JPH10280005A - Iron based powder mixture for powder metallurgy and its production - Google Patents
Iron based powder mixture for powder metallurgy and its productionInfo
- Publication number
- JPH10280005A JPH10280005A JP9095953A JP9595397A JPH10280005A JP H10280005 A JPH10280005 A JP H10280005A JP 9095953 A JP9095953 A JP 9095953A JP 9595397 A JP9595397 A JP 9595397A JP H10280005 A JPH10280005 A JP H10280005A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- acid amide
- iron
- lubricant
- weight
- 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.)
- Granted
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000000843 powder Substances 0.000 title claims abstract description 98
- 239000000203 mixture Substances 0.000 title claims abstract description 52
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 46
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000000314 lubricant Substances 0.000 claims abstract description 57
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims abstract description 23
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008117 stearic acid Substances 0.000 claims abstract description 13
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims abstract description 11
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims description 39
- 230000008018 melting Effects 0.000 claims description 31
- 239000010687 lubricating oil Substances 0.000 claims description 15
- WGOROJDSDNILMB-UHFFFAOYSA-N octatriacontanediamide Chemical compound NC(=O)CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC(N)=O WGOROJDSDNILMB-UHFFFAOYSA-N 0.000 claims description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 239000010723 turbine oil Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- 238000005204 segregation Methods 0.000 abstract description 14
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 0.000 abstract description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 6
- 239000011701 zinc Substances 0.000 abstract description 6
- 229910052725 zinc Inorganic materials 0.000 abstract description 6
- 230000000996 additive effect Effects 0.000 abstract description 2
- 150000001408 amides Chemical class 0.000 abstract description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract 1
- 239000005977 Ethylene Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 8
- 230000032258 transport Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- FEEPBTVZSYQUDP-UHFFFAOYSA-N heptatriacontanediamide Chemical compound NC(=O)CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC(N)=O FEEPBTVZSYQUDP-UHFFFAOYSA-N 0.000 description 1
- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- FHSJASSJVNBPOX-UHFFFAOYSA-N octadecanamide Chemical class CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O FHSJASSJVNBPOX-UHFFFAOYSA-N 0.000 description 1
- NJNNJTZOZPHSRA-UHFFFAOYSA-N octatriacontanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O NJNNJTZOZPHSRA-UHFFFAOYSA-N 0.000 description 1
- -1 olein Acid amide Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 230000009291 secondary effect Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、見掛密度が安定
し、添加物の偏析が少なく、成形時の金型からの抜出力
が低く、亜鉛の含有が少なく、とりわけホッパからの流
出性に優れた粉末冶金用鉄基粉末混合物及びその製造方
法に関する。BACKGROUND OF THE INVENTION The present invention relates to a method for producing an ink, which has a stable apparent density, a small segregation of additives, a low ejection force from a mold at the time of molding, a low content of zinc, and a particularly high flowability from a hopper. An excellent iron-based powder mixture for powder metallurgy and a method for producing the same.
【０００２】[0002]
【従来の技術】粉末冶金用鉄基粉末混合物は、鉄粉に、
銅粉、黒鉛粉、燐化鉄粉等の合金粉末とステアリン酸亜
鉛等の潤滑剤とを混合し、さらに必要に応じて切削性改
善用粉末を加えて製造するのが一般的である。しかし、
このような混合物は以下のような欠点を持っている。先
ず、その欠点はこのような混合物が偏析を生ずることで
ある。偏析について述べると、混合物は大きさ、形状及
び密度の異なる粉末を含んでいるため、混合後の輸送、
ホッパへの装入、払出し、又は成形処理等の際に容易に
偏析が生じてしまう。2. Description of the Related Art Iron-base powder mixtures for powder metallurgy are
Generally, alloy powders such as copper powder, graphite powder and iron phosphide powder are mixed with a lubricant such as zinc stearate and, if necessary, a powder for improving machinability is added. But,
Such a mixture has the following disadvantages. First, its disadvantage is that such mixtures cause segregation. Talking about segregation, the mixture contains powders of different sizes, shapes and densities, so transport after mixing,
Segregation easily occurs at the time of charging, dispensing, forming, or the like into the hopper.
【０００３】例えば、鉄系粉末と黒鉛粉との混合物は、
トラック輸送中の振動によって輸送容器内に偏析が起こ
り、黒鉛粉が浮かび上がることは良く知られている。ま
た、ホッパに装入された黒鉛はホッパ内偏析のためホッ
パより排出する際、排出の初期、中期、終期でそれぞれ
黒鉛粉の濃度が異なることも知られている。これらの偏
析によって製品は組成にばらつきを生じ、寸法変化及び
強度のばらつきが大きくなって不良品の原因となる。ま
た、黒鉛粉などはいずれも微粉末であるため混合物の比
表面積を増大させる。その結果、混合物は流動性が低下
する。このような流動性の低下は成形用金型への充填速
度を低下させるため、圧粉体の生産速度を低下させてし
まうという欠点もある。For example, a mixture of an iron-based powder and a graphite powder is
It is well known that vibration during truck transport causes segregation in the transport container and graphite powder emerges. It is also known that when the graphite charged in the hopper is discharged from the hopper due to segregation in the hopper, the concentration of the graphite powder differs at the initial, middle and final stages of the discharge. Due to these segregations, the composition of the product varies, causing dimensional changes and variations in strength to increase, causing defective products. In addition, since graphite powder and the like are all fine powders, the specific surface area of the mixture is increased. As a result, the mixture becomes less fluid. Such a decrease in fluidity lowers the filling speed of the molding die, and therefore has the disadvantage of lowering the production speed of the green compact.
【０００４】従来常用される、潤滑剤のステアリン酸亜
鉛は、焼結時に結合材中の金属元素が酸化物として炉内
を汚染したり、焼結体組成を変化させるという問題点を
有する。特開平５−１４８５０５号公報には、ステアリ
ン酸、オレイン酸モノアミド、ステアリン酸モノアミド
から選ばれた１種以上と、エチレンビスステアリン酸ア
ミド、メチレンビスステアリン酸アミドから選ばれた１
種以上との溶融混合物を結合剤として、鉄基粉末表面に
合金用粉末及び／又は切削性改善用粉末が固着されてい
ることを特徴とする粉末冶金用鉄基粉末混合物を開示し
ている。さらに、同公報には、ステアリン酸、オレイン
酸アミド、ステアリン酸アミド、ステアリン酸アミドと
エチレンビスステアリン酸アミドとの溶融混合物、エチ
レンビスステアリン酸アミドから選ばれた１種以上の加
熱溶融物０．１重量％以上１．０重量％以下を結合材と
して合金用粉末及び／又は切削性改善用粉末が表面に固
着されている鉄基粉末と、ステアリン酸、オレイン酸ア
ミド、ステアリン酸アミド、ステアリン酸アミドとエチ
レンビスステアリン酸アミドとの溶融混合物、エチレン
ビスステアリン酸アミドから選ばれた１種以上の遊離粉
末０．１重量％以上０．５重量％以下と、ステアリン酸
亜鉛の遊離粉末０．０１重量％以上０．２重量％以下と
の混合物であることを特徴とする粉末冶金用鉄基粉末混
合物が開示されている。[0004] Zinc stearate, which is conventionally used as a lubricant, has problems in that the metal element in the binder contaminates the furnace as an oxide during sintering and changes the composition of the sintered body. JP-A-5-148505 discloses that at least one selected from stearic acid, oleic acid monoamide, and stearic acid monoamide and one or more selected from ethylene bisstearic acid amide and methylene bisstearic acid amide are disclosed.
Disclosed is an iron-based powder mixture for powder metallurgy, wherein a powder for alloying and / or a powder for improving machinability is fixed to the surface of the iron-based powder using a molten mixture of at least one kind as a binder. Further, the publication discloses that at least one kind of a heated molten material selected from stearic acid, oleic acid amide, stearic acid amide, a molten mixture of stearic acid amide and ethylenebisstearic acid amide, and ethylenebisstearic acid amide. An iron-based powder having a powder for alloying and / or a powder for improving machinability fixed to the surface with 1% by weight or more and 1.0% by weight or less as a binder, stearic acid, oleic amide, stearic amide, stearic acid A molten mixture of amide and ethylenebisstearic acid amide, one or more free powders selected from ethylenebisstearic acid amide of 0.1% by weight to 0.5% by weight, and zinc stearate free powders of 0.01% by weight or less; There is disclosed an iron-based powder mixture for powder metallurgy, which is a mixture of not less than 0.2% by weight and not more than 0.2% by weight.
【０００５】特開平５−１４８５０５号公報に記載の技
術により、見掛け密度の安定性、偏析、ホッパからの流
出性はかなり改善された。しかしながら、ホッパからの
流出性を含む流動性と金型からの抜出力をバランスよく
確保するという点でいまだ不十分であった。鉄基粉末混
合物を貯蔵した容器からプレス機械にまで搬送する装置
として、例えば日本興産株式会社社製の商品名トランジ
粉・粒体供給機が知られている。この供給機は、ステン
レス鋼、ナイロン又はゴム製の外径４０〜１００ｍｍの
チューブ内に内蔵された１本のヘリカルコイルの回転運
動によって搬送する装置である。この搬送をチューブ・
コイル搬送という、このチューブ・コイル搬送の際に、
前記ヘリカルコイルやチューブの内部に、鉄基粉末混合
物が付着し、特にその中の有機潤滑剤が付着するという
問題があった。[0005] By the technique described in Japanese Patent Application Laid-Open No. 5-148505, the stability of apparent density, segregation and outflow from the hopper have been considerably improved. However, it was still insufficient to ensure a good balance between fluidity including outflow from the hopper and ejection from the mold. As a device for transporting an iron-based powder mixture from a container storing the mixture to a press machine, for example, a transi powder / granule feeder (trade name) manufactured by Nihon Kosan Co., Ltd. is known. This feeder is a device that transports by rotating one helical coil contained in a tube of stainless steel, nylon or rubber having an outer diameter of 40 to 100 mm. Transfer this tube and
At the time of this tube and coil transfer called coil transfer,
There is a problem that the iron-based powder mixture adheres to the inside of the helical coil or tube, and particularly the organic lubricant therein adheres.
【０００６】[0006]
【発明が解決しようとする課題】本発明は上記問題点に
鑑み、従来の粉体特性及び圧粉体特性を十分に維持しな
がら、見掛け密度の安定性、偏析、ホッパからの流出
性、流動性、金型からの抜出力をバランスよく確保し、
かつ、焼成炉を痛める亜鉛の発生を極力押え、鉄粉チュ
ーブ・コイル輸送時のチューブ・コイル内部への付着が
ない粉末冶金用鉄基混合物及びその製造方法を提供する
ものである。SUMMARY OF THE INVENTION In view of the above-mentioned problems, the present invention is to maintain the conventional powder characteristics and green compact characteristics sufficiently while maintaining the apparent density stability, segregation, outflow from the hopper, and fluidity. Characteristics, ensuring a good balance of ejection from the mold,
It is another object of the present invention to provide an iron-based mixture for powder metallurgy which suppresses the generation of zinc which damages a firing furnace as much as possible and which does not adhere to the inside of a tube or a coil during transportation of an iron powder tube or a coil, and a method for producing the same.
【０００７】[0007]
【課題を解決するための手段】本発明は上記課題を解決
するために、提案されたもので、次の各項目に示す技術
的手段を構成とするものである。本発明の第１の発明
は、鉄基粉末と、該鉄基粉末に溶融・付着した、ステア
リン酸、オレイン酸アミド、ステアリン酸アミド、ステ
アリン酸アミドとエチレンビスステアリン酸アミドとの
溶融混合物及びエチレンビスステアリン酸アミドからな
る群から選ばれた異なる融点の２種以上の有機潤滑剤
０．２〜１．０重量％の内の低融点有機潤滑剤と、該低
融点潤滑剤の溶融により粉末形態で前記鉄基粉末に付着
した、前記低融点潤滑剤を除く有機潤滑剤並びに合金用
粉末及び／又は切削性改善粉末と、ステアリン酸亜鉛の
遊離粉末０．１〜０．３５重量％とからなることを特徴
とする粉末冶金用鉄基粉末混合物である。Means for Solving the Problems The present invention has been proposed to solve the above problems, and has the following technical means. The first invention of the present invention relates to an iron-based powder, stearic acid, oleic acid amide, stearic acid amide, a molten mixture of stearic acid amide and ethylenebisstearic acid acid, which is melted and adhered to the iron-based powder; Two or more kinds of organic lubricants having different melting points selected from the group consisting of bis-stearic acid amides; a low melting point organic lubricant of 0.2 to 1.0% by weight; and melting of the low melting point lubricant to form a powder. And an organic lubricant other than the low melting point lubricant, an alloy powder and / or a machinability improving powder adhered to the iron-based powder, and 0.1 to 0.35% by weight of a free zinc stearate powder. An iron-based powder mixture for powder metallurgy characterized by the following.
【０００８】この場合、前記有機潤滑剤にオレイン酸、
スピンドル油、タービン油の内から選ばれた１種以上の
有機質液体潤滑剤０．０１重量％以上０．３重量％以下
を加えると好適である。鉄基粉末に溶融・付着した低融
点有機潤滑剤をステアリン酸アミドとエチレンビスステ
アリン酸アミドとの溶融混合物とし、低融点潤滑剤の溶
融により粉末形態で前記鉄基粉末に付着した有機潤滑剤
をエチレンビスステアリン酸アミドとするのが、ホッパ
流出性が特によくなり好ましい。[0008] In this case, oleic acid,
It is preferable to add 0.01% by weight or more and 0.3% by weight or less of one or more organic liquid lubricants selected from spindle oil and turbine oil. The low-melting organic lubricant melted and adhered to the iron-based powder is a molten mixture of stearic acid amide and ethylenebisstearic acid amide, and the organic lubricant adhered to the iron-based powder in powder form by melting the low-melting lubricant is used. Ethylene bisstearic acid amide is preferred because the hopper outflow is particularly improved.
【０００９】本発明は上記特開平５−１４８５０５号公
報に記載の技術に対して、粉末冶金用鉄基粉末混合物に
粉末として混合している特定の有機化合物を粉末として
混合しない構成としている。本発明の第２の発明は、鉄
基粉末と、合金用粉末及び／又は切削性改善用粉末と、
ステアリン酸、オレイン酸アミド、ステアリン酸アミ
ド、ステアリン酸アミドとエチレンビスステアリン酸ア
ミドとの溶融混合物、エチレンビスステアリン酸アミド
の内から選択した異なる融点の２種以上の有機潤滑剤
０．２〜１．０重量％とを混合した後、前記有機潤滑剤
の内最も低い融点以上、前記潤滑剤の内の最も高い融点
以下の温度範囲で加熱・混合し、さらに冷却した後、ス
テアリン酸亜鉛の粉末０．１〜０．３５重量％を添加・
混合することを特徴とする粉末冶金用鉄基粉末混合物の
製造方法である。According to the present invention, a specific organic compound which is mixed as a powder with an iron-based powder mixture for powder metallurgy is not mixed as a powder with respect to the technique described in the above-mentioned JP-A-5-148505. A second invention of the present invention provides an iron-based powder, a powder for alloy and / or a powder for improving machinability,
Stearic acid, oleic acid amide, stearic acid amide, molten mixture of stearic acid amide and ethylenebisstearic acid amide, two or more organic lubricants having different melting points selected from ethylenebisstearic acid amide 0.2 to 1 And then mixed and heated in a temperature range of not less than the lowest melting point of the organic lubricant and not more than the highest melting point of the lubricant, and further cooled, and then powdered zinc stearate. 0.1 to 0.35% by weight
A method for producing an iron-based powder mixture for powder metallurgy, which comprises mixing.
【００１０】この場合にも、前記有機潤滑剤にオレイン
酸、スピンドル油、タービン油の内から選ばれた１種以
上の有機質液体潤滑剤０．０１重量％以上０．３重量％
以下を加えると好適である。次に、本発明を完成するに
至った知見について説明する。本発明者らは、ステアリ
ン酸亜鉛０．３５重量％以下の添加量で、従来の粉体特
性及び圧粉体特性を維持し、見掛密度が安定し、偏析が
少なく、ホッパからの流出性に優れ、かつ亜鉛含有量が
少ない粉末冶金用鉄基粉末混合物について鋭意研究を重
ねた結果、以下に示す知見を得て本発明に至った。[0010] In this case, the organic lubricant may contain one or more organic liquid lubricants selected from among oleic acid, spindle oil and turbine oil in an amount of 0.01% by weight to 0.3% by weight.
It is preferable to add the following. Next, the findings that led to the completion of the present invention will be described. The present inventors maintain the conventional powder properties and green compact properties at a content of 0.35% by weight or less of zinc stearate, stabilize the apparent density, reduce segregation, and improve the flowability from the hopper. As a result of intensive studies on an iron-based powder mixture for powder metallurgy having excellent zinc content and a low zinc content, the present inventors have obtained the following findings and reached the present invention.
【００１１】本発明は以下の２点のポイントからなる。 （ａ）ステアリン酸、オレイン酸アミド、ステアリン酸
アミド、ステアリン酸アミドとエチレンビスステアリン
酸アミドとの溶融混合物とエチレンビスステアリン酸ア
ミドから選ばれた２種以上の有機潤滑剤０．２〜１．０
重量％を、さらに必要に応じて有機液体潤滑剤を添加し
たものを、前記有機潤滑剤の融点のうち最低の融点以
上、最高の融点以下に加熱し、さらに冷却した後、遊離
粉末を添加混合する。 （ｂ）遊離粉末としてステアリン酸亜鉛を単独で０．１
重量％以上、０．３５重量％以下混合添加する。The present invention comprises the following two points. (A) Stearic acid, oleic acid amide, stearic acid amide, a molten mixture of stearic acid amide and ethylenebisstearic acid amide, and two or more organic lubricants selected from ethylenebisstearic acid amide 0.2-1. 0
Weight percent, and further, if necessary, an organic liquid lubricant added thereto, heated to a minimum melting point or higher and a maximum melting point or lower among the melting points of the organic lubricant, further cooled, and then mixed with a free powder. I do. (B) Zinc stearate alone as free powder in 0.1
% By weight and 0.35% by weight or less.
【００１２】このように、従来の粉体特性及び圧粉体特
性を維持しながら、見掛け重量が安定し、偏析が少な
く、ホッパからの排出性に優れ、かつステアリン酸亜鉛
の含有量が０．３５重量％以下の粉末冶金用鉄基粉末が
得られ、とくに流動性に関しては特開平５−１４８５０
５号公報で提案された鉄基粉末混合物よりも一層優れた
粉末が得られ、チューブ・コイル輸送をする場合、コイ
ル内部への潤滑剤の付着がなくなる。Thus, while maintaining the conventional powder properties and green compact properties, the apparent weight is stable, the segregation is small, the dischargeability from the hopper is excellent, and the content of zinc stearate is 0.1%. An iron-based powder for powder metallurgy of 35% by weight or less was obtained.
A powder which is more excellent than the iron-based powder mixture proposed in Japanese Patent No. 5 is obtained, and when the tube and the coil are transported, the adhesion of the lubricant to the inside of the coil is eliminated.
【００１３】本発明においては、合金用粉末及び／又は
切削性改善用粉末が、鉄基粉末表面に有機潤滑剤の内の
溶融した低融点有機潤滑剤である結合材によって固着さ
れているので偏析を防止することができる。鉄基粉末と
しては、粉砕又はアトマイズ等による純鉄粉及び／又は
合金鉄粉が用いられ、合金用粉末としては黒鉛粉末、合
金粉末等が、焼結体の被切削性を改善する切削性改善用
粉末としては、タルク、金属硫化物等が、製品に要求さ
れる特性を考慮して選定され必要量用いられる。In the present invention, the powder for alloying and / or the powder for improving machinability is segregated on the surface of the iron-based powder by the binder, which is a low-melting organic lubricant which is a molten organic lubricant among the organic lubricants. Can be prevented. Pure iron powder and / or alloyed iron powder obtained by pulverization or atomization is used as the iron-based powder, and graphite powder or alloy powder is used as the alloy powder to improve the machinability of the sintered body. As the powder for use, talc, metal sulfide, or the like is selected and used in a necessary amount in consideration of characteristics required for a product.
【００１４】特開平５−１４８５０５号公報によれば、
鉄基粉末混合物に粉末遊離粉末としてステアリン酸亜鉛
を単独で用いると、抜き出し力が高くなるとされていた
が、その後、鋭意検討を行った結果、結合剤として、ス
テアリン酸（融点６９℃）、オレイン酸アミド（融点７
６℃）、ステアリン酸アミド（融点１０３℃）、ステア
リン酸アミドとエチレンビスステアリン酸アミドとの溶
融混合物（融点１２５℃）、エチレンビスステアリン酸
アミド（融点１４７℃）から選ばれた２種以上の有機潤
滑剤０．２重量％以上１．０重量％以下と必要に応じて
液体潤滑剤を加えることにより抜き出し力を低減させる
ことが可能となった。According to JP-A-5-148505,
It was believed that the use of zinc stearate alone as the powder free powder in the iron-based powder mixture would increase the extraction force. However, as a result of intensive studies, it was found that stearic acid (melting point 69 ° C.), olein Acid amide (mp 7
6 ° C.), stearic acid amide (melting point 103 ° C.), a molten mixture of stearic acid amide and ethylenebisstearic acid amide (melting point 125 ° C.), and ethylenebisstearic acid amide (melting point 147 ° C.) The removal force can be reduced by adding a liquid lubricant as needed, from 0.2% by weight to 1.0% by weight of the organic lubricant.
【００１５】前記有機潤滑剤をステアリン酸、オレイン
酸アミド、ステアリン酸アミド、ステアリン酸アミドと
エチレンビスステアリン酸アミドとの溶融混合物単独あ
るいはエチレンビスステアリン酸アミド単独の添加では
このような抜出力低減効果はない。これに対して、本発
明で鋳型からの抜出力を低減できるのは、このような該
混合粉の製造粉として、融点のうち最低の融点以上、最
高の融点以下に加熱することにより、図１に示すよう
に、鉄粉１に付着する有機潤滑剤４は、溶融した低融点
の有機潤滑剤３と未溶融の高融点潤滑剤２とからなる構
造となる。この未溶融の潤滑剤２の部分が抜出力を低下
させると思われる。When the organic lubricant is used alone, stearic acid, oleic acid amide, stearic acid amide, a molten mixture of stearic acid amide and ethylene bisstearic acid amide alone, or ethylene bisstearic acid amide alone, such an effect of reducing the ejection force is obtained. There is no. On the other hand, in the present invention, the extraction power from the mold can be reduced by heating the mixed powder to a temperature higher than the lowest melting point and lower than the highest melting point as shown in FIG. As shown in (1), the organic lubricant 4 attached to the iron powder 1 has a structure composed of a molten low-melting organic lubricant 3 and an unmelted high-melting lubricant 2. It is considered that the unmelted portion of the lubricant 2 lowers the ejection force.
【００１６】有機潤滑剤の量が０．２重量％未満では合
金用粉末等の付着性が低下すると共に、金型からの抜出
力が劣化するためである。有機潤滑剤の量が１．０重量
％を越えて多すぎると、潤滑剤としてステアリン酸亜鉛
を過度の添加してもホッパからの流出性を向上させるこ
とができない。また、ステアリン酸、オレイン酸アミ
ド、ステアリン酸アミド、ステアリン酸アミドとエチレ
ンビスステアリン酸アミドとの溶融混合物、エチレンビ
スステアリン酸アミドから選ばれた１種を加熱溶融した
有機潤滑剤では抜出力が劣化するので不可である。If the amount of the organic lubricant is less than 0.2% by weight, the adhesion of the alloy powder and the like is reduced, and the ejection force from the mold is deteriorated. If the amount of the organic lubricant exceeds 1.0% by weight, the outflow from the hopper cannot be improved even if zinc stearate is excessively added as a lubricant. In addition, the output power is deteriorated with stearic acid, oleic acid amide, stearic acid amide, a molten mixture of stearic acid amide and ethylene bis stearic acid amide, and an organic lubricant obtained by heating and melting one of ethylene bis stearic acid amide. It is not possible.
【００１７】ステアリン酸亜鉛の粉末は０．１０重量％
以上添加しないとホッパからの流出性が得られない。一
方、０．３５重量％を越えて添加すると焼結時に発生す
る亜鉛により緒焼成炉を痛める可能性がある。従って、
０．１０重量％以上０．３５重量％以下に限定する。ま
た、ステアリン酸亜鉛に加え、脂肪酸又は脂肪酸アミド
を添加すると、鉄粉をチューブ・コイル輸送中に付着物
が生成する。0.10% by weight of zinc stearate powder
Unless it is added above, the outflow property from the hopper cannot be obtained. On the other hand, if it exceeds 0.35% by weight, zinc generated during sintering may damage the firing furnace. Therefore,
It is limited to 0.10% by weight or more and 0.35% by weight or less. In addition, when fatty acids or fatty acid amides are added in addition to zinc stearate, deposits are generated during transport of the iron powder in the tube and coil.
【００１８】なお、オレイン酸、スピンドル油、タービ
ン油から選ばれた１種以上の有機質液体潤滑剤０．０１
重量％以上０．３重量％以下を有機潤滑剤に混合するこ
とによってさらに付着は強固となると共に、見掛け密度
を安定させる効果を有する。液体潤滑剤の添加量が０．
０１重量％未満では見掛け密度を安定する効果がなく、
０．３重量％を越えるとホッパからの流出性が低下す
る。液体潤滑剤の添加時期は鉄基粉末と他の添加物を混
合する前が好ましい。液体潤滑剤は撹拌混合時に鉄基粉
末表面を速やかに覆い、撹拌による鉄基粉末同士の表面
摩擦、衝突による変形を抑制し、変形による流出性の低
下を押えると共に、鉄基粉末表面への添加物の均一付着
を容易にする作用を有するためである。One or more organic liquid lubricants selected from the group consisting of oleic acid, spindle oil and turbine oil.
By mixing the organic lubricant in an amount of from 0.3% by weight to 0.3% by weight, the adhesion is further strengthened and the apparent density is stabilized. The amount of liquid lubricant added is 0.
If it is less than 01% by weight, there is no effect of stabilizing the apparent density,
If it exceeds 0.3% by weight, the outflow property from the hopper is reduced. It is preferable to add the liquid lubricant before mixing the iron-based powder and other additives. The liquid lubricant quickly covers the surface of the iron-based powder during stirring and mixing, suppresses surface friction between the iron-based powders due to stirring and deformation due to collision, suppresses the decrease in outflow due to deformation, and adds it to the surface of the iron-based powder. This is because it has an effect of facilitating uniform attachment of objects.
【００１９】液体潤滑剤の添加時期は鉄粉と他の添加物
とを混合する前である。混合中では見掛密度の安定化作
用が小さく流出性も低下し、さらに混合後では見掛密度
安定作用、流出性ともに低下するからである。すなわち
液体潤滑剤は鉄粉と他の添加物との撹拌混合時にすみや
かに鉄粉表面を覆い、撹拌による鉄粉粒子の表面摩擦、
衝突による変形を抑制し、変形による流出性の低下を抑
制するものである。また鉄粉表面への添加物の均一付着
を容易にする作用も副次的に有する。The liquid lubricant is added before mixing the iron powder with other additives. This is because during the mixing, the effect of stabilizing the apparent density is small and the outflow property is reduced, and after the mixing, both the apparent density stabilizing action and the outflow property are reduced. That is, the liquid lubricant quickly covers the surface of the iron powder when stirring and mixing the iron powder and other additives, and the surface friction of the iron powder particles due to the stirring,
It suppresses deformation due to collision and suppresses a decrease in outflow properties due to deformation. It also has a secondary effect of facilitating uniform attachment of the additive to the surface of the iron powder.
【００２０】液体潤滑剤以外の他の結合材すなわち、加
熱溶融混合によって結合材として用いる前記有機化合物
の添加量は、液体潤滑剤を用いない場合の前述の添加量
と同等でよい。またステアリン酸亜鉛の選択添加量も前
述と同様でよい。加熱温度は、用いられる結合材構成物
（液体潤滑剤を除く有機化合物）の最低融点以上、好ま
しくは構成物の最低融点プラス１０℃以上、最高融点の
構成物の融点以下とする。これにより、熱分解による機
能低下を防止するとともに、流出性能を向上させる。The addition amount of the binder other than the liquid lubricant, that is, the amount of the organic compound used as the binder by heating and melting and mixing may be the same as the above-mentioned addition amount when the liquid lubricant is not used. The selective addition amount of zinc stearate may be the same as described above. The heating temperature is not lower than the minimum melting point of the binder constituent (organic compound excluding the liquid lubricant) used, preferably not lower than the minimum melting point of the constituent plus 10 ° C. and not higher than the melting point of the constituent having the highest melting point. This prevents the functional degradation due to the thermal decomposition and improves the outflow performance.
【００２１】[0021]
【実施例】平均粒径７８μｍの粉末冶金用鉄粉に、平均
粒径２３μｍの黒鉛粉末１重量％、平均粒径２５μｍの
電解銅粉を２重量％と、表１に示した有機潤滑剤を十分
混合後、有機潤滑剤中最低の融点以上、最高の融点以下
で混合加熱し（１次混合）、さらに混合しながら８５℃
以下に冷却した。冷却後、遊離粉末として表１に示す２
次混合の潤滑剤を均一に混合後（２次混合とする）、加
熱混合機から排出した。EXAMPLE 1% by weight of graphite powder having an average particle size of 23 μm, 2% by weight of electrolytic copper powder having an average particle size of 25 μm, and an organic lubricant shown in Table 1 were added to iron powder for powder metallurgy having an average particle size of 78 μm. After thorough mixing, the mixture is mixed and heated at a temperature not lower than the lowest melting point and lower than the highest melting point in the organic lubricant (primary mixing).
Cooled below. After cooling, 2
After the next mixture of lubricants was uniformly mixed (secondary mixing), the mixture was discharged from the heating mixer.
【００２２】表２にはこれらの混合粉末を直径２５ｍ
ｍ、高さ２０ｍｍのタブレットを５ｔ／ｃｍ2 で成形し
たのち金型から抜出すときの押圧力（抜出力）と、流動
度はオリフィス径５ｍｍの容器に鉄粉１００ｇを充填
後、排出するまでの時間で示す流動度の結果を示した。
粉末のホッパ流出性は、内径１００ｍｍ、高さ２００ｍ
ｍの容器の底部中央に設けた直径２．０ｍｍのオリフィ
スから混合物１０００ｇを排出させるまでの加振回数で
評価した。また、混合粉末を５ｔ／ｃｍ2 で成形したの
ち、ＲＸ雰囲気中で１１３０℃２０分焼結後、焼結体表
面に煤があるか否か目視で判断した結果を表２に示し
た。Table 2 shows that these mixed powders have a diameter of 25 m.
m, a tablet having a height of 20 mm, molded at 5 t / cm 2 , and the pressing force (extraction force) when ejecting from the mold and the fluidity are measured after filling 100 g of iron powder into a container having an orifice diameter of 5 mm until it is discharged. The result of the flow rate shown by the time was shown.
Hopper outflow of powder is 100mm inside diameter, 200m height
The evaluation was made by the number of times of vibration until 1000 g of the mixture was discharged from an orifice having a diameter of 2.0 mm provided at the center of the bottom of the m container. Table 2 shows the result of molding the mixed powder at 5 t / cm 2 , sintering at 1130 ° C. for 20 minutes in an RX atmosphere, and visually determining whether or not soot was present on the surface of the sintered body.
【００２３】偏析防止処理粉末１０ｔをチューブ・コイ
ル型輸送機（商品名トランジー、日本興産製ＴＳ−０５
−７ＡＢ）を用いて、１．３ｔ／ｈｒの送り速度で輸送
した。１０ｔ輸送後チューブ・コイル内部のコイル内付
着物の有無を調べ、その結果を表２に示した。実施例１
〜８に示すように、本願発明の配合で鉄基混合粉末を製
造すれば、流動性に格段優れ、ホッパ排出性が良好で、
抜出力が低く、焼結体に煤の発生が見られないか僅かに
見られる程度でチューブ・コイル輸送中付着物の発生の
ない、粉末冶金用鉄基混合粉末を容易に製造することが
できる。比較例１の２次混合物のステアリン酸亜鉛が少
ない場合、ホッパ排出時にホッパ流動度の時間が多とな
り、流動性が低下し、比較例このステアリン酸亜鉛が多
い場合、焼結体に煤が発生した。比較例３、４では、２
次混合する潤滑剤である遊離粉末としてステアリン酸亜
鉛に加え、脂肪酸アミド又はエチレンビスステアリン酸
アミドを含むので、流動性が低下し、さらにチューブ・
コイル輸送時に付着物が発生する。10 t of the segregation preventing powder was transferred to a tube-coil type transport machine (trade name: TS-05, manufactured by Nihon Kosan Co., Ltd.).
-7AB) at a feed rate of 1.3 t / hr. After transporting 10 tons, the presence or absence of deposits in the coil inside the tube / coil was examined. The results are shown in Table 2. Example 1
As shown in Nos. To 8, if the iron-based mixed powder is produced by the blending of the present invention, the fluidity is remarkably excellent, the hopper discharge property is excellent,
It is possible to easily produce an iron-based mixed powder for powder metallurgy, which has a low extraction power and no or little soot is generated in the sintered body and no deposit is generated during transportation of the tube and coil. . When the zinc stearate of the secondary mixture of Comparative Example 1 is small, the hopper fluidity time becomes long when the hopper is discharged, and the fluidity is reduced. Comparative Example When the zinc stearate is large, soot is generated in the sintered body. did. In Comparative Examples 3 and 4, 2
As it contains fatty acid amide or ethylene bisstearic acid amide in addition to zinc stearate as free powder, which is a lubricant to be mixed next, the fluidity is reduced, and the tube and
Deposits are generated during coil transport.
【００２４】比較例５の１次混合の有機潤滑剤が多い場
合、流動性が低下し、比較例６の１次混合有機潤滑剤が
少ない場合抜き出し力が高い。When the amount of the primary mixed organic lubricant of Comparative Example 5 is large, the fluidity is reduced, and when the amount of the primary mixed organic lubricant of Comparative Example 6 is small, the extraction force is high.
【００２５】[0025]
【表１】 [Table 1]
【００２６】[0026]
【表２】 [Table 2]
【００２７】[0027]
【発明の効果】本発明により、従来の混合物に比して、
チューブ・コイル輸送中の付着の発生を防止でき、さら
に合金用粉末や切削性改善用粉末の偏析が少なく、ホッ
パからの流出性に優れるので見掛密度が安定し、金型か
らの抜出力が小さいので成形体の損傷がなく、粉末冶金
製品の品質が安定し切削性が改善され、さらに、結合材
や潤滑剤の金属成分が少ないので焼結体組成の変化や焼
結炉の汚染を生じることの少ない粉末冶金用鉄基粉末混
合物及びその製造方法を提供することができ、寄与する
ところが大きい。According to the present invention, compared with the conventional mixture,
Prevents adhesion during transportation of tubes and coils, minimizes segregation of alloy powder and machinability improving powder, and excels in outflow from the hopper, stabilizing the apparent density and improving output from the mold. Because of its small size, there is no damage to the molded product, the quality of the powder metallurgy product is stable and the machinability is improved.In addition, since the metal components of the binder and the lubricant are small, the composition of the sintered body changes and the sintering furnace is contaminated. It is possible to provide an iron-based powder mixture for powder metallurgy and a method for producing the iron-based powder mixture, which are less likely to contribute.
【図１】鉄粉の表面の結合材の付着構造を示す模式図で
ある。FIG. 1 is a schematic diagram showing a structure of a bonding material attached to a surface of iron powder.
１ 鉄粉 ２ 未溶融の有機潤滑剤 ３ 溶融した有機潤滑剤 ４ 有機潤滑剤 Reference Signs List 1 iron powder 2 unmelted organic lubricant 3 molten organic lubricant 4 organic lubricant
Claims (4)
なる融点の２種以上の有機潤滑剤０．２〜１．０重量％
の内の低融点有機潤滑剤と、 該低融点潤滑剤の溶融により粉末形態で前記鉄基粉末に
付着した、前記低融点潤滑剤を除く有機潤滑剤並びに合
金用粉末及び／又は切削性改善粉末と、 ステアリン酸亜鉛の遊離粉末０．１〜０．３５重量％と
からなることを特徴とする粉末冶金用鉄基粉末混合物。 記 ステアリン酸、オレイン酸アミド、ステアリン酸アミ
ド、ステアリン酸アミドとエチレンビスステアリン酸ア
ミドとの溶融混合物、エチレンビスステアリン酸アミド1. An iron-based powder and 0.2 to 1.0% by weight of two or more organic lubricants having different melting points selected from the following, which are melted and adhered to the iron-based powder.
A low-melting point organic lubricant, and an organic lubricant other than the low-melting point lubricant and an alloy powder and / or a machinability improving powder adhered to the iron-based powder in powder form by melting the low-melting point lubricant. An iron-based powder mixture for powder metallurgy, comprising: 0.1 to 0.35% by weight of a free powder of zinc stearate. Note Stearic acid, oleic acid amide, stearic acid amide, molten mixture of stearic acid amide and ethylenebisstearic acid amide, ethylenebisstearic acid amide
レイン酸、スピンドル油、タービン油の内から選ばれた
１種以上の有機質液体潤滑剤０．０１重量％以上０．３
重量％以下を加えたことを特徴とする粉末冶金用鉄基粉
末混合物。2. The method according to claim 1, wherein the organic lubricant is at least 0.01% by weight of at least 0.3% by weight of an organic liquid lubricant selected from oleic acid, spindle oil and turbine oil.
An iron-based powder mixture for powder metallurgy characterized by adding not more than 10% by weight.
性改善用粉末と、下記の内から選択した異なる融点の２
種以上の有機潤滑剤０．２〜１．０重量％とを混合した
後、前記有機潤滑剤の内最も低い融点以上、前記潤滑剤
の内の最も高い融点以下の温度範囲で加熱・混合し、さ
らに冷却した後、ステアリン酸亜鉛の粉末０．１〜０．
３５重量％を添加・混合することを特徴とする粉末冶金
用鉄基粉末混合物の製造方法。 記 ステアリン酸、オレイン酸アミド、ステアリン酸アミ
ド、ステアリン酸アミドとエチレンビスステアリン酸ア
ミドとの溶融混合物、エチレンビスステアリン酸アミド3. An iron-based powder, an alloy powder and / or a machinability improving powder having a different melting point selected from the following:
After mixing with 0.2 to 1.0% by weight of at least one kind of organic lubricant, the mixture is heated and mixed in a temperature range from the lowest melting point of the organic lubricant to the highest melting point of the lubricant. After further cooling, the powder of zinc stearate 0.1 to 0.1.
A method for producing an iron-based powder mixture for powder metallurgy, comprising adding and mixing 35% by weight. Note Stearic acid, oleic acid amide, stearic acid amide, molten mixture of stearic acid amide and ethylenebisstearic acid amide, ethylenebisstearic acid amide
ン酸、スピンドル油、タービン油の内から選ばれた１種
以上の有機質液体潤滑剤０．０１重量％以上０．３重量
％以下を加えたことを特徴とする粉末冶金用鉄基粉末混
合物の製造方法。4. The organic lubricant according to claim 3, wherein one or more organic liquid lubricants selected from oleic acid, spindle oil and turbine oil are added in an amount of 0.01% by weight to 0.3% by weight. A method for producing an iron-based powder mixture for powder metallurgy, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP09595397A JP3903520B2 (en) | 1997-04-14 | 1997-04-14 | Iron-based powder mixture for powder metallurgy and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP09595397A JP3903520B2 (en) | 1997-04-14 | 1997-04-14 | Iron-based powder mixture for powder metallurgy and method for producing the same |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006274249A Division JP2007002340A (en) | 2006-10-05 | 2006-10-05 | Iron based powder mixture for powder metallurgy, and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10280005A true JPH10280005A (en) | 1998-10-20 |
| JP3903520B2 JP3903520B2 (en) | 2007-04-11 |
Family
ID=14151625
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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| Country | Link |
|---|---|
| JP (1) | JP3903520B2 (en) |
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| WO2001032337A1 (en) * | 1999-10-29 | 2001-05-10 | Kawasaki Steel Corporation | Lubricating agent for mold at elevated temperature, iron-based powder composition for elevated temperature compaction with lubricated mold and high density formed product from iron-based powder composition, and method for producing high density iron-based sintered compact |
| JP2003515661A (en) * | 1999-12-02 | 2003-05-07 | ホガナス アクチボラゲット | Lubricant composite and method for producing the same |
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| JP2003515661A (en) * | 1999-12-02 | 2003-05-07 | ホガナス アクチボラゲット | Lubricant composite and method for producing the same |
| JP2010265454A (en) * | 1999-12-02 | 2010-11-25 | Hoganas Ab | Lubricant combination and process for preparing the same |
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