1311507 玖、發明說明： 【發明所屬之技術領域】 本發明係關於在粉末冶金工業中有用之新金屬粉末组合 物。本發明亦關於藉使用這些組合物製備高密度金屬元件 之方法。 【先前技術】 藉使用♦分末冶I法製造結冑零件比全密集鋼之傳統相配 2相較有幾項優點。如此，能量消耗較低且材料利用率較 同。有利於粉末冶金路徑之另一重要因子為具網形或接近 網形之元件可在燒結過程後不需要耗廢成本之成形法（如 車錠、銑削、鏜孔或研磨）直接製造。然而，正常下全密集 岡材料比PM元件有卓越之機械性質。這主要由於pM元件中 孔隙之發生。因此，持續努力增加pM元件之密度以達到儘 可能接近全密集鋼之密度值之值。 在為達到較咼岔度之PM元件使用之方法中，粉末鍛造法 具有可得到全密集元件之優點。然而此法是耗成本的且主 要用l較重元件（如連接桿）之大量生產。全密集材料亦可由 壓力在高溫下（如在熱等靜壓，HIp)得到，但此法亦 為耗成本的。 藉使用暖壓緊’一種壓緊在提高之溫度（典型上在120至 25〇°C)下進行之方法，密度增加約〇_2 g/Cm3，這造成機械 性㊆ < 明顯改良。然而缺點為暖壓緊法包括额外之投資及 加工’其他方法（如雙重壓緒、雙重燒結、在提高之溫度下 燒結等）可進一步增加密度。這些方法亦將進一步增加製造 88878 1311507 成本因而減少整體成本之效率。 為了擴張粉末冶金成份之市場且利用粉末冶金技術之優 點’如此有完成具改良靜態及動態機械強度之高密度壓緊 物之簡單、較不昂貴之方法有需求。 【發明内容】 現在未預期地發現高密度元件可藉使用高壓緊壓力結合 新形式粉末組合物得到。這些组合物之特殊特徵為小於约 5 %之鐵或鐵基粉末之粒子大小小於4 5 μιη且該組合物包括 潤滑量之烷基烷氧基或聚乙醚烷氧基矽烷。本發明亦包括 由這些組合物製備濕及視需要燒結之壓緊物的方法。這方 法包括提供該組合物，視需要混合該組合物與石墨及其他 添加劑（如合金元素、機械加工性能改良劑等），單軸在高壓 力下壓緊模内之組合物及排出隨後可燒結之濕坯。 本發明之另一觀點關於具此形式秒燒結合各種粒子大小 之鐵或鐵基粉末（即結合傳統使用之粉末）。在此情況中亦可 得到相當高之密度。 【實施方式】 问被度」一詞意指具約至少7 3 g/cm3之密度的壓緊 物。「向密度」不是絕對值。根據單壓緊、單燒結元件之技 藝界水準可達到之典型密度為約7,1 g/cm3。藉使用暖壓緊 可知到約〇.2 g/cm3之增加。 ,?尤此而論「高密度」意指具約7.35-7.65 g/cm3及更高之密 度 < 壓緊物’視使用添加劑之形式及量與使用之鐵基粉末 之形式而足。具較低密度之元件當然亦可製造。但相信將 8S878 1311507 較不令人感與趣。 根據本毛明之鐵基粉末包括鐵基粉末（如水或氣體微粒 之鐵卷末、泡绵鐵粉末、還原鐵粉末）、部分擴散合金鋼粉 末及冗全合金鋼粉末。部分擴散合金鋼粉末以與Cu、Ni、 Mo之一或更多部分合金化之鋼粉末較佳。完全合金鋼粉末 以與 Mn、Cu、Ni、Cr、Mo、V、Co、W、Nb、Ti、Al、P、 S及B。不銹鋼粉末亦為令人感與趣的。 關於粒子形狀以如由水噴霧得到之不規則形式之粒子較 佳。海綿鐵粉末亦具有不規則形狀粒子且可為令人感與趣 的。 本發明之一項特徵為使用之粉末具有粗糙粒子（即粉末 基本上沒有微細粒子）。「基本上沒有微細粒子」意指小於 約5%之鐵或鐵基粉末粒子之大小&SS_EN 24 497描述之方 法測量小於45 μιη。到目前為止最有趣之結果以基本上由大 於約1 06 μιη之粒子（特是大於約212 μιη)組成之粉末達到。 「基本上由…組成」一詞意指至少40%之粒子粒子大小大 於1 0 ό μιη。以至少6 0 %大於2 1 2 μηι較佳。到目前為止以平均 粒子大小大於約2 1 2 μπι且只有小於5 %小於2 1 2 μπι之粉末得 到最佳之結果。最大粒子大小可為約2 mm。ΡΜ製造使用之 鐵基粉末之粒子大小分佈通常為平均粒子直徑在3 〇至1 〇 〇 μπι之範圍内且約10-30%小於45 μιη之高斯分佈。基本上無 微細粒子之鐵基粉末可藉移除粉末之較細部分或藉製造具 要求粒子大小分佈之粉末。 粒子大小分佈及粒子形狀在壓緊體之壓緊性質及性質上 88S78 1311507 之影響已徹底地研究。如此美國專利5,594，186號揭示一種 利用具三角形截面之基本上為線性、針狀金屬粒予製造密 度回於95%理論密度之pm元件之方法。具粗糙粒子之粉末 亦用於製造軟磁元件，如美國專利6 3〇9 748號及4 190 441 號中所揭示。 根據本發明以得到高密度產物之重要特徵為潤滑劑之形 式及量。如此已發現先前未使用之特定形式潤滑劑結合金 屬粉末給予非常有希望之結果。這些潤滑劑屬於烷基烷氧 基或聚醚矽烷之群且更特別地是烷基烷氧基或聚醚矽烷’ 其中在Si原子上至少一個取代基為具至少8個碳原子之烷 基，其中該烧基可被一或多個〇原子中斷，其中燒基包括一 或多個氧原子之根據本發明使用之化合物稱為聚醚矽烷。 烷基或聚醚基之鏈長為根據本發明使用之矽烷的重要特徵 且對矽烷之潤滑性質有影響。到目前為止已發現以具8至3〇 個碳原子得到最令人感興趣之結果，以1〇至24個碳原子較 佳。矽烷以選自由辛基三曱氧基矽烷、十六烷基三曱氧基 矽烷及具10個乙二醚基之聚乙二醚三曱氧基矽烷組成之 群。 就此而論可提及美國專利57663〇4、59893〇4、61 396⑻、 623 5076及645 1 Q82號揭示可使用極小量（即以欲壓緊之總組 。物重I计0.05或更少之％)之有機烷氧基矽烷作結合潤滑 劑之鐵或鐵基粉末之表面處理劑。在首四項美國專利中試驗 下列矽烷化合物：γ-甲丙烯氧丙基三曱氧基矽烷、γ_去水甘 油基氧丙基三甲氧基矽烷、Ν_β_(胺基乙基）_γ_三曱氧基矽 88878 1311507 烷、甲基三曱氧基矽烷、芬基（fenyl)三曱氧基矽烷及二苯 基一甲氧基矽烷。在美國專利0451082號中使用三苯基曱氧 基矽烷、二苯基二甲氧基矽烷、苯基三甲氧基矽烷、異丁 基二甲氧基矽烷及曱基三乙烷基矽烷。根據本發明使用之 具潤滑效應之有機矽烷的形式既未提及也未試驗。 根據本發明使用具潤滑效應之有機矽烷以溶解或分散在 通當溶劑（如有機溶劑，像丙酮或乙醇）中溶解或分散之方式 使用較佳。得到之溶液或分散物隨後在混合及視需要之加 熱時添加鐵基粉末，溶劑最後（視需要在真空中）蒸發。 根據本發明之較佳具體實施例及與粉末冶金中一般習用 相反的（傳統PM潤滑劑用於鐵粉末混合，或潤滑劑結合黏著 劑及/或表面處理使用，如參照上面美國專利中所敘述”鐵 或鐵基粉末不必在移入模具内前與分離之（傳統的）潤滑劑 混合。亦不必使用在壓緊進行前供給模壁潤滑劑之外潤滑 (才旲壁潤滑）。然而本發明在其令人感興趣時不排除利用傳統 内潤/S)(以重量计最兩〇 5 %之量），外潤滑或二者之組合的可 能性。 對一些應用添加微量石墨至欲壓緊之粉末混合物為必須 的。如此在壓緊前應添加以總混合物重量計0.1-1.0%之量之 石墨，以0.2-1.〇重量％較佳且以〇 3_〇 8重量％最佳。 在緊壓則可加至鐵基粉末之其他添加劑如包括Mn、Cu、 Νι、Cr、Mo、v、c〇、w、Nb、Τι、A卜 P、S及 B之合金 元素機械加工性成增強化合物、硬相材料及流動劑。 冋壓緊壓力」—詞意指約至少800 MPa之壓力。以較高 88878 -10- 1311507 之壓力（如高於900 MPa之壓力，以高於1〇〇〇較佳，以高於 1100 MPa更佳）得到更令人感興趣之結果。在高壓下文傳統 壓緊（即高於約800 MPa之壓力並傳統地使用包括較細粒子 之粉末）通常視為不適當的，因為由模具 二伴隨模具之高磨耗且元件之表面傾向較不= 損壞。藉使用根據本發明之粉末未預期地發現在高壓下（约 1000 MPa)排出力;減少且可得到具可接受或甚至完美之表 面0 壓緊可用心準裝備執行，這指執行新方法可不需要昂貴 <投資。|緊在環境或提高之溫度下單軸地執行，且以單 步驟較佳。另—選擇為壓緊可在振動機器（Hydropulsor型號 HYP 35_4)(幫助下執行，如專利公開案WO 02/38315中所 敍述。 燒結可在PM領域内正常使用之溫度（如u〇(M 14代低溫 或如120(M3〇(rc之較高溫度）及傳統使用之氣氛或真空下 進行。 同樣可應用濕或燒結元件之其他處理，如濕機械加工、 表面硬代、表面密實化、蒸氣處理。 簡言之使用根據本發明方法得到之優點為高密度 :可成本有效地製造。新方法亦允許使用傳統技術困難製 件之製造。此外可使用標準壓緊設備製造具可 接又甚至冗美表面成品之高密度壓緊物。 f通合由新方法製造產物之實例為高性能結構零件如連接 干凸輪I凸出部分、齒輪及受高負載之其他結構元件。 -11 - 1311507 藉使用不镑鋼粉末輪緣為特別令人感興趣的。 本奩明〈王要目的為完成高密度產物。具潤滑效應之兮 垸已特別地與粗糙粉末相關連敘述。然而亦發現這些錢 亦可結合包括車交高量之細粒子之粉末(即今天傳統上用於 PM工業中（粉末式）使用。下面實例4指述根據本發明之秒 烷在傳統粉末及粗糙粉末上之效應。如所見亦以包括較高 里之細粒子:C傳統粉末得到極高之密度。包括具一般粒子 大小分佈之鐵或鐵基粉末與根據本發明之矽烷的組合物對 某些應用可為特別令人感與趣的且亦在本發明之範圍内。 本發明進一步以下列實例描述。 實例1 由Astaloy Mo製備鐵基粉末組合物，其為可購自瑞典 H0ganas ABhls重量％之鉬合金化之預合金鐵基粉末且 此處小於212 μιη之粒子已除去。分別與〇丨及〇 15%之十六 垸基三甲氧基矽烷混合。混合過程如下進行： 十TTfe基二曱基矽烷在乙醇中稀釋至以重量計2〇%之溶 液，且溶液攪拌60分鐘。在混合時分別加〇」及〇丨5重量％ ;量之溶液至先前在混合器内加熱至751.之鐵基粉末混合 物。在相同之混合器内執行徹底之混合3分鐘隨後在低速混 合3 0分鐘並在真空中以揮發溶劑。得到之混合物以5〇〇 μιη 之篩篩選。 具35 mm之内直徑及14 mm之外直徑及〗〇 mm之高之環在 不同之壓緊壓力下以單一步驟單軸地壓緊。如圖所見在 1100 MPa之壓力下二組合物均得到7 67 g/cm3之濕密度。由 88878 -12- 1311507 ’、。。沙广製備〈®緊物排出需要之總能量稍為低於 已由重量％〈硬燒處理之粉末製備壓緊物排出需要之始 能量，見圖1-2。 實例2 使用λ例1中之相同粉末之相同步驟，除了粉末與〇 2 重量％之十六烷基三甲氧基矽垸混合之外。製備二種組a 物，一種具有0.2重量％之石墨且另一種具有〇6重量％之石 墨。測量濕密度及濕強度。 如圖2-2所見到，在12〇〇MPa下壓緊之含〇2%石墨之濕元 · 件得到7.65 g/cm3之濕密度。含〇 6%之石墨之濕元件則得到 7.58 g/cm3之濕密度。 圖2-1顯示強度隨壓緊壓力之增加而增加且濕強度高到 足以允許處理濕元件。 實例3 本實例顯示除去鐵基粉末之不同碎片之效應。試驗四種 不同鐵基粉末組合物。其中三種鐵基粉末組合物含有包括鲁 0.2%十7T垸基三甲氧基碎燒之Astaloy Mo並使用實例1中之 混合步驟。第一種组合物含有比45 μιη粗糙之Astaloy Mo， 第二種組合物含有比106 μπι粗較之Astaloy Mo且第三種組 合物含有比212 μιη之Astaloy Mo。第四種组合物含有具比 2 12 μιη粗糙之粒子的Astaloy Mo。此組合物之粒子與〇 1重 量％之十六烷基三曱氧基矽燒混合。此外，所有組合物含 有0.2%之石墨。所有組合物在模具内以單~步驟單軸地壓 緊，形成外直徑35 mm、内直徑14 mm且高10 mm之環。 -13 - H8878 1311507 圖3 -1顯示隨粒子大小增加濕密度增加且排出力減少。 圖3-2顯示當矽烷之量由0.1至〇2重量％增加時排出力減 少。 ίΜΑ ' 此實例證實烷基或聚醚基之鏈長、粒子大小分佈及矽烷 之添加量在以高壓壓緊後排出時之潤滑性質上之效應。使 用二種粉末’即標準100網目鐵基粉末，具約20%小於45 μπ1 (S-粉末）之粒子的Astaloy 85 Mo，以及具相同化學組成而沒 有微細粒子且重量平均粒子大小為約212 μπι (c_粉末）之粉 末。 使用根據表a)之五種不同種類之梦燒 A 甲基三曱氧基矽烷 B 丙基三曱氧基碎燒 C 辛基三曱氧基矽燒 D 十六烷基三曱氧基矽烷 E 具10個乙二醚基之聚乙二醚三曱氧基矽烷 加不同量之矽烷至鐵基粉末且得到之混合物單軸壓縮機 械裝置中在1100 MPa下壓緊形成直徑25 mm且高12 mm之金 屬小塊。在排出時測量動態排出力並在排出後評價濕表面 且測量密度，如表中所示： 88878 •14- 13115071311507 发明, DESCRIPTION OF THE INVENTION: TECHNICAL FIELD OF THE INVENTION The present invention relates to novel metal powder compositions useful in the powder metallurgy industry. The invention also relates to a method of making high density metal components by using these compositions. [Prior Art] There are several advantages to the use of the ♦ 末 冶 I I method to make the knot parts more than the traditional dense steel. As such, energy consumption is lower and material utilization is the same. Another important factor that favors the powder metallurgy path is that the meshed or nearly meshed components can be fabricated directly without the costly forming process (e.g., ingot, milling, boring or grinding) after the sintering process. However, normally under-dense materials have superior mechanical properties than PM components. This is mainly due to the occurrence of voids in the pM element. Therefore, efforts continue to increase the density of pM components to achieve values that are as close as possible to the density of fully dense steel. Among the methods used to achieve a higher degree of PM element, the powder forging method has the advantage of obtaining a fully dense element. However, this method is costly and is mainly produced in large quantities using heavy components such as connecting rods. Fully intensive materials can also be obtained by high pressures (e.g., in hot isostatic pressing, HIp), but this method is also costly. By using a warm pressing method, a method of compacting at an elevated temperature (typically 120 to 25 ° C), the density is increased by about 〇 2 g/cm 3 , which results in a mechanical improvement. However, the disadvantage is that the warm compression method includes additional investment and processing. Other methods (such as double press, double sintering, sintering at elevated temperatures, etc.) can further increase the density. These methods will also further increase the cost of manufacturing 88878 1311507 and thus reduce overall costs. In order to expand the market for powder metallurgy components and utilize the advantages of powder metallurgy technology, there is a need for a simple, less expensive method of accomplishing high density compacts with improved static and dynamic mechanical strength. SUMMARY OF THE INVENTION It has now unexpectedly been found that high density components can be obtained by combining high pressure compaction pressure with a new form of powder composition. A particular feature of these compositions is that less than about 5% of the iron or iron based powder has a particle size of less than 4<5>> and the composition comprises a lubricating amount of alkylalkoxy or polyether alkoxydecane. The present invention also encompasses a process for preparing wet and optionally sintered compacts from these compositions. The method comprises providing the composition, mixing the composition with graphite and other additives (such as alloying elements, machinability improvers, etc.) as needed, singulating the composition in the mold under high pressure and discharging and subsequently sintering Wet blank. Another aspect of the present invention pertains to iron or iron-based powders of various particle sizes in combination with this form (i.e., in combination with conventionally used powders). A relatively high density can also be obtained in this case. [Embodiment] The term "degree of care" means a compact having a density of at least about 7 3 g/cm3. "To density" is not an absolute value. A typical density achievable according to the art level of a single compression, single sintered component is about 7,1 g/cm3. By using the warm compression, an increase of about 2 g/cm3 is known. In particular, "high density" means a density of about 7.35-7.65 g/cm3 and higher <compacts' depending on the form and amount of the additive used and the form of the iron-based powder used. Components with lower density can of course also be manufactured. But I believe that 8S878 1311507 is less interesting. The iron-based powder according to the present invention includes iron-based powders (e.g., iron or gas particles of iron ore, foamed iron powder, reduced iron powder), partially diffused alloy steel powder, and redundant alloy steel powder. The partially diffused alloy steel powder is preferably a steel powder alloyed with one or more of Cu, Ni, Mo. Complete alloy steel powder with Mn, Cu, Ni, Cr, Mo, V, Co, W, Nb, Ti, Al, P, S and B. Stainless steel powder is also interesting. It is preferred that the particle shape is in the form of particles in an irregular form as obtained by water spray. Sponge iron powder also has irregularly shaped particles and can be interesting. A feature of the invention is that the powder used has coarse particles (i.e., the powder is substantially free of fine particles). "Substantially free of fine particles" means less than about 5% of the size of iron or iron-based powder particles & SS_EN 24 497. The method described is less than 45 μηη. The most interesting result to date is achieved with a powder consisting essentially of particles larger than about 106 μηη (especially greater than about 212 μηη). The term "consisting essentially of" means that at least 40% of the particles have a particle size greater than 10 ό μιη. It is preferably at least 60% greater than 2 1 2 μηι. The best results have been obtained so far with powders having an average particle size greater than about 2 1 2 μπι and only less than 5% less than 2 1 2 μπι. The maximum particle size can be about 2 mm. The particle size distribution of the iron-based powder used in the manufacture of yttrium is generally a Gaussian distribution having an average particle diameter in the range of 3 〇 to 1 〇 〇 μπι and about 10-30% less than 45 μηη. An iron-based powder substantially free of fine particles may be obtained by removing a finer portion of the powder or by making a powder having a desired particle size distribution. The effect of particle size distribution and particle shape on the compression properties and properties of the compression body has been thoroughly investigated. Thus, U.S. Patent No. 5,594,186 discloses the use of a substantially linear, acicular metal particle having a triangular cross section to produce a pm element having a density back to 95% theoretical density. Powders with coarse particles are also used in the manufacture of soft magnetic components, as disclosed in U.S. Patent Nos. 6,300,748 and 4,190,441. An important feature of obtaining a high density product in accordance with the present invention is the form and amount of lubricant. It has thus been found that the particular form of lubricant previously used in combination with the metal powder gives very promising results. These lubricants belong to the group of alkylalkoxy or polyether decanes and more particularly alkylalkoxy or polyether decanes wherein at least one substituent on the Si atom is an alkyl group having at least 8 carbon atoms, Wherein the alkyl group can be interrupted by one or more deuterium atoms, wherein the compound used in accordance with the invention comprising one or more oxygen atoms is referred to as a polyether decane. The chain length of the alkyl or polyether group is an important feature of the decane used in accordance with the present invention and has an effect on the lubricating properties of the decane. It has been found so far that the most interesting result is obtained with 8 to 3 carbon atoms, preferably 1 to 24 carbon atoms. The decane is a group selected from the group consisting of octyltrimethoxy decane, hexadecyltrimethoxy decane, and polyethylene glycol trioxane decane having 10 ethylene ether groups. In this connection, reference may be made to U.S. Patents 57,663,4,59,893,4, 61,396 (8), 623 5076, and 645 1 Q82, which disclose the use of very small amounts (i.e., in the total group to be compacted, weight I, 0.05 or less). The organoalkoxydecane of %) is used as a surface treatment agent for iron or iron-based powders in combination with a lubricant. The following decane compounds were tested in the first four U.S. patents: gamma-methacryloxypropyltrimethoxy decane, gamma-dehydroglyceryloxypropyltrimethoxynonane, Ν_β_(aminoethyl)_γ_triazine Oxygen 矽 88878 1311507 alkane, methyl trimethoxy decane, fenyl trimethoxy decane and diphenyl monomethoxy decane. Triphenylphosphonium decane, diphenyldimethoxydecane, phenyltrimethoxydecane, isobutyldimethoxydecane and mercaptotriethanedecane are used in U.S. Patent No. 4,051,082. The form of the organic decane having a lubricating effect used in accordance with the present invention is neither mentioned nor tested. It is preferred to use the organic decane having a lubricating effect in accordance with the present invention to dissolve or disperse in a solvent (e.g., an organic solvent such as acetone or ethanol). The resulting solution or dispersion is then added with an iron-based powder upon mixing and, if desired, heating, and the solvent is finally evaporated (as needed in a vacuum). In accordance with a preferred embodiment of the present invention and in contrast to conventional practice in powder metallurgy (conventional PM lubricants are used for iron powder mixing, or lubricants in combination with adhesives and/or surface treatments, as described in the above U.S. Patent "The iron or iron-based powder does not have to be mixed with the separated (conventional) lubricant before it is moved into the mold. It is also not necessary to use lubrication outside the mold wall lubricant before the compaction is carried out. It is interesting to exclude the possibility of using traditional internal moist/S) (up to 5% by weight), external lubrication or a combination of the two. Add traces of graphite to some applications to compact A powder mixture is necessary. Thus, a graphite in an amount of from 0.1 to 1.0% by weight based on the total mixture should be added before compression, preferably from 0.2 to 1.% by weight and most preferably from 〇3 to 8% by weight. Other additives such as Mn, Cu, Νι, Cr, Mo, v, c〇, w, Nb, Τ, A, P, S, and B, which are added to the iron-based powder, can be mechanically strengthened. Compounds, hard phase materials and flow agents. "- the word means about the pressure of at least 800 MPa. At higher pressures of 88878 -10- 1311507 (eg, pressures above 900 MPa, preferably above 1 ,, more preferably above 1100 MPa) give more interesting results. Conventional compaction under high pressure (i.e., pressures above about 800 MPa and conventional use of powders comprising finer particles) is generally considered to be inadequate because of the high wear of the mold accompanying the mold and the tendency of the surface of the component to be less = damage. Unexpectedly, the discharge force under high pressure (about 1000 MPa) is found by using the powder according to the present invention; the reduction and the availability of an acceptable or even perfect surface 0 compaction can be performed by the standard equipment, which means that the implementation of the new method may not be required. Expensive &investment; | Performing uniaxially at ambient or elevated temperatures, and preferably in a single step. Alternatively—selection for compression can be performed with the help of a vibrating machine (Hydropulsor model HYP 35_4), as described in patent publication WO 02/38315. Sintering can be used normally in the PM field (eg u〇 (M 14 Generation of low temperature or as 120 (M3 〇 (higher temperature of rc) and conventionally used atmosphere or vacuum. Other treatments of wet or sintered components can also be applied, such as wet machining, surface hardening, surface densification, steam In short, the advantages obtained using the method according to the invention are high density: it can be produced cost-effectively. The new method also allows the manufacture of difficult parts using conventional techniques. In addition, it can be made using standard compression equipment. High-density compacts for finished surfaces. f Examples of products manufactured by new methods are high-performance structural parts such as connecting dry cam I projections, gears and other structural components subject to high loads. -11 - 1311507 The non-pound steel powder rim is of particular interest. Ben Mingming [Wang wants to complete high-density products. The lubrication effect has been specifically associated with rough powders. However, it has also been found that the money can also be combined with the powder comprising a high amount of fine particles (i.e., conventionally used in the PM industry (powder type). Example 4 below refers to the sulane according to the present invention in conventional powders and The effect on the rough powder. As can be seen, the density of the fine particles including the higher ones is obtained: C. The conventional powder obtains a very high density. The composition comprising iron or iron-based powder having a general particle size distribution and the decane according to the present invention is Some applications may be particularly interesting and are also within the scope of the invention.The invention is further described by the following examples.Example 1 An iron-based powder composition prepared from Astaloy Mo, which is commercially available from HGganas ABhls, Sweden, wt% The molybdenum alloyed prealloyed iron-based powder and wherein less than 212 μηη particles have been removed, respectively, mixed with 〇丨 and 〇 15% of hexadecanyltrimethoxy decane. The mixing process is carried out as follows: Ten TTfe base 曱The decane is diluted in ethanol to 2% by weight of the solution, and the solution is stirred for 60 minutes. When mixing, 〇 and 〇丨 5% by weight respectively; the amount of the solution is previously heated to 7 in the mixer. 51. Iron-based powder mixture. Thorough mixing was carried out in the same mixer for 3 minutes and then mixed at low speed for 30 minutes and in a vacuum to evaporate the solvent. The resulting mixture was sieved through a 5 〇〇μη sieve. The inner diameter and the outer diameter of 14 mm and the height of 〇mm are uniaxially compressed in a single step under different compression pressures. As shown, the two compositions obtained 7 67 g at a pressure of 1100 MPa. The wet density of /cm3. From 88878 -12- 1311507 ',.. The total energy required for the preparation of the tightness of the product is slightly lower than the initial energy required for the preparation of the compacted material by the weight percent of the hard-burned powder. , see Figure 1-2. Example 2 The same procedure as in the same powder of Example 1 was used except that the powder was mixed with 〇 2% by weight of cetyltrimethoxyindole. Two groups of a, a graphite having 0.2% by weight of graphite and the other having 6% by weight of graphite were prepared. Wet density and wet strength were measured. As seen in Fig. 2-2, the wetted material containing 2% graphite at 12 MPa was obtained at a wet density of 7.65 g/cm3. A wet component containing 6% graphite has a wet density of 7.58 g/cm3. Figure 2-1 shows that the strength increases as the compression pressure increases and the wet strength is high enough to allow the wet component to be processed. Example 3 This example shows the effect of removing different fragments of an iron-based powder. Four different iron-based powder compositions were tested. Three of the iron-based powder compositions contained Astaloy Mo including Lu 0.2% of 10 7-decyltrimethoxycalcin and the mixing procedure of Example 1 was used. The first composition contained Astaloy Mo which was coarser than 45 μηη, the second composition contained Astaloy Mo which was thicker than 106 μπι and the third composition contained Astaloy Mo of 212 μηη. The fourth composition contains Astaloy Mo having a coarser than 2 12 μηη. The particles of this composition were mixed with 1% by weight of cetyltridecyloxy oxime. In addition, all compositions contained 0.2% graphite. All compositions were uniaxially compressed in a single step in a mold to form a ring having an outer diameter of 35 mm, an inner diameter of 14 mm and a height of 10 mm. -13 - H8878 1311507 Figure 3-1 shows that as the particle size increases, the wet density increases and the discharge force decreases. Fig. 3-2 shows that the discharge force is reduced when the amount of decane is increased from 0.1 to 〇2% by weight. ΜΑ ' This example demonstrates the chain length of the alkyl or polyether group, the particle size distribution, and the effect of the amount of decane added on the lubricating properties when discharged under high pressure. Using two powders, a standard 100 mesh iron-based powder, Astaloy 85 Mo with about 20% less than 45 μπ1 (S-powder) particles, and the same chemical composition without fine particles and a weight average particle size of about 212 μπι (c_powder) powder. Use five different types of dreams according to Table a) to burn A methyltrimethoxy decane B propyl trimethoxy cleavage C octyl tridecyloxy oxime D cetyltrimethoxy decane E 10 ethylene glycol ether-containing polyethylene glycol trimethoxy decane plus different amounts of decane to iron-based powder and the mixture obtained is compacted at 1100 MPa to form a diameter of 25 mm and a height of 12 mm in a uniaxial compression mechanism. Small pieces of metal. The dynamic discharge force was measured at the time of discharge and the wet surface was evaluated after discharge and the density was measured as shown in the table: 88878 • 14-1311507
ΟΚΒ?3·^/»^^!^'®】 命鶴-it丰_S1&丝til妗捋缚命蘇) > a Ο ΓΠ 矽烷 Seizure 丨 O V s 粉末 c 62 kN OK 7,67 g/cm3 o s 粉末 c 48 kN OK 7,65 g/cm3 39 kN OK 7,66 fi/cin3 |03l°/〇 粉末 c 46 kN OK 7,66 g/cm3 39 kN OK 7,67 : g/cm3 i 10,2% I η麥 > 47 kN OK 7,63 g/cm3 65 kN OK 7,6 i g/cm3 10,2% Ί ?末 Seizure \ Seizure 1 ； I_ Seizure 36 kN OK 7,64 •t g/cm 33 kN OK 7,66 g/cm'1 η举 > 34 kN OK 7,62 gfcm3___ 38 kN OK 7,63 g/cm3 δ 粉末 s_! 37 kN OK 7,60 g/cm5 ο 式 > 66 kN OK 7,60 g/cm3 Ο 粉末 S 97 kN* OK 7,53 ig/cm3 29 kN OK 7,56 g/cm3 Ο 粉末 SΟΚΒ?3·^/»^^!^'®] Life Crane-it Feng_S1& silk til妗捋 binding life) > a Ο 矽 矽 Se Seizure 丨 OV s powder c 62 kN OK 7,67 g/ Cm3 os powder c 48 kN OK 7,65 g/cm3 39 kN OK 7,66 fi/cin3 |03l°/〇 powder c 46 kN OK 7,66 g/cm3 39 kN OK 7,67 : g/cm3 i 10 , 2% I η麦> 47 kN OK 7,63 g/cm3 65 kN OK 7,6 ig/cm3 10,2% Ί ?End Seizure \ Seizure 1 ; I_ Seizure 36 kN OK 7,64 •tg/cm 33 kN OK 7,66 g/cm'1 η举> 34 kN OK 7,62 gfcm3___ 38 kN OK 7,63 g/cm3 δ powder s_! 37 kN OK 7,60 g/cm5 ο 式 > 66 kN OK 7,60 g/cm3 Ο Powder S 97 kN* OK 7,53 ig/cm3 29 kN OK 7,56 g/cm3 Ο Powder S
88878 -15 - 1311507 中斤見到，需要烷烯鏈中至少8個原子之鏈長以成功 地排出添加〇·〇5·〇 5%之發燒之元件。咸信添加量高於 因廣7C件〈密度受負面地影響較不令人感與趣的。此表示 ’’>、丁矽认含里小於〇 〇5%時對鏈長3〇個碳原子之矽烷排出 而不損壞元件或模具表面為不可能的。 由上表亦可下結論為具標準粒子大小分佈之粉末可壓緊 成7.60 g/cm3及更高之高密度，並成功地排出，供給其添加 教（量小於0.5%且上述垸歸或聚乙二鍵鏈之長度大於8 個原子。- 【圖式簡單說明】 圖1-1顯不1100 MPa之壓力下二組合物均得到7 67 g/cm3 之濕密度。 圖1-2顯不由〇.1重量％之矽烷處理之粉末製備壓緊物排 出需要之總能量。 圖2-1顯示強度隨壓緊壓力之增加而增加且濕強度高到 足以允許處理濕元件。 圖2-2顯示在1200 MPa下壓緊之含〇·2%石墨之濕元件得 到7.65 g/cm3之濕密度。 圖3 -1顯示隨粒子大小增加濕密度增加且排出力減少。 圖3-2顯示當矽烷之量由0.1至〇.2重量％增加時排出力減 少、〇 88878 -16 -88878 -15 - 1311507 In the case of Zhong Jin, the chain length of at least 8 atoms in the alkylene chain is required to successfully discharge the component with 5% 发 〇 5% of the fever. The amount of salty letters added is higher than that of the 7C pieces. The density is less affected by the negative influence. This means that ’’>, in the case of Ding 矽, is less than 〇 〇 5%, and it is impossible to discharge decane having a chain length of 3 碳 carbon atoms without damaging the surface of the element or the mold. From the above table, it can also be concluded that the powder with the standard particle size distribution can be compacted to a high density of 7.60 g/cm3 and higher, and successfully discharged, and supplied with additional teaching (the amount is less than 0.5% and the above-mentioned Zigui or poly The length of the B bond chain is greater than 8 atoms.- [Simple description of the figure] Figure 1-1 shows that the two compositions all get a wet density of 7 67 g/cm3 under the pressure of 1100 MPa. .1% by weight of decane-treated powder to prepare the total energy required for the compact to be discharged. Figure 2-1 shows that the strength increases with increasing compression pressure and the wet strength is high enough to allow the wet component to be processed. Figure 2-2 shows A wet component containing 〇·2% graphite compacted at 1200 MPa gives a wet density of 7.65 g/cm3. Figure 3-1 shows an increase in wet density and a decrease in discharge force as the particle size increases. Figure 3-2 shows the amount of decane When the increase is from 0.1 to 〇.2% by weight, the discharge force is reduced, 〇88878 -16 -