CN1223422C - 经过磷化处理的铁粉及其制造方法 - Google Patents
经过磷化处理的铁粉及其制造方法 Download PDFInfo
- Publication number
- CN1223422C CN1223422C CNB97192452XA CN97192452A CN1223422C CN 1223422 C CN1223422 C CN 1223422C CN B97192452X A CNB97192452X A CN B97192452XA CN 97192452 A CN97192452 A CN 97192452A CN 1223422 C CN1223422 C CN 1223422C
- Authority
- CN
- China
- Prior art keywords
- powder
- iron
- phosphoric acid
- hypoxemia
- matrix
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title description 6
- 229910019142 PO4 Inorganic materials 0.000 title description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title description 3
- 239000010452 phosphate Substances 0.000 title description 3
- 239000000843 powder Substances 0.000 claims abstract description 74
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052742 iron Inorganic materials 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 24
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 17
- 238000000576 coating method Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 206010021143 Hypoxia Diseases 0.000 claims description 11
- 208000018875 hypoxemia Diseases 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 2
- 238000009692 water atomization Methods 0.000 claims description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000004888 barrier function Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical compound [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 abstract 1
- 235000011007 phosphoric acid Nutrition 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 4
- 230000001976 improved effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 125000004437 phosphorous atom Chemical group 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920004738 ULTEM® Polymers 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
- C23C22/03—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions containing phosphorus compounds
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- 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
- H01F1/20—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 in the form of particles, e.g. powder
-
- 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
- H01F1/20—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 in the form of particles, e.g. powder
- H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—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 in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Glanulating (AREA)
- Materials For Medical Uses (AREA)
Abstract
本发明涉及一种新颖的低氧粉末，它包括主要由具有绝缘的含氧和含磷隔离层的纯铁构成的基体粉末的颗粒。新粉末的含氧量按重量计至多比基体粉末的含氧量高0.2%，并且在用ESCA方法测量时，O∶P比为30～1，最好为15～12，更好为10～3。本发明还涉及一种制备铁基粉末的新方法，它包括下列步骤：制备由水粉碎铁粉或海绵铁粉构成的基体粉末；用磷酸在有机溶剂中的溶液处理混合物并干燥得到的混合物，由此在混合的同时将磷酸溶液喷射到基体粉末上。
Description
技术领域
本发明涉及一种新的铁基粉末。更具体一些，本发明涉及一种用于制备软磁材料的新的铁基粉末，该软磁材料在高频和低频下使用时都具有改进的性能。本发明还涉及一种用于制造新的铁基粉末的新方法。
背景技术
在用粉末冶金方法制造结构元件时，铁基颗粒曾长期被用作基体材料。铁基颗粒首先在高压下在模具中被模制，以便得到所要求的形状。在模制步骤之后，结构元件通常要经过烧结步骤，从而赋予零件以必要的强度。
磁芯元件也曾经用这种粉末冶金方法制造，但是，在这些方法中所用的铁基颗粒通常都涂覆以环绕的绝缘材料层。
铁芯元件的两个主要特性是其磁导率和铁芯损耗特性。材料的磁导率是其被磁化的能力或其传播磁通量的能力的指标。磁导率被定义为感应的磁通量与磁化力或磁场强度之比。当磁性材料受到快速变化的磁场的作用时，芯部的总能量由于产生滞后回线损失和/或涡流损耗而减少。滞后回线损失是由于必须消耗能量，以在铁芯元件中克服剩余磁力而产生的。涡流损耗的产生是因为交流(AC)条件所引起的磁通变化而在铁芯元件中产生电流。
磁芯元件通常用层压的薄钢板制造，但是这些元件难于制造成得到小的复杂零件的网状，并且在高频时遭受大的铁芯损耗。这些叠片基芯子的应用还受到这样的限制，即必须只在薄板的平面中传播磁通量，以免有过大的涡流损耗。作为用于磁芯元件的材料，曾经用烧结的金属粉末代替层压的薄钢板，但是这些烧结的零件也有高的铁芯损失并且主要限于直流(DC)工作。
采用包覆铁基粉末通过粉末冶金制造磁芯元件的研究曾经针对铁粉成分的研制，这种铁粉成分能加强某些物理性能和磁性能，而且不会不利地影响其它性能。所要求的性能包括经过宽广的频率范围的高磁导率，高的压缩强度，低的铁芯损耗和用于压缩模制技术的适合性。
当模制一用于AC动力场合的芯部元件时，通常要求铁颗粒有电绝缘涂层，以减少铁芯损耗。
在文献中公开了各种类型的用于铁颗粒的绝缘涂层。
按照DE 129 1028，用磷酸溶液处理铁粉，接着经过洗涤和干燥。这一工艺的特征为，铁粉的颗粒尺寸最大为10μm，并且除了磷酸以外还用铬酸处理铁粉。该公报没有公开由铁粉制备的材料的磁性能。
此领域中的另一公开文献为DE2825235，它公开了一种由被涂覆以氧化物层的颗粒组成的铁粉。颗粒尺寸在0.05mm至0.15mm之间，并且颗粒具有氧化物涂层，该涂层按颗粒重量计算包括0.3％-0.8wt％的氧。氧化物涂层可以通过在空气中加热或通过化学氧化得到，但是没有公开任何工艺参数和包覆粉粒的分析。根据一些例子可以计算出，所得到的磁导率的范围为30-35。
欧洲专利申请434669涉及一种磁粉，其中，电绝缘涂层将磁粉颗粒分开。颗粒具有10-300μm的平均颗粒尺寸，并且包覆磁粉的每个颗粒的绝缘材料包括厚度为10μm或更小的连续绝缘膜，而且此膜包括一金属酚盐或其分解产物。
WO 95/29490公开了通过采用一种以水中的磷酸为基础的方法得到的绝缘层。
最后，DE专利3439397公开了由磷酸盐涂层电绝缘的铁颗粒。这种涂层可以例如是磷酸镁或磷酸锌。绝缘的磷酸盐涂层应当为铁颗粒的重量的0.1％-1.5％。此公开文献的例1较详细地披露了这种电绝缘的涂层是通过在浓度为89％的磷酸在丙酮中的溶液中搅拌铁粉而得到的。按照WO专利申请的粉末和按照DE专利的粉末之间的比较性研究表明，按照DE专利的绝缘层包括比按照WO申请的粉末多得多的氧和磷。
现在已经非常意外地发现，通过采用按照本发明的新的低氧粉末可以得到显著改进的性能。这些性能包括强度、密度、磁感和磁导率，同时有较低的损耗。
发明内容
新的粉末以一种基体粉末为基础，它主要由纯铁组成并且可以例如是可从市场上得到的水雾化铁粉或具有圆的、不规则的或扁平的颗粒的海绵铁粉。可以使用的不规则的、水雾化的铁粉的典型例子为可以从瑞典Hgans公司得到的ABC 100和ASC100系列的粉末。基体粉末的颗粒尺寸取决于粉末的预定最终用途并且通常小于200μm，而且最好小于150μm。对于较高的频率，优选小于45μm的颗粒尺寸。更为优选的是，多数铁基粉末的颗粒应有大于10μm的颗粒尺寸。
按照本发明，此基体粉末设有一氧涂层或隔离层，其与众不同的新特征在于，新粉末的氧气量只比基体粉末的略高一些。更具体一些，新粉末中的氧气量按重量百分比计比基体粉末中的至多多0.2％，最好至多多0.15％。
可以认为，对于新粉末的性能来说，颗粒的表面结构和成分是重要的，为此，曾经用FSCA法研究了新粉末(参看：“第六届国际X射线光学和微量分析会议会刊”东京大学出版社，1972，385～392页和393～398页；或Anthony R.west著的“固体化学及其应用”，由John willey and sons出版社出版1984，第86页和第92～96页)。按照此方法，O∶P比应当小于30并大于1。此比例最好应小于15，且大于2，小于10并大于3更好。
新粉末的颗粒的表面隔离层的另一重要特征为厚度，而且通过使用AES方法(参看上面所引用的出版物“固体化学及其应用”)已发现，绝缘隔离层或涂层应当小于100nm，最好小于70nm，更好的是小于50nm。
按照本发明的绝缘涂层是通过以一段足以得到所要求的量的时间用有机溶剂中的磷酸处理基体粉末而施加在基体粉末上的。磷酸在有机溶剂中的浓度应当大大地低于在DE专利中公开的浓度并在0.5％～50％之间变化，最好在0.5％～20％之间变化，更好一些在1％～5％之间变化。新粉末可以通过在一段足以达到上述水平的时间内将磷酸溶液喷射在基体粉末上而得到。磷酸的浓度最好应当小于按重量计的10％，更好一些小于5％。
按照本发明的新的铁基粉末在压实步骤之前可以与按重量计为0.1％～1.0％的润滑剂和任选的一种有机热固性或热塑性树脂结合。润滑剂的代表性例子为Kenolube、H蜡、EBS和像硬脂酸锌这样的硬脂酸盐。有机树脂可以从由Peracit、Ultem组成的组中选取。
压实可以在最高达1000Mpa的传统压力下进行，而且压实可在环境温度或高温下进行。
附图说明
图1示出了按照本发明的低氧粉末的磁性能的改进的效果。
图2示出了做为总含氧量的函数的改进的效果。
具体实施方式
本发明进一步地由下列试验说明。
使1kg在市场上可从瑞典Hgans公司得到的粉末ABC100。30的试样分别通过使用在水和乙醇中的正磷酸而受到涂层处理。在一段足以得到氧和磷的涂层或隔离层的时间内，将其量在2.5～120ml/kg间变化的溶液喷射在铁基粉末上随后干燥所有的试样，以便去掉溶剂。所得到的粉末的ESCA分析显示，通过使用水溶液得到的粉末的O∶P比(原子％O∶原子％P)约为30，而且通过采用按照本发明的方法得到的同样比例在5～10之间变化。
对试样的化学分析表明，通过使用水溶液得到的粉末的氧含量要比基体粉末中的高0.2％以上，而通过采用按照本发明的方法得到的粉末的氧含量要比基体粉末中的高0.2％以下。试样的AES分析表明，所有试样的氧化物厚度均小于100nm。
下表综合了用由A指代的新粉末得到的数据，以与本发明范围以外的粉末比较。
表1
| 试样 | O/P | 原子％P | 原子％0 | O总量 | O增加 | P总量 | P增加 |
| 基体粉末(1) | 0.00 | 53.98 | 0.067 | 0 | 0.003 | 0 | |
| A4 | 9.3 | 5.83 | 53.98 | 0.070 | 0.003 | 0.004 | 0.001 |
| A3 | 6.95 | 5.91 | 41.13 | 0.093 | 0.026 | 0.014 | 0.011 |
| A2 | 4.6 | 13.49 | 61.92 | 0.171 | 0.104 | 0.048 | 0.045 |
| 参考B | 29.7 | 1.92 | 57.01 | 0.214 | 0.147 | 0.013 | 0.010 |
采用以单色Al作为X射线源的KRATOS AXIS HS光谱仪的ESCA测量O/P比，Kα＝1486.6eV；～39.5nm。
O和P的量用化学分析测量。
参考B是根据在WO 95/29490中公开的方法用水溶液制备的试样。
表2公开了与本发明范围以外的粉末相比，用从新型粉末制备的材料得到的生坯强度和密度。粉末在800Mpa下压实并加入0.6％的Kenolube作为润滑剂。
表2
| 材料 | 生坯强度(N/mm2) | 密度(g/cm3) |
| 参考B | 26.71 | 7.25 |
| A | 39.55 | 7.31 |
| 参考C | 19.24 | 7.14 |
参考C是按照DE专利3439397制备的试样。
图1示出了按照本发明的低氧粉末在用低氧粉末制备的试样的磁性能方面的改进效果。粉末曾经用其由ESCA方法测量的O/P比定义。试样通过在800MPa下压实粉末并在500℃加热压实的试样30min而制备。“参考B”代表通过对同样的铁基粉末采用水处理而得到的结果。可以看出，采用按照本发明的新的低氧铁可以得到惊人的改进。
图2公开了作为图1中示出的试样的总含氧量的函数的改进效果。
Claims (12)
1.一种低氧粉末，包括主要由具有绝缘的含氧和含磷隔离层的纯铁构成的基体粉末的颗粒，其特征为，粉末的含氧量按重量计比基体粉末的含氧量至多高0.2％，而且在用ESCA方法测量时，O∶P比在30和1之间，并且在用AES方法测量时，隔离层的厚度至多为100nm。
2.如权利要求1所述的低氧粉末，其特征为，所述的O∶P比在15和2之间。
3.如权利要求1所述的低氧粉末，其特征为，所述的O∶P比在10和3之间。
4.如权利要求1所述的低氧粉末，其特征为，基体粉末为海绵铁粉或水雾化的铁粉。
5.如权利要求1至4之一所述的低氧粉末，其特征为，隔离层的厚度小于70nm。
6.如权利要求1至4之一所述的低氧粉末，其特征为，隔离层的厚度小于50nm。
7.一种用于制备铁基粉末的方法，包括下列步骤：制备由水雾化铁粉或海绵铁粉构成的基体粉末；用浓度按重量计为在0.5％和50％之间变化的磷酸在有机溶剂中的溶液处理混合物并干燥所得到的混合物，其特征为，在混合的同时将上述磷酸溶液喷射到基体粉末上。
8.如权利要求7所述的方法，其特征为，有机溶剂中磷酸的浓度按重量计在0.5％和20.0％之间变化。
9.如权利要求7所述的方法，其特征为，有机溶剂中磷酸的浓度按重量计在0.5％和5％之间变化。
10.如权利要求7至9之一所述的方法，其特征为，有机溶剂是从包括乙醇和丙酮的组中选取的。
11.如权利要求7所述的方法，其特征为，在一段足以提供一按AES方法测量至多为100nm的绝缘涂层的时间内，将磷酸溶液喷射到铁基粉末上。
12.如权利要求7所述的方法，其特征为，在一段足以提供按重量计比基体粉末的含氧量最多高0.2％的粉末的含氧量的时间内，将磷酸溶液喷射到铁基粉末上。
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE9600724A SE9600724D0 (sv) | 1996-02-23 | 1996-02-23 | Iron based powder |
| SE96007240 | 1996-02-23 | ||
| SE9600725A SE9600725D0 (sv) | 1996-02-23 | 1996-02-23 | Manufacturing method |
| SE96007257 | 1996-02-23 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1211943A CN1211943A (zh) | 1999-03-24 |
| CN1223422C true CN1223422C (zh) | 2005-10-19 |
Family
ID=26662527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB97192452XA Expired - Lifetime CN1223422C (zh) | 1996-02-23 | 1997-02-19 | 经过磷化处理的铁粉及其制造方法 |
Country Status (14)
| Country | Link |
|---|---|
| US (1) | US6348265B1 (zh) |
| EP (1) | EP0881959B1 (zh) |
| JP (1) | JP4187266B2 (zh) |
| KR (1) | KR100454855B1 (zh) |
| CN (1) | CN1223422C (zh) |
| AT (1) | ATE248674T1 (zh) |
| AU (1) | AU714473B2 (zh) |
| BR (1) | BR9707648A (zh) |
| DE (1) | DE69724589T2 (zh) |
| ES (1) | ES2203784T3 (zh) |
| MX (1) | MX220648B (zh) |
| PL (1) | PL183359B1 (zh) |
| RU (1) | RU2176577C2 (zh) |
| WO (1) | WO1997030810A1 (zh) |
Families Citing this family (52)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3815563B2 (ja) | 2001-01-19 | 2006-08-30 | 株式会社豊田中央研究所 | 圧粉磁心およびその製造方法 |
| SE0102103D0 (sv) | 2001-06-13 | 2001-06-13 | Hoeganaes Ab | High density soft magnetic products and method for the preparation thereof |
| JP4060101B2 (ja) | 2002-03-20 | 2008-03-12 | 株式会社豊田中央研究所 | 絶縁皮膜、磁心用粉末および圧粉磁心並びにそれらの製造方法 |
| SE0203851D0 (sv) * | 2002-12-23 | 2002-12-23 | Hoeganaes Ab | Iron-Based Powder |
| SE0302427D0 (sv) * | 2003-09-09 | 2003-09-09 | Hoeganaes Ab | Iron based soft magnetic powder |
| US7494600B2 (en) * | 2003-12-29 | 2009-02-24 | Höganäs Ab | Composition for producing soft magnetic composites by powder metallurgy |
| SE0303580D0 (sv) * | 2003-12-29 | 2003-12-29 | Hoeganaes Ab | Composition for producing soft magnetic composites by powder metallurgy |
| JP2005213621A (ja) * | 2004-01-30 | 2005-08-11 | Sumitomo Electric Ind Ltd | 軟磁性材料および圧粉磁心 |
| CN102800455A (zh) * | 2004-03-31 | 2012-11-28 | 住友电气工业株式会社 | 软磁性材料及压粉铁心 |
| US7416578B2 (en) * | 2004-09-17 | 2008-08-26 | Höganäs Ab | Powder metal composition |
| CN101142044B (zh) * | 2005-01-25 | 2010-12-01 | 大冶美有限公司 | 含Mg氧化膜包覆的铁粉末 |
| RU2389099C2 (ru) | 2005-06-15 | 2010-05-10 | Хеганес Аб | Магнитно-мягкие композиционные материалы |
| US7824324B2 (en) | 2005-07-27 | 2010-11-02 | Neuronetics, Inc. | Magnetic core for medical procedures |
| WO2007036679A1 (en) * | 2005-09-30 | 2007-04-05 | Loughborough University Enterprises Limited | Method for preparing insulated particulate metals |
| CH698498B1 (de) * | 2006-03-31 | 2009-08-31 | Alstom Technology Ltd | Magnetische abschirmung im stirnbereich des stators eines drehstromgenerators. |
| TWI456599B (zh) * | 2006-12-07 | 2014-10-11 | Hoganas Ab Publ | 軟磁粉末 |
| CN101978579B (zh) * | 2008-03-19 | 2013-12-11 | 霍加纳斯股份有限公司 | 具有聚集通量的极片的永磁体转子 |
| BRPI0908975A2 (pt) * | 2008-03-20 | 2015-07-28 | Hoeganaes Ab Publ | Composição pulverizada ferromagnética e processo para sua produção |
| WO2009136854A1 (en) * | 2008-05-09 | 2009-11-12 | Höganäs Ab (Publ) | Method for improving the magnetic properties of a compacted and heat treated soft magnetic composite component |
| US8911663B2 (en) | 2009-03-05 | 2014-12-16 | Quebec Metal Powders, Ltd. | Insulated iron-base powder for soft magnetic applications |
| EP2513918B1 (en) | 2009-09-18 | 2016-07-13 | Höganäs AB | Ferromagnetic powder composition and method for its production |
| IN2012DN03313A (zh) | 2009-09-21 | 2015-10-23 | Hoganas Ab Publ | |
| EP2489683A4 (en) * | 2009-10-15 | 2015-03-18 | Toray Industries | METHOD FOR PRODUCING CORE-COAT PARTICLES, CORE-COAT PARTICLES AND PASTE COMPOSITION AND FILM COMPOSITION THEREWITH |
| KR20120106984A (ko) | 2009-12-21 | 2012-09-27 | 회가내스 아베 | 변조 극기용 회전자 |
| WO2011076579A1 (en) | 2009-12-21 | 2011-06-30 | Höganäs Ab (Publ) | Stator element for a modulated pole machine |
| EP2537165A1 (en) | 2010-02-18 | 2012-12-26 | Höganäs AB | Ferromagnetic powder composition and method for its production |
| EP2566639B1 (en) | 2010-05-07 | 2014-11-19 | Hoeganaes Corporation | Improved compaction methods |
| RU2433018C1 (ru) * | 2010-08-27 | 2011-11-10 | Трофимов Сергей Иванович | Способ получения железного порошка, содержащего фосфор |
| WO2012035044A1 (en) | 2010-09-17 | 2012-03-22 | Höganäs Ab (Publ) | Rotor for modulated pole machine |
| RU2013133838A (ru) | 2010-12-22 | 2015-01-27 | Хеганес Аб (Пабл) | Статор для машины с модулированными полюсами |
| JP2014505165A (ja) | 2010-12-23 | 2014-02-27 | ホガナス アクチボラグ （パブル） | 軟磁性粉末 |
| EP2509081A1 (en) | 2011-04-07 | 2012-10-10 | Höganäs AB | New composition and method |
| CN102218532B (zh) * | 2011-06-10 | 2013-04-24 | 莱芜钢铁集团粉末冶金有限公司 | 一种绝缘铁粉的生产设备和方法 |
| RU2465669C1 (ru) * | 2011-08-12 | 2012-10-27 | Геннадий Антонович Говор | Способ изготовления композиционного магнитно-мягкого материала |
| JP2015510389A (ja) | 2012-03-12 | 2015-04-02 | ホガナス アクチボラグ （パブル） | 電気機械用の固定子及び回転子 |
| RU2015101504A (ru) | 2012-06-20 | 2016-08-10 | Хеганес Аб (Пабл) | Ротор для модулируемой полюсной машины |
| WO2014095495A1 (en) | 2012-12-19 | 2014-06-26 | Höganäs Ab (Publ) | Inductor core |
| CN104871264B (zh) | 2012-12-19 | 2018-10-26 | 霍加纳斯股份有限公司 | 电感器和电感器芯 |
| CN103537700A (zh) * | 2012-12-31 | 2014-01-29 | 袁志刚 | 一种片状铝粉粉末涂料的生产方法 |
| DE102013200229B4 (de) * | 2013-01-10 | 2024-06-06 | Robert Bosch Gmbh | Verfahren zum Herstellen eines weichmagnetischen Verbundwerkstoffs |
| EP2787612A1 (en) | 2013-04-02 | 2014-10-08 | Höganäs AB (publ) | Flux switching modulated pole machine |
| WO2014184105A1 (en) | 2013-05-13 | 2014-11-20 | Höganäs Ab (Publ) | Inductor |
| EP3083106A1 (en) | 2013-12-20 | 2016-10-26 | Höganäs Ab (publ) | Soft magnetic composite powder and component |
| EP3083109B1 (en) | 2013-12-20 | 2019-10-23 | Höganäs AB (publ) | Soft magnetic powder mix |
| KR101730307B1 (ko) * | 2014-06-20 | 2017-04-25 | 소에이 가가쿠 고교 가부시키가이샤 | 탄소 피복 금속분말, 탄소 피복 금속분말을 함유하는 도전성 페이스트 및 이를 이용한 적층 전자부품 |
| EP3199264A1 (en) | 2016-02-01 | 2017-08-02 | Höganäs Ab (publ) | New composition and method |
| CN105742049A (zh) * | 2016-04-29 | 2016-07-06 | 成都锦粼科技有限公司 | 一种铁芯及其制作方法 |
| EP3576110A1 (en) | 2018-05-30 | 2019-12-04 | Höganäs AB (publ) | Ferromagnetic powder composition |
| JP2022522636A (ja) * | 2019-03-07 | 2022-04-20 | エイジェンシー・フォー・サイエンス，テクノロジー・アンド・リサーチ | 複合材及びその調製方法 |
| JP7347354B2 (ja) * | 2020-07-17 | 2023-09-20 | トヨタ自動車株式会社 | 圧粉磁心の製造方法 |
| KR102237022B1 (ko) | 2020-08-07 | 2021-04-08 | 주식회사 포스코 | 연자성 철계 분말 및 그 제조방법, 연자성 부품 |
| US20240029952A1 (en) * | 2020-12-04 | 2024-01-25 | Hengdian Group Dmegc Magnetics Co., Ltd | Integrated co-fired inductor and preparation method therefor |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2232352A (en) * | 1936-04-29 | 1941-02-18 | Rca Corp | Production of magnetic material |
| GB1046241A (en) | 1961-08-31 | 1966-10-19 | Secr Defence | Improvements in the production of iron powder having high electrical resistivity |
| US4177089A (en) * | 1976-04-27 | 1979-12-04 | The Arnold Engineering Company | Magnetic particles and compacts thereof |
| JPS5416664A (en) | 1977-06-08 | 1979-02-07 | Nippon Kinzoku Co Ltd | Reactor |
| US4601765A (en) * | 1983-05-05 | 1986-07-22 | General Electric Company | Powdered iron core magnetic devices |
| EP0434669B1 (en) * | 1984-09-29 | 1994-08-10 | Kabushiki Kaisha Toshiba | Method of making a coated magnetic powder and a compressed magnetic powder core |
| DE3439397A1 (de) * | 1984-10-27 | 1986-04-30 | Vacuumschmelze Gmbh, 6450 Hanau | Verfahren zur pulvermetallurgischen herstellung eines weichmagnetischen koerpers |
| SU1454573A1 (ru) * | 1987-07-17 | 1989-01-30 | Государственный научно-исследовательский институт химии и технологии элементоорганических соединений | Раствор дл фосфатировани порошка карбонильного железа |
| JP2602883B2 (ja) * | 1988-03-11 | 1997-04-23 | 株式会社メイト | 金属微粉末の表面処理方法 |
| RU2040810C1 (ru) * | 1992-08-27 | 1995-07-25 | Галина Анатольевна Дорогина | Способ получения магнито-мягкого материала |
| SE9401392D0 (sv) * | 1994-04-25 | 1994-04-25 | Hoeganaes Ab | Heat-treating of iron powders |
-
1997
- 1997-02-19 PL PL97328509A patent/PL183359B1/pl unknown
- 1997-02-19 CN CNB97192452XA patent/CN1223422C/zh not_active Expired - Lifetime
- 1997-02-19 AU AU22382/97A patent/AU714473B2/en not_active Expired
- 1997-02-19 ES ES97905537T patent/ES2203784T3/es not_active Expired - Lifetime
- 1997-02-19 RU RU98117805/02A patent/RU2176577C2/ru active
- 1997-02-19 AT AT97905537T patent/ATE248674T1/de active
- 1997-02-19 DE DE69724589T patent/DE69724589T2/de not_active Expired - Lifetime
- 1997-02-19 EP EP97905537A patent/EP0881959B1/en not_active Expired - Lifetime
- 1997-02-19 JP JP53006797A patent/JP4187266B2/ja not_active Expired - Lifetime
- 1997-02-19 KR KR19980706508A patent/KR100454855B1/ko not_active Expired - Lifetime
- 1997-02-19 BR BR9707648A patent/BR9707648A/pt not_active IP Right Cessation
- 1997-02-19 WO PCT/SE1997/000283 patent/WO1997030810A1/en active IP Right Grant
-
1998
- 1998-08-21 US US09/137,311 patent/US6348265B1/en not_active Expired - Lifetime
- 1998-08-24 MX MX9806871A patent/MX220648B/es unknown
Also Published As
| Publication number | Publication date |
|---|---|
| MX220648B (en) | 2004-05-28 |
| MX9806871A (en) | 1999-01-31 |
| PL183359B1 (pl) | 2002-06-28 |
| JP2000504785A (ja) | 2000-04-18 |
| WO1997030810A1 (en) | 1997-08-28 |
| CN1211943A (zh) | 1999-03-24 |
| KR19990087118A (ko) | 1999-12-15 |
| PL328509A1 (en) | 1999-02-01 |
| DE69724589D1 (de) | 2003-10-09 |
| BR9707648A (pt) | 1999-07-27 |
| RU2176577C2 (ru) | 2001-12-10 |
| ATE248674T1 (de) | 2003-09-15 |
| DE69724589T2 (de) | 2004-08-05 |
| AU714473B2 (en) | 2000-01-06 |
| EP0881959A1 (en) | 1998-12-09 |
| EP0881959B1 (en) | 2003-09-03 |
| US6348265B1 (en) | 2002-02-19 |
| AU2238297A (en) | 1997-09-10 |
| ES2203784T3 (es) | 2004-04-16 |
| JP4187266B2 (ja) | 2008-11-26 |
| KR100454855B1 (ko) | 2004-12-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1223422C (zh) | 经过磷化处理的铁粉及其制造方法 | |
| EP2147445B1 (en) | Soft magnetic powder | |
| US20230207168A1 (en) | Composite magnetic material and inductor using the same | |
| DE112009000263B4 (de) | Herstellungsverfahren für weichmagnetisches Material | |
| JP6265210B2 (ja) | リアクトル用圧粉磁心 | |
| EP3441989A1 (en) | Dust core coated with silica-based insulation, method for manufacturing same, and electromagnetic circuit component | |
| CN101233586A (zh) | 软磁性材料、软磁性材料的制造方法、压粉铁心以及压粉铁心的制造方法 | |
| JP2006225766A (ja) | 磁性鉄粉末の熱処理 | |
| JP2010196101A (ja) | 圧粉磁心用鉄基軟磁性粉末およびその製造方法、ならびに圧粉磁心 | |
| JP5372481B2 (ja) | 圧粉磁心及びその製造方法 | |
| CN1167089C (zh) | 复合磁性体及其制造方法 | |
| WO2012173239A1 (ja) | 圧粉磁心用鉄基軟磁性粉末およびその製造方法、ならびに圧粉磁心 | |
| CN1910706A (zh) | 软磁材料和压粉磁芯及其制备方法 | |
| Slovenský et al. | Preparation and characterization of fe based soft magnetic composites coated by SiO2 layer prepared by Stöber method | |
| US11948715B2 (en) | Magnetic composite | |
| JP2006183121A (ja) | 圧粉磁芯用鉄基粉末およびそれを用いた圧粉磁芯 | |
| EP1675137B1 (en) | Process for producing soft magnetism material | |
| JP2006278833A (ja) | 高強度、高磁束密度および高抵抗を有する複合軟磁性焼結材の製造方法 | |
| CN1931480A (zh) | 高磁导率铁粉芯的制造方法 | |
| JP2009185340A (ja) | 剥離型複水酸化物を使用した絶縁皮膜形成金属粉末及びその製造方法 | |
| JPH04160102A (ja) | 複合材料およびその製造方法 | |
| KR102831763B1 (ko) | 절연 코팅된 연자성 재료, 이의 제조방법, 연자성 복합체의 제조방법 및 이로부터 제조된 연자성 복합체 | |
| CA2247150C (en) | A low oxygen iron powder and method for the manufacturing thereof | |
| JP2009038256A (ja) | 圧粉磁心用鉄基軟磁性粉末および圧粉磁心 | |
| CN117649991A (zh) | 一种软磁复合材料粉体的制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20051019 |
|
| CX01 | Expiry of patent term |