with a composition of Nb1@, 5 (
Sample layer 45) and film thickness 1150 GA t> Go,,
,,Fe,5Nb,. (sample 46) formed of an amorphous magnetic material with a composition of
Prepare a constant magnetic field (Hm) of 100 e
Table 6 shows the results of measuring the magnetic properties under the conditions of 550H2.
The amorphous magnetic material having composition No. 5 exhibits more preferable magnetic properties than the amorphous magnetic material of sample A46. By heat-treating the amorphous magnetic material of the present invention at a temperature below its crystallization temperature, the coercive force can be improved as described above, and the anisotropy magnetic field (Hk) can also be improved. Table 7 shows examples in which the amorphous magnetic material of the sample layer 45 was heat-treated at various temperatures.As is clear from this table, it is clear that the anisotropic magnetic field can be further improved by heat-treating. . Based on the results shown in Tables 1 to 7 and Figures 2 and 3, the Go-Ni amorphous magnetic material of the present invention is mainly composed of cobalt and contains up to 40 at% of niobium. It was found that if the material is 100%, it exhibits good soft magnetism. Also, Sendust has the highest saturation magnetic flux density of any head material currently in use, with a saturation magnetic flux density of 0.9 kilogauss! As mentioned above, the binary amorphous magnetic material which is mainly composed of niobium and contains 4ON% or less, particularly preferably 30 atoms or less, is a material that can be put to practical use, and is further shown in Table 2. Adding a third element to this will greatly improve the regional magnetic flux density than K, so the above-mentioned cobalt will be the main component, and iono will be included at less than 40 atoms, preferably at most 30 at%. Amorphous magnetic materials with extremely high magnetic flux density i can be easily obtained. As explained in detail above, the present invention has good soft magnetic properties.
WA has good mechanical and chemical properties, so for example, magnetic head 0
It has great practicality as a material, low-frequency and high-frequency transformers, magnetic amplifiers, and magnetic filters, and furthermore, because the Chieri point changes depending on its composition, it can also be used as a thermal sensor. Table 2, No. 31I, No. 4 - Table No. 1 * 4, Brief description of the drawings No. 111 is a schematic cross-sectional view of the apparatus Nf1 for producing the sputtered amorphous magnetic material of the present invention, and FIG. A graph showing the corrosion resistance of the ivy amorphous material, No. BWJ shows the heat treatment of the ivy amorphous material of the present invention! This is a graph showing the effect of Turtle 1111111.0! Volume I1.2kttl:/-￥,
3417/- code, 4, 5, 7.9 are power supplies, 6 is the target electrical number, and 8 is the base plate. (3 people who don't like it) Gaku13 Wi Netsumawari Seihada Ta ('C)
Claims (1)
以下含むことを特徴とするスパッタ非晶質磁性材料。 ２）コバルトを主体とし、ニオブを４０原子パー竜ント
以下含み、更にチタン、ジルコニウム、ハフニウム、バ
ナジウム、タンタル、銅、モリブデン２１ングスデンか
ら成る群から選ばれ良少なくと４１種の追加的元素を含
む仁とを特徴とする特許饋求Ｏ範日第１項記載のスパッ
タ非晶質磁性材料。 ３）コバルトか主体とし、ニオブ會４０ｊ［子バー士ン
ト以下含み、更にり寵ム、マンガン、ニッケル、鉄から
載る詳からａばれた少なくとも１゛種Ｏ追加的元嵩を會
むことを特徴とする特許―求の軛囲第１項配蒙Ｏスパッ
タ非晶質磁性材れ。 リ コバルト【主体とし、ニオブを４０原子パーセント
以下含み、更にほう素、炭素、けい素、リン、ゲルマニ
ウム、すす、インジウム、ひ素、アンチモンから成る群
から違ばれた少くとも１種Ｏ追加的元素を含む仁とを特
徴とする特許請求の範囲９１項記載のスパッタ非晶質磁
性材料。 ５）コバルトを主体とし、ニオブｆｒ４０Ｊ［子パーセ
ント以下含み更に鉄及びマンガンからなる群から選ばれ
え少くとも１種Ｏ追加的元素を含むこと１＊黴とする特
許請求の範囲第Ｓ項記載Ｏスパッタ非晶質磁性材料。 ６）コバルトを主体とし、ニオブを４０５子パー七ント
以下含むスパッタ非晶質磁性材料【結晶化Ｉｌｌ以下Ｏ
ＩＩ度で熱処理すること七％黴とするスパッタ非晶質磁
性材料Ｏ製造方法。[Scope of Claims] 1) A sputtered amorphous magnetic material which is mainly composed of copal and contains 40 atomic percent or less of niobium. 2) Mainly composed of cobalt, containing up to 40 atoms per ton of niobium, and further containing at least 41 additional elements selected from the group consisting of titanium, zirconium, hafnium, vanadium, tantalum, copper, and 21 ngsdenum of molybdenum. The sputtered amorphous magnetic material according to item 1 of the patent application, characterized in that: 3) Mainly composed of cobalt, containing at least 100% of niobium (including niobium, manganese, nickel, iron, etc.) and an additional mass of at least 1 species, which is further atomized from manganese, nickel, and iron. Patent entitled - Clause 1: Dispersion of sputtered amorphous magnetic materials. cobalt [mainly containing 40 atomic percent or less of niobium, and at least one additional element different from the group consisting of boron, carbon, silicon, phosphorus, germanium, soot, indium, arsenic, and antimony. 92. The sputtered amorphous magnetic material according to claim 91, characterized in that the sputtered amorphous magnetic material comprises: 5) Mainly composed of cobalt, containing less than 40% of niobium fr40J, and further containing at least one additional element selected from the group consisting of iron and manganese. Sputtered amorphous magnetic material. 6) Sputtered amorphous magnetic material mainly composed of cobalt and containing less than 405% niobium [crystallized Ill or less O
A method for producing sputtered amorphous magnetic material O by heat treatment at II degree to make it 7% moldy.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57028064A JPS58147538A (en) | 1982-02-25 | 1982-02-25 | Sputtered amorphous magnetic material and its manufacture |
| FR8303001A FR2522188B1 (en) | 1982-02-25 | 1983-02-24 | MAGNETIC MATERIAL AMORPHOUS BY SPRAYING PROCESS AND METHOD FOR THE PRODUCTION THEREOF |
| NL8300695A NL8300695A (en) | 1982-02-25 | 1983-02-24 | SPUTTER PROCESS AMORF MAGNETIC MATERIAL AND METHOD FOR PREPARING THE SAME |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57028064A JPS58147538A (en) | 1982-02-25 | 1982-02-25 | Sputtered amorphous magnetic material and its manufacture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS58147538A true JPS58147538A (en) | 1983-09-02 |
Family
ID=12238329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57028064A Pending JPS58147538A (en) | 1982-02-25 | 1982-02-25 | Sputtered amorphous magnetic material and its manufacture |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPS58147538A (en) |
| FR (1) | FR2522188B1 (en) |
| NL (1) | NL8300695A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62210607A (en) * | 1986-03-12 | 1987-09-16 | Matsushita Electric Ind Co Ltd | Magnetic alloy film |
| CN102649162A (en) * | 2012-04-26 | 2012-08-29 | 中山大学 | Method for preparing noble metal nano material or transitional metal oxide nano material |
| CN104451467A (en) * | 2014-12-15 | 2015-03-25 | 郑州大学 | Cobalt-based block amorphous alloy and preparation method thereof |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59193235A (en) * | 1983-04-15 | 1984-11-01 | Hitachi Ltd | Co-nb-zr type amorphous magnetic alloy and magnetic head using the same |
| US20160160331A1 (en) * | 2013-07-12 | 2016-06-09 | Hewlett-Packard Development Company, L.P. | Amorphous thin metal film |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE7511398L (en) * | 1974-10-21 | 1976-04-22 | Western Electric Co | MAGNETIC DEVICE |
| US4056411A (en) * | 1976-05-14 | 1977-11-01 | Ho Sou Chen | Method of making magnetic devices including amorphous alloys |
| WO1981000861A1 (en) * | 1979-09-21 | 1981-04-02 | Hitachi Metals Ltd | Amorphous alloys |
| JPS5789450A (en) * | 1980-11-21 | 1982-06-03 | Matsushita Electric Ind Co Ltd | Amorphous magnetic alloy |
-
1982
- 1982-02-25 JP JP57028064A patent/JPS58147538A/en active Pending
-
1983
- 1983-02-24 FR FR8303001A patent/FR2522188B1/en not_active Expired
- 1983-02-24 NL NL8300695A patent/NL8300695A/en not_active Application Discontinuation
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62210607A (en) * | 1986-03-12 | 1987-09-16 | Matsushita Electric Ind Co Ltd | Magnetic alloy film |
| JPH0573242B2 (en) * | 1986-03-12 | 1993-10-14 | Matsushita Electric Ind Co Ltd | |
| CN102649162A (en) * | 2012-04-26 | 2012-08-29 | 中山大学 | Method for preparing noble metal nano material or transitional metal oxide nano material |
| CN104451467A (en) * | 2014-12-15 | 2015-03-25 | 郑州大学 | Cobalt-based block amorphous alloy and preparation method thereof |
| CN104451467B (en) * | 2014-12-15 | 2016-04-27 | 郑州大学 | A kind of cobalt-base body amorphous alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| NL8300695A (en) | 1983-09-16 |
| FR2522188A1 (en) | 1983-08-26 |
| FR2522188B1 (en) | 1988-06-24 |
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