• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Reduced iron powder that has fewer coarse inclusions, has excellent formability, has high porosity after sintering, has excellent reactivity per unit mass, and can be effectively used as reaction material even to the particle inside is provided. Reduced iron powder has an apparent density of 1.00 Mg/mto 1.40 Mg/m.
    公开号:SE1750827A1
    申请号:SE1750827
    申请日:2016-01-14
    公开日:2017-06-27
    发明作者:Machida Satoshi；Nakamura Naomichi
    申请人:Jfe Steel Corp；
    IPC主号:
    专利说明:

    [2] [0002] Two main types of iron powder based on its preparation method aretypically known: reduced iron powder; and atomized iron powder. Theapparent density of iron powder currently known is 2.3 Mg/m3 or more inreduced iron powder, and 2.5 Mg/mg or more in atomized iron powder. Thespecific surface area of iron powder is 0.10 mZ/g or less in reduced ironpowder, and 0.07 mZ/g or less in atomized iron powder.[0003] Iron powder having such characteristics has many uses, andparticularly its uses in chemical reaction material, sintered machine parts, etc.make up a high proportion. In chemical reaction material, large specificsurface area is required for efficient reaction. In sintered machine parts,high porosity is required as oilless bearings (which is also referred to as "oilretaining bearings").
    [4] [0004] The specific surface area is larger when the apparent density is lower.Iron powder with low apparent density is needed to produce sintered machineparts with high porosity.
    [5] [0005] As an example of sintered machine parts, an oilless bearing isdescribed below. It is important that the oilless bearing maintainsappropriate oil content. If the oil content is low, adequate lubricity anddurability cannot be obtained. To maintain appropriate oil content, thesintered body needs to be increased in porosity. JP 2001-132755 A (PTL 1)describes a relevant technique.
    [6] [0006] With reduction in size of machine parts, oilless bearings ofapproximately 2 mm in outer diameter and 0.6 mm in inner diameter havebeen produced in recent years. However, the use of conventional reducediron powder for smaller parts causes poor formability and poor yield rate because conventional reduced iron powder has coarse pores and iron portions, PO154754-PCT-ZZ (1/15) making production difficult. This has increased demand for iron powder thatis finer in microstructure, is more porous, and has fewer inclusions thanconventional iron powder.
    [7] [0007] If a part requires contacting with another part as in the case of abearing, the presence of inclusions in the part damages the other part andshortens the life of the product. Besides, in the case where the inclusions donot sinter with the surrounding iron powder, the inclusions cause structuraldefects. This significantly decreases the yield rate or the strength,particularly when producing small machine parts.
    [8] [0008] The Reduced iron powder is produced from iron ore or mill scale. “inclusions” mentioned here has the following meaning.The purity ofthe reduced iron powder as the product is determined by the purity of the ironThe most common impurity is oxygen. oxide as the raw material. Oxygen mostly appears as a thin film of surface oxide. Basic impurities include carbon, magnesium, aluminum, silicon, phosphorus, sulfur, chromium, manganese, nickel, and copper. Many of these impurities are present asoxides, and are called inclusions.[0009] For use in chemical reaction material, iron powder with large specificsurface area, i.e. low apparent density, is known to be useful as described inJP 4667835 B2 (PTL 2) and JP 4667937 B2 (PTL 3), given that larger specific surface area of powder contributes to more efficient reaction.
    [10] [0010] PTL 1: JP 2001-132755 APTL 2: JP 4667835 B2PTL 3: JP 4667937 B2 SUMMARY(Technical Problem)[0011] In the case of using conventional reduced iron powder to produce abearing, the shaft is damaged or the bearing develops structural defectsbecause the reduced iron powder contains inclusions exceeding 200 um.
    [12] [0012] Besides, in the production of bearings, there is a possibility that the PO154754-PCT-ZZ (2/15) circulation performance of lubricating oil cannot be obtained because, withreduction in size of bearings, pores or iron microstructure becomes largerelative to a bearing as mentioned above. In other words, althoughconventional reduced iron powder has fine pores, its many inclusions causethe product to fail. Bearings with inner diameter of 0.6 mm and outerdiameter of 2.0 mm can be produced at a relatively high yield rate even whenconventional reduced iron powder is used. In the case of producing smallerbearings, for example, with inner diameter of 0.4 mm and outer diameter of1.4 mm using conventional reduced iron powder, however, formability isinsufficient and the yield rate drops significantly, making mass productiondifficult.
    [13] [0013] Atomized iron powder is not suitable for use in the aforementionedsmall bearings, as its smooth surface causes insufficient bonding powerbetween iron powder particles during forming and leads to a significantlylower rattler value. Moreover, in the production of oilless bearings,atomized iron powder has a major drawback of having few pores andhindering sufficient circulation of oil. Atomized iron powder is alsoproblematic in that it has few fine pores, although its inclusions are few.[0014] From the perspective of using reduced iron powder as chemicalreaction material, the powder is required to have large specific surface area sothat the powder has excellent reactivity per unit mass and even the particleinside can be effectively used as reaction material.
    [15] [0015] As described above, reduced iron powder whose apparent density ismuch lower than 2.0 Mg/m3 and whose specific surface area is 0.2 m3/g ormore, which is much higher than 0.1 m3/g, is needed in order to producebearings with inner diameter of less than 0.6 mm and outer diameter of lessthan 2.0 mm at a high yield rate. Such reduced iron powder, however, cannotbe prepared by conventional production methods.
    [16] [0016] It could therefore be helpful to provide reduced iron powder that hasfewer coarse inclusions, has excellent formability, has high porosity aftersintering, has excellent reactivity per unit mass, and can be effectively used asreaction material even to the particle inside, a method for preparing the same, and a bearing produced from the reduced iron powder.
    [24] [0024] It is thus possible to obtain reduced iron powder that has fewer coarseinclusions, has excellent formability, has high porosity after sintering, hasexcellent reactivity per unit mass, and can be effectively used as reaction material even to the particle inside.
    [27] [0027] The following describes a method for preparing reduced iron powderaccording to one of the disclosed embodiments, with reference to FIG. 1.First, iron oxide powder (precursor iron oxide powder) having apredetermined mean particle size is agglomerated to obtain iron oxide powder.The obtained iron oxide powder is then classified and selected so that its meanparticle size is set to a predetermined range. After this, the iron oxidepowder is reduced with hydrogen gas (FezOg + 3H2 = 2Fe + 3H2O) and crushedas appropriate to obtain reduced iron powder (porous iron powder).
    [28] [0028] It is important to refine the precursor iron oxide powder as startingmaterial so that its mean particle size (D50) measured by a laser diffractionmethod is 3.0 um or less, in order to set the apparent density of the reducediron powder to 1.40 Mg/m3 or less to thus make the inclusions in the reducediron powder finer. The refinement makes pores smaller, which contributes tofiner inclusions. The mean particle size of the precursor iron oxide powderis preferably 2.0 um or less. No lower limit is placed on the mean particlesize ofthe precursor iron oxide powder, yet in industrial terms the lower limitis approximately 0.5 um.
    [29] [0029] An example of the method for preparing the precursor iron oxide PO154754-PCT-ZZ (5/15) powder is a method of neutralizing and extracting Waste acid after picklingsteel sheets in a steelworks. For example, a method using a spray roastingfurnace by the Ruthner process and a fluidized roasting method by the Lurgiprocess are available.
    [30] [0030] It is essential to agglomerate the precursor iron oxide powder to obtainiron oxide powder formed by the coagulation of the precursor iron oxidepowder. Effective methods of agglomerating the precursor iron oxidepowder include a method of mixing a binder and water into the precursor ironoxide powder using a Henschel mixer and drying the mixture, and a method ofdissolving the precursor iron oxide powder in water together with a binder toform slurry and then drying the droplets with hot air (spray dryer). In bothmethods, the binder may be PVA, starch, or the like.
    [31] [0031] When a vessel or a reducing furnace is charged with the iron oxidepowder to reduce the iron oxide powder, voids formed between coagulatedparticles ensure appropriate air permeability, thus facilitating the reduction.To achieve this, the mean particle size of the iron oxide powder after theagglomeration is important. Moreover, the particle size of the iron oxidepowder to be reduced correlates with the particle size of the reduced ironpowder. It is therefore preferable to classify and select the iron oxidepowder after the agglomeration to control its mean particle size, beforereducing the iron oxide powder. size of the after the
    [32] [0032] The mean particle iron oxide powder agglomeration is important, as mentioned above. However, not all particlesnecessarily maintain their shape. For example, a plurality of particles maybond with each other, or one particle may be broken. Accordingly, we madecareful examination, and discovered that the mean particle size of the reducediron powder effective in practical terms is 50 um to 100 um and, to achievethis, the mean particle size of the iron oxide powder is preferably 50 um to200 um. Thus, it is preferable to appropriately classify and select the ironoxide powder after the agglomeration so that its mean particle size is set to 50um to 200 um.
    [33] [0033] It is also preferable that the iron content in the iron oxide powder is68.8 mass% or more. This sufficiently reduces the amount of oxygen in the reduced iron powder, and further enhances the effect of improving chemical POl54754-PCT-ZZ (6/15) reactivity and the effect of producing high-strength bearings at a high yieldrate. No upper limit is placed on the iron content in the iron oxide powder,yet the upper limit is approximately 77 mass%.
    [34] [0034] The iron oxide powder after the agglomeration is reduced to obtainreduced iron powder (also simply referred to as iron powder). We discoveredthe conditions for preparing iron powder that has low apparent density, i.e.approximately half that of conventional reduced iron powder or atomized ironpowder, and in which inclusions are finely dispersed, by appropriatelymanaging the reduction temperature in this reduction step which is hydrogenreduction of iron oxide. It is important to set the reduction temperatureduring the reduction to 800 °C or more and 1000 °C or less. If the reductiontemperature is less than 800 °C, it is difficult to remove oxygen in the reducediron powder by reduction reaction. As a result, a large amount of oxygenremains in the iron powder. This causes insufficient chemical reactivity anddecreases formability, and leads to a lower yield rate in the production ofbearings. If the reduction temperature is more than 1000 °C, the sintering ofthe iron powder progresses and the apparent density exceeds 1.40 Mg/m3.This causes insufficient chemical reactivity, and leads to a lower yield rate inthe production of bearings.
    [35] [0035] The reduction time is preferably 120 min or more, to sufficientlyreduce iron oxide powder yielded from fine precursor iron oxide powder of3.0 um or less in mean particle size to obtain reduced iron powder of 1.00Mg/m3 to 1.40 Mg/m3 in apparent density. No upper limit is placed on thereduction time, yet the upper limit may be approximately 240 min in terms ofprocess efficiency.
    [36] [0036] The conditions other than the reduced iron powder preparationdescribed preparation conditions. conditions above may be well-known reduced iron powderAn example of the reduction method is a method of heating iron powder at atmospheric pressure using a belt furnace or the like in a reducing atmosphere such as hydrogen.
    [37] [0037] The following describes reduced iron powder according to one of the disclosed embodiments. The reduced iron powder has an apparent density of 1.00 Mg/m3 to 1.40 Mg/m3, and can be prepared by the preparation method described above for the first time. If the apparent density of the reduced iron PO154754-PCT-ZZ (7/15) powder is less than 1.00 Mg/m3, the specific surface area is excessively large,which increases the risk of a dust explosion, i.e. rapidly progressing reactionwith oxygen in the air. If the apparent density of the reduced iron powder ismore than 1.40 Mg/m3, chemical reactivity is insufficient. Besides, thestrength of the green compact decreases. This facilitates failures insubsequent steps, and leads to a lower yield rate in the production of bearings.[0038] When the apparent density of the reduced iron powder is in the rangeof 1.00 Mg/m3 to 1.40 Mg/m3, the green strength increases, and bearings canbe produced at a high yield rate. Moreover, by limiting the apparent densityto this range, coarse inclusions are effectiVely reduced, and the strength aftersintering is improved, thus contributing to higher bearing quality. Further,the reduced iron powder has excellent reactiVity per unit mass, and can beeffectiVely used as reaction material even to the particle inside. Theapparent density is measured according to JIS-Z-2504.
    [39] [0039] The amount of oxygen in the reduced iron powder is preferably 0.38mass% or less. This further enhances the effect of improving chemicalreactiVity and the effect of producing high-strength bearings at a high yieldrate. No lower limit is placed on the amount of oxygen in the reduced ironpowder, yet the lower limit is approximately 0.10 mass%.
    [40] [0040] Ifthe specific surface area ofthe reduced iron powder is less than 0.20mZ/g, iron powder particles characteristic of the disclosure are not formedsufficiently, leading to insufficient chemical reactiVity. The specific surfacearea of the reduced iron powder is therefore preferably 0.20 mZ/g or more.No upper limit is placed on the specific surface area of the iron powder, yetthe upper limit is preferably approximately 0.4 mZ/g in terms of handling andthe like. nitrogen gas.
    [41] [0041] A bearing can be produced from the reduced iron powder as rawmaterial. The bearing has an excellent yield rate in bearing production andexcellent strength and porosity, and has high chemical reactiVity, as describedin the following examples. The method for producing the bearing from thereduced iron powder as raw material may be a conventional method except that the reduced iron powder is used as raw material.
    [42] [0042] Table 1 compares conventional reduced iron powder (reduced ironpowder obtained through two reduction steps), conventional atomized ironpowder, and reduced iron powders (Comparative Examples 1 to 5, Examples 1to 4) obtained through the preparation process illustrated in FIG. 1. InComparative Examples 1 to 5 and Examples 1 to 4, hydrogen was used asreducing gas. The conventional reduced iron powder was prepared asfollows: Using iron ore or mill scale as raw material, coke powder was addedand primary reduction using a tunnel furnace was performed without anagglomeration step and a classification step in FIG. 1, and then reduction inthe thick-line box was performed.[0043] The iron powder evaluation items listed in Table 1 were evaluated asfollows.
    [46] [0046] The porosity is a factor determining the performance of an oillessbearing, and its appropriate value is 18% to 22%.The porosity was measured by mercury porosimetry.
    [47] [0047] The reaction rate in chemical reaction was evaluated based on thereaction in which sulfur content in soil adsorbed to iron (Fe + S = FeS).Adsorptivity by this reaction is required to be a predetermined level or morein practical terms. Accordingly, in Table l, chemical reactivity is set as anindex represented by a ratio to l as the minimum required level.
    [48] [0048] FIG. 2 illustrates an appearance image and cross-sectional image ofthe reduced iron powder of each of Examples 1 and 2, in comparison with theconventional reduced iron powder. The appearance image was taken using ascanning electron microscope (SEM), and the cross-sectional image was takenusing an optical microscope. Many pores were contained inside particles in Examples 1 and 2, as compared with the conventional reduced iron powder.
    [49] [0049] o ooïåm Û NN oN oo oo.o oo.o oo oo._ ooo ooN oo o.oo o.oo ooïåm N._ o_ 2 oo oo.o oN.o oo N_ ._ ooo ooN o__ N.oo o.No ooïåm Û oN oN oo oo.o oN.o oo oo._ ooo ooN oN_ o.oo o.NN ooïåm Û _N oN oo oN.o oN.o oo NÛ ooo_ ooN oN_ o.oo o.N_ ooïåm Û NN _N oo oN.o NN.o oo oÛ ooo_ ooN oo o.oo o.No ooooëom oêåooäoo o.o oN o_ No oo.o oo.o oo_ oo.o ooo ooN oNN o.oo o.N_. ooooëom oêåooäoo o.o o_ o_ oo _N.o NN.o oo oï ooo ooN oo o.oo o.No owoäoom oêåooäoo o.o oN o_ No oo.o oN.o oo oo.o ooo ooN oo_ o.oo NoN ooooëom oêåooäoo o.o _N 2 No oo.o _o.o oo oo.o ooo ooN oN_ o.oo o.N_ ooooëom oêåooäoo o.o oN o_ No NN.o oN.o oo_ oï ooo_ ooN oN_ o.oo o.N.oošoo oo... oëäooo . . oo.o oo _ .o_o..o_8..o>..oo o o oN o No oo ov 8 oo. o 8 oo 8 o.N - - - - -.oošoo oo... oooooo. . . o_ .o oo_ o.N_o..o_8..o>..oo o o o_ o_ oo 8 ov 8 oo.o 8 oo 8 N.No.åwæo . oo ä.. :o.oo oc. ...o ä.. .åšo ä.oxo _ ...o.o/c oxo oo.o oN.o m .oošoo .oošoo .oošoo ooäo.o N oooooo . ä. ëoo ošohoošoo oo.o .C äâoo .wooozo 8.: _o_o_> oooošw oëfioo . ooos oo... oo om: ooooo oo... .... oo... .oæoooš oooo 8....o...< ooäooo/o oouoooom ooooooomÉÉEQM .fioàooooo oooooomm :_32 ooofioom :_32 Éofiooo :ooo oNoo ooofioom :_32_ä_...o._ooonooooš oaäoo o.. wonwcoooozmö .oošoo oo... oooooo. oo wouwcoooozooo .oošoo oo... oooooo. .oo äoššoo ooäaoooxo _ ošfl Ref. No. PO154754-PCT-ZZ (11/15) _12-
    [50] [0050] Comparative Example 1 is iron powder obtained by reducing ironoxide powder at 1050 °C. Its apparent density was 1.48 Mg/m3, which isoutside the range according to the disclosure. While the degree of reductionwas relatively favorable, the yield rate in bearing production was evaluated asfail. The chemical reactivity was also evaluated as fail.
    [51] [0051] Comparative Example 2 is iron powder obtained by reducing ironoxide powder at 780 °C. Its apparent density was 0.98 Mg/m3, which isoutside the range according to the disclosure. The yield rate in bearingproduction and the chemical reactivity were evaluated as fail.
    [52] [0052] Comparative Example 3 is iron powder obtained using precursor ironoxide powder of 3.2 um in mean particle size and by reducing iron oxidepowder after agglomeration at 850 °C. Its apparent density was 0.95 Mg/m3,which is outside the range according to the disclosure. The degree ofreduction was relatively low. The yield rate in bearing production was poor,and the chemical reactivity was evaluated as fail.
    [53] [0053] Comparative Example 4 is reduced iron powder obtained using ironoxide powder after agglomeration of 45 um in mean particle size. Itsapparent density was 1.49 Mg/m3, which is outside the range according to thedisclosure. The degree of reduction was high, and the strength ofthe bearingwas evaluated as pass. Meanwhile, the yield rate in bearing production wasevaluated as fail. The chemical reactivity was also evaluated as fail.
    [54] [0054] Comparative Example 5 is reduced iron powder obtained using ironoxide powder after agglomeration of 220 um in mean particle size. Itsapparent density was 0.95 Mg/m3, which is outside the range according to thedisclosure. The strength of the bearing was evaluated as pass, but the yieldrate in bearing production was evaluated as fail. The porosity was excessive,and the chemical reactivity was evaluated as fail.
    [55] [0055] Example 1 is iron powder obtained using iron oxide powder afteragglomeration of 50 um in mean particle size and by reducing the iron oxidepowder after agglomeration at 1000 °C.The degree of reduction was high, and the yield rate in bearing production andthe strength and porosity of the bearing were all evaluated as pass. Thechemical reactivity was also favorable.
    [56] [0056] Example 2 is iron powder obtained using iron oxide powder afterRef. No. POl54754-PCT-ZZ (12/15) Its apparent density was 1.38 Mg/m3. _13- agg1on1eration of 120 uni in n1ean particle size and by reducing the iron oxidepowder after agg1on1eration at 1000 °C.The degree of reduction was faVorable, and the yield rate in bearingproduction and the strength and porosity of the bearing were all eValuated aspass. The chemical reactivity was also favorable.
    [57] [0057] Exaniple 3 is iron powder obtained using iron oxide powder afteragg1on1eration of 120 uni in n1ean particle size and by reducing the iron oxidepowder after agg1on1eration at 800 °C. Its apparent density was 1.03 Mg/n13.The degree of reduction was faVorable, and the yield rate in bearingproduction and the strength and porosity of the bearing were all eValuated aspass. The chen1ica1 reactivity was also favorable.
    [58] [0058] Exaniple 4 is iron powder obtained using iron oxide powder afteragg1on1eration having an iron content of 68.2 n1ass%. Its apparent densitywas 1.12 Mg/n13, while the amount of oxygen in the reduced iron powder was0.43 n1ass%. bearing production and the strength and porosity of the bearing were all The chen1ica1 reactiVity was faVorable, and the yield rate in eVa1uated as pass.
    [59] [0059] Exaniple 5 is iron powder obtained using precursor iron oxide powderof 0.7 uni in n1ean particle size, with the n1ean particle size of iron oxidepowder being 90 uni. Its apparent density was 1.05 Mg/n13. The chen1ica1reactiVity was faVorable, and the yield rate in bearing production and the strength and porosity of the bearing were all eValuated as pass.
    Ref. No. PO154754-PCT-ZZ (13/15) Its apparent density was 1.32 Mg/n13.
    权利要求:
    Claims (7)
    [1] 1. Reduced iron powder having an apparent density of 1.00Mg/nf to 1.40 Mg/m
    [2] 2. The reduced iron powder according to claim 1, having an amount of oxygen of 0.38 mass% or less.
    [3] 3. The reduced iron powder according to claim 1 or 2, having a specific surface area of 0.20 mZ/g or more.
    [4] 4. A method for preparing reduced iron powder, for use inpreparing the reduced iron powder according to any one of claims 1 to 3,comprising: agglomerating precursor iron oxide powder whose mean particle sizemeasured by a laser diffraction method is 3.0 um or less to obtain iron oxidepowder; and thereafter reducing the iron oxide powder at 800 °C to 1000 °C with hydrogen to obtain the reduced iron powder.
    [5] 5. The method for preparing reduced iron powder according toclaim 4, comprising classifying and selecting the iron oxide powder so that its meanparticle size measured by the laser diffraction method is 50 um to 200 um, before the reduction ofthe iron oxide powder.
    [6] 6. The method for preparing reduced iron powder according toclaim 4 or 5,wherein the iron oxide powder has an iron content of 68.8 mass% or IIIOTC.
    [7] 7. A bearing produced from the reduced iron powder according to any one of claims 1 to 3 as a raw material. Ref. No. PO154754-PCT-ZZ (14/15)
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    同族专利:
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    CN107107186A|2017-08-29|
    WO2016114142A1|2016-07-21|
    US20180221960A1|2018-08-09|
    CA2972864A1|2016-07-21|
    CN107107186B|2019-05-31|
    JPWO2016114142A1|2017-04-27|
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    引用文献:
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    CN1201021C|2001-02-14|2005-05-11|川崎制铁株式会社|Method for producing sponge iron, and reduced iron powder and method for production thereof|
    JP4667835B2|2004-11-25|2011-04-13|Ｊｆｅケミカル株式会社|Hydrogen generating medium and method for producing the same|
    JP4667937B2|2005-04-08|2011-04-13|ウチヤ・サーモスタット株式会社|Hydrogen generating medium and method for producing the same|CN108025357B|2015-09-18|2020-03-03|杰富意钢铁株式会社|Mixed powder for powder metallurgy, sintered body, and method for producing sintered body|
    KR101878604B1|2017-06-20|2018-07-13|현대자동차주식회사|Grinding method of deoxidated cake using laser-supersound measurement|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP2015005264|2015-01-14|
    PCT/JP2016/000170|WO2016114142A1|2015-01-14|2016-01-14|Reduced iron powder and method for preparing same and bearing|
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