TW202202251A - Metal composite - Google Patents
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- TW202202251A TW202202251A TW110104684A TW110104684A TW202202251A TW 202202251 A TW202202251 A TW 202202251A TW 110104684 A TW110104684 A TW 110104684A TW 110104684 A TW110104684 A TW 110104684A TW 202202251 A TW202202251 A TW 202202251A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
- B23B27/18—Cutting tools of which the bits or tips or cutting inserts are of special material with cutting bits or tips or cutting inserts rigidly mounted, e.g. by brazing
- B23B27/20—Cutting tools of which the bits or tips or cutting inserts are of special material with cutting bits or tips or cutting inserts rigidly mounted, e.g. by brazing with diamond bits or cutting inserts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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Abstract
Description
本發明係關於一種金屬組成物。本案主張2020年2月13日於日本提出申請之特願2020-022348號之優先權,其內容藉由引用併入本文中。The present invention relates to a metal composition. This case claims the priority of Japanese Patent Application No. 2020-022348 filed in Japan on February 13, 2020, the contents of which are incorporated herein by reference.
以往,於進行形成有半導體裝置或電子零件之半導體晶圓之切割、金屬或陶瓷之切削加工、挖削、研磨、研削等切削對象構件之加工時,例如有時會使用採用微米尺寸之金剛石粒子作為研磨粒之工具。作為上述工具,例如已知有使用金剛石燒結體之工具,該金剛石燒結體具有第1金剛石粒子群及第2金剛石粒子群,第1金剛石粒子群之平均粒徑為50 μm以上,且為第2金剛石粒子群之平均粒徑之5倍以上,黏合相至少具有鐵族金屬(參照專利文獻1)。 [先前技術文獻] [專利文獻]Conventionally, for example, micron-sized diamond particles have been used in the dicing of semiconductor wafers on which semiconductor devices or electronic components are formed, cutting of metals or ceramics, digging, grinding, grinding, and other processing of objects to be cut. As a tool for abrasive particles. As the above-mentioned tool, for example, there is known a tool using a diamond sintered body having a first diamond particle group and a second diamond particle group, the average particle diameter of the first diamond particle group being 50 μm or more, and the second diamond particle group being 50 μm or more. The average particle size of the diamond particles is 5 times or more, and the binder phase has at least an iron group metal (see Patent Document 1). [Prior Art Literature] [Patent Literature]
[專利文獻1]日本特開2010-228073號公報[Patent Document 1] Japanese Patent Laid-Open No. 2010-228073
[發明所欲解決之課題][The problem to be solved by the invention]
於欲使用採用金剛石研磨粒之以往工具高速進行切削加工之情形時,考慮使用大尺寸之金剛石研磨粒。然而,於使用大尺寸之金剛石研磨粒之情形時,存在切削對象物產生之碎片(切屑)變大之問題。In the case of high-speed cutting with conventional tools using diamond abrasive grains, consider using large-sized diamond abrasive grains. However, when large-sized diamond abrasive grains are used, there is a problem that chips (chips) generated from the cutting object become large.
因此,本發明之目的在於提供一種金屬組成物,其能夠獲得可抑制進行切削對象構件之加工時所產生之切屑之工具。 [解決課題之技術手段]Therefore, an object of the present invention is to provide a metal composition capable of obtaining a tool capable of suppressing chips generated when machining a member to be cut. [Technical means to solve the problem]
本發明之發明人為了實現上述目的而進行了潛心研究,結果發現,根據含有金屬、奈米金剛石粒子及微米金剛石粒子之金屬組成物,於使用上述金屬組成物進行切削對象構件之加工時,能夠獲得可抑制進行該加工時所產生之切屑之工具。本發明係關於基於該等見解而完成者。The inventors of the present invention have made intensive studies in order to achieve the above-mentioned object, and as a result found that, according to a metal composition containing a metal, nano-diamond particles and micro-diamond particles, when machining a member to be cut using the above-mentioned metal composition, it is possible to Obtain a tool that suppresses the chips generated during this machining. The present invention is completed based on these findings.
本發明提供一種金屬組成物,其含有金屬、奈米金剛石粒子及微米金剛石粒子。The present invention provides a metal composition containing metal, nano-diamond particles and micro-diamond particles.
較佳為,上述金屬組成物中,上述奈米金剛石粒子及上述微米金剛石粒子分散於由上述金屬構成之金屬基質中。Preferably, in the above-mentioned metal composition, the above-mentioned nano-diamond particles and the above-mentioned micro-diamond particles are dispersed in a metal matrix composed of the above-mentioned metal.
較佳為,上述奈米金剛石粒子之含量相對於上述金屬之總量100體積份為0.05~50體積份。Preferably, the content of the nano-diamond particles is 0.05-50 parts by volume relative to 100 parts by volume of the total amount of the metal.
上述金屬亦可作為上述金屬組成物中之黏合劑。The above-mentioned metal can also be used as a binder in the above-mentioned metal composition.
上述金屬較佳為藉由燒結法而成形之金屬黏結劑。The above-mentioned metal is preferably a metal binder formed by a sintering method.
上述金屬較佳為包含含銅之合金。The above metal is preferably an alloy containing copper.
上述金屬組成物亦可含有上述奈米金剛石粒子之二次粒子。The above-mentioned metal composition may also contain secondary particles of the above-mentioned nanodiamond particles.
上述金屬組成物中之上述奈米金剛石粒子之一次粒子平均粒徑(D50)較佳為1~240 nm。The average primary particle diameter (D50) of the nano-diamond particles in the metal composition is preferably 1 to 240 nm.
上述金屬組成物中之上述微米金剛石粒子之平均粒徑(D50)較佳為1~600 μm。The average particle diameter (D50) of the micro-diamond particles in the metal composition is preferably 1 to 600 μm.
上述奈米金剛石粒子較佳為包含爆轟法奈米金剛石。The above-mentioned nanodiamond particles preferably comprise detonation method nanodiamonds.
上述金屬組成物較佳為切削構件。 [發明之效果]The above-mentioned metal composition is preferably a cutting member. [Effect of invention]
於使用上述金屬組成物進行切削對象構件之加工時,可抑制進行該加工時所產生之切屑。並且,藉此提昇了上述加工步驟中之良率,因此達成提昇製程能力之效果。When the above-described metal composition is used to process a member to be cut, chips generated during the process can be suppressed. In addition, the yield in the above-mentioned processing steps is improved, thereby achieving the effect of improving the process capability.
本發明之一實施方式之金屬組成物至少含有金屬、奈米金剛石粒子及微米金剛石粒子。The metal composition of one embodiment of the present invention contains at least metal, nano-diamond particles and micro-diamond particles.
圖1表示上述金屬組成物之一實施方式之放大示意圖。金屬組成物1含有金屬2、奈米金剛石粒子3及微米金剛石粒子4。更詳細而言,金屬組成物1中,奈米金剛石粒子3及微米金剛石粒子4分散於由金屬2構成之金屬基質中。FIG. 1 shows an enlarged schematic view of one embodiment of the above-mentioned metal composition. The
於上述金屬組成物中,上述金屬發揮作為上述奈米金剛石粒子及上述微米金剛石粒子之黏合劑(黏結劑)之作用。於上述金屬組成物中,上述金屬可為藉由燒結法而成形之金屬黏結劑,亦可為藉由電鑄法進行鍍覆生長而製作之電鑄黏結劑。其中,就切屑抑制性更加優異之觀點而言,較佳為金屬黏結劑。In the above-mentioned metal composition, the above-mentioned metal functions as a binder (binder) for the above-mentioned nano-diamond particles and the above-mentioned micro-diamond particles. In the above-mentioned metal composition, the above-mentioned metal may be a metal binder formed by a sintering method, or an electroforming binder produced by plating growth by an electroforming method. Among them, a metal binder is preferable from the viewpoint of being more excellent in chip suppression.
作為上述金屬,可列舉:鋰、鎂、鋁、鈣、鉻、鈦、釩、鐵、鈷、鎳、銅、鋅、銀、錫、銻、碲、鎢、金、鉍、及包含該等金屬之合金。作為上述合金,較佳為青銅、銅-錫-鋅合金等含銅之合金。上述金屬可僅使用一種,亦可使用2種以上。Examples of the above-mentioned metals include lithium, magnesium, aluminum, calcium, chromium, titanium, vanadium, iron, cobalt, nickel, copper, zinc, silver, tin, antimony, tellurium, tungsten, gold, bismuth, and metals including these of alloys. As said alloy, copper-containing alloys, such as bronze and a copper-tin-zinc alloy, are preferable. Only one type of the above-mentioned metals may be used, or two or more types may be used.
上述奈米金剛石粒子為奈米尺寸之金剛石粒子,並無特別限制,可使用公知或慣用之奈米金剛石粒子。上述奈米金剛石粒子可為經表面修飾之奈米金剛石粒子,亦可為未經表面修飾之奈米金剛石粒子。再者,未經表面修飾之奈米金剛石粒子於表面具有羥基(-OH)。上述奈米金剛石粒子可僅使用一種,亦可使用2種以上。The above-mentioned nano-diamond particles are nano-sized diamond particles, which are not particularly limited, and known or conventional nano-diamond particles can be used. The above-mentioned nano-diamond particles can be either surface-modified nano-diamond particles or non-surface-modified nano-diamond particles. Furthermore, the unmodified nano-diamond particles have hydroxyl groups (-OH) on the surface. Only one type of the above-mentioned nanodiamond particles may be used, or two or more types may be used.
於上述表面修飾奈米金剛石中,作為對奈米金剛石粒子進行表面修飾之化合物或官能基,例如可列舉:矽烷化合物、羧基(-COOH)、膦酸離子或膦酸殘基、末端具有乙烯基之表面修飾基、醯胺基、陽離子界面活性劑之陽離子、包含聚甘油鏈之基、包含聚乙二醇鏈之基等。In the above-mentioned surface-modified nano-diamond, as the compound or functional group for surface-modifying the nano-diamond particle, for example, silane compound, carboxyl group (-COOH), phosphonic acid ion or phosphonic acid residue, a vinyl group at the end can be listed. surface modification groups, amide groups, cations of cationic surfactants, groups containing polyglycerol chains, groups containing polyethylene glycol chains, etc.
上述金屬組成物中之上述奈米金剛石粒子較佳為包含奈米金剛石之一次粒子。此外,亦可包含數個至數十個左右之上述一次粒子凝聚(凝附)而成之二次粒子。即,上述奈米金剛石粒子於上述金屬組成物中亦可為二次粒子(奈米金剛石粒子簇)。The above-mentioned nano-diamond particles in the above-mentioned metal composition are preferably primary particles containing nano-diamond. Moreover, the secondary particle which aggregated (agglomerated) the said primary particle from several to several dozen may be contained. That is, the above-mentioned nano-diamond particles may be secondary particles (nano-diamond particle clusters) in the above-mentioned metal composition.
上述金屬組成物中之上述奈米金剛石粒子之一次粒子平均粒徑(D50,中值徑)例如為1~240 nm,較佳為2~100 nm,更佳為3~50 nm,進而較佳為4~20 nm,尤佳為4~10 nm。上述平均粒徑可藉由動態光散射法來進行測定。The primary particle average particle size (D50, median diameter) of the above-mentioned nano-diamond particles in the above-mentioned metal composition is, for example, 1-240 nm, preferably 2-100 nm, more preferably 3-50 nm, and more preferably It is 4 to 20 nm, particularly preferably 4 to 10 nm. The above-mentioned average particle diameter can be measured by a dynamic light scattering method.
作為上述奈米金剛石粒子,例如可使用藉由爆轟法生成之奈米金剛石(爆轟法奈米金剛石)或藉由高溫高壓法生成之奈米金剛石(高溫高壓法奈米金剛石)。其中,就可容易地獲得一次粒子粒徑為個位數奈米之奈米金剛石之方面而言,較佳為爆轟法奈米金剛石。As the above-mentioned nanodiamond particles, for example, nanodiamond produced by a detonation method (detonation method nanodiamond) or nanodiamond produced by a high temperature and high pressure method (high temperature and high pressure method nanodiamond) can be used. Among them, detonation method nanodiamonds are preferred in terms of easily obtaining nanodiamonds whose primary particle diameters are single-digit nanometers.
作為上述爆轟法奈米金剛石,可列舉藉由空氣冷卻式爆轟法生成之奈米金剛石(空氣冷卻式爆轟法奈米金剛石)及藉由水冷式爆轟法生成之奈米金剛石(水冷式爆轟法奈米金剛石)。其中,較佳為空氣冷卻式爆轟法奈米金剛石,因其一次粒子小於水冷式爆轟法奈米金剛石。Examples of the above-mentioned detonation method nanodiamond include nanodiamonds produced by an air-cooled detonation method (air-cooled detonation nanodiamonds) and nanodiamonds produced by a water-cooled detonation method (water-cooled nanodiamonds). detonation method nanodiamond). Among them, the air-cooled detonation method nano-diamond is preferred because the primary particles are smaller than the water-cooled detonation method nano-diamond.
爆轟可於大氣環境進行,亦可於氮氣環境、氬氣環境、二氧化碳環境等非活性氣體環境進行。Detonation can be carried out in an atmospheric environment or in an inert gas environment such as a nitrogen environment, an argon environment, and a carbon dioxide environment.
上述微米金剛石粒子為微米尺寸之金剛石粒子,並無特別限制,可使用公知或慣用之微米金剛石粒子。上述微米金剛石粒子可僅使用一種,亦可使用2種以上。The above-mentioned micro-diamond particles are micro-sized diamond particles, which are not particularly limited, and known or conventional micro-diamond particles can be used. Only one type of the above-mentioned microdiamond particles may be used, or two or more types may be used.
上述金屬組成物中之上述微米金剛石粒子之平均粒徑(D50,中值徑)例如為1~600 μm,較佳為5~300 μm,更佳為7~100 μm,進而較佳為10~50 μm。上述平均粒徑可藉由動態光散射法來進行測定。The average particle size (D50, median diameter) of the micro-diamond particles in the metal composition is, for example, 1 to 600 μm, preferably 5 to 300 μm, more preferably 7 to 100 μm, and further preferably 10 to 10 μm. 50 μm. The above-mentioned average particle diameter can be measured by a dynamic light scattering method.
上述金屬組成物中之上述奈米金剛石之含量可根據上述金屬組成物之用途來進行適當調整,相對於上述金屬之總量100體積份,例如為0.05~50體積份,較佳為0.1~20體積份,更佳為1~10體積份。The content of the above-mentioned nanodiamond in the above-mentioned metal composition can be appropriately adjusted according to the application of the above-mentioned metal composition, relative to the total amount of the above-mentioned metal 100 parts by volume, for example, 0.05-50 parts by volume, preferably 0.1-20 parts by volume The volume part is more preferably 1 to 10 volume parts.
上述金屬組成物中之上述微米金剛石之含量可根據上述金屬組成物之用途來進行適當調整,相對於上述金屬之總量100體積份,例如為1~30體積份,較佳為5~20體積份,更佳為8~15體積份。The content of the above-mentioned micro-diamonds in the above-mentioned metal composition can be appropriately adjusted according to the application of the above-mentioned metal composition, relative to the total amount of the above-mentioned metal 100 parts by volume, for example, 1-30 parts by volume, preferably 5-20 parts by volume parts, more preferably 8 to 15 parts by volume.
上述金屬組成物還可含有除金屬、奈米金剛石粒子、及微米金剛石粒子以外之其他成分。作為上述其他成分,例如可列舉:除金剛石粒子以外之無機粒子、金屬氧化物、金屬碳化物、碳酸鹽、陶瓷等。作為上述無機粒子,可列舉作為研磨粒發揮作用之粒子(例如:氮化硼、碳化矽、氧化鋁等)、奈米碳管等。上述其他成分可僅使用一種,亦可使用2種以上。再者,上述金屬組成物中之金屬、奈米金剛石粒子及微米金剛石粒子的合計含有比率相對於上述金屬組成物之總量100質量%,例如可為90質量%以上、95質量%以上、98質量%以上、99質量%以上。又,上述金屬組成物中之金屬、奈米金剛石粒子及微米金剛石粒子的合計含有比率相對於上述金屬組成物之總量100體積%,例如可為90體積%以上、95體積%以上、98體積%以上、99體積%以上。The above-mentioned metal composition may also contain other components other than metal, nano-diamond particles, and micro-diamond particles. Examples of the above-mentioned other components include inorganic particles other than diamond particles, metal oxides, metal carbides, carbonates, ceramics, and the like. As said inorganic particle, the particle|grain which functions as an abrasive grain (for example, boron nitride, silicon carbide, alumina, etc.), a carbon nanotube, etc. are mentioned. Only one type of the above-mentioned other components may be used, or two or more types may be used. Furthermore, the total content ratio of metal, nano-diamond particles and micro-diamond particles in the above-mentioned metal composition may be, for example, 90% by mass or more, 95% by mass or more, 98% by mass relative to the total amount of the above-mentioned metal composition 100% by mass. mass % or more and 99 mass % or more. In addition, the total content ratio of the metal, nano-diamond particles and micro-diamond particles in the above-mentioned metal composition may be, for example, 90 vol. % or more, 95 vol. % or more, or 98 vol. % or more, 99% or more by volume.
作為上述金屬組成物,可列舉:切削工具、研磨工具、研削工具、挖削工具等用於進行切削對象構件之加工之工具中用於切削對象構件之切削構件;散熱器;滑動構件等。其中,上述金屬組成物較佳為切削構件,更佳為切削工具用之切削構件(例如切刀)。於上述金屬組成物為切削構件之情形時,其形狀較佳為片狀。Examples of the above-mentioned metal composition include cutting members, heat sinks, sliding members, etc., among the tools used for processing the cutting target member, such as cutting tools, grinding tools, grinding tools, and digging tools. Among them, the above-mentioned metal composition is preferably a cutting member, more preferably a cutting member for a cutting tool (eg, a cutter). When the above-mentioned metal composition is a cutting member, its shape is preferably a flake.
於上述金屬組成物為切削構件之情形時,上述微米金剛石粒子作為研磨粒發揮作用,且以與公知或慣用之切削構件中之研磨粒之形狀及配置相同之方式設計。並且推測,於上述切削構件中,上述奈米金剛石粒子發揮減少摩擦、磨耗之效果。推斷其原因在於,當作為研磨粒之微米金剛石切削對象構件時,於對象構件表面形成源自奈米金剛石粒子之轉移黏著膜(碳轉移黏著膜),該轉移黏著膜抑制了研磨粒之過度磨耗或切屑。如此,根據上述金屬組成物,可抑制切屑。並且,藉此提昇了上述加工步驟中之良率,故達成提昇製程能力之效果。When the above-mentioned metal composition is a cutting member, the above-mentioned micro-diamond particles function as abrasive grains, and are designed in the same manner as the shape and arrangement of abrasive grains in known or conventional cutting members. In addition, in the above-mentioned cutting member, the nano-diamond particles are presumed to exhibit the effect of reducing friction and wear. The reason for this is presumed to be that when the micro-diamond as an abrasive grain cuts the target member, a transfer adhesive film (carbon transfer adhesive film) derived from the nano-diamond particles is formed on the surface of the target member, and the transfer adhesive film suppresses excessive wear of the abrasive grains or chips. In this way, according to the above-mentioned metal composition, chips can be suppressed. In addition, the yield in the above-mentioned processing steps is thereby improved, thereby achieving the effect of improving the process capability.
上述金屬組成物可根據與用途相應之製法,參照公知或慣用之方法來適當地製造。例如,作為片狀切刀之上述金屬組成物可藉由燒結法使摻合有金屬、奈米金剛石粒子及微米金剛石粒子之組成物成形,或藉由電鑄法使上述組成物鍍覆生長,而進行製造。The above-mentioned metal composition can be appropriately produced by referring to a known or conventional method according to a production method according to the application. For example, the above-mentioned metal composition as a sheet cutter can be formed by sintering a composition mixed with metal, nano-diamond particles and micro-diamond particles, or by electroforming. to manufacture.
本說明書中揭示之各態樣亦可與本說明書中揭示之其他任意特徵加以組合。各實施方式中之各構成及該等之組合等為一例,可於不脫離本發明之主旨之範圍內適當進行構成之附加、省略、置換及其他變更。又,本發明之各發明不受實施方式或以下實施例之限定,僅由申請專利範圍來限定。 [實施例]The aspects disclosed in this specification can also be combined with any other features disclosed in this specification. The respective configurations and combinations thereof in each embodiment are examples, and additions, omissions, substitutions, and other modifications of the configurations can be appropriately performed within the scope of not departing from the gist of the present invention. In addition, each invention of the present invention is not limited to the embodiments or the following examples, but is limited only by the scope of the patent application. [Example]
以下,基於實施例對本發明之一實施方式進行更詳細之說明。Hereinafter, one embodiment of the present invention will be described in more detail based on examples.
實施例1 經由下述步驟製造爆轟法奈米金剛石粒子及切刀。Example 1 Detonation method nanodiamond particles and cutters were fabricated through the following steps.
(爆轟法奈米金剛石之製作) 首先,進行利用爆轟法生成奈米金剛石之步驟。本步驟中,首先,將「於錐形炸藥(shaped charge)中安裝電雷管而成者」設置於爆轟用耐壓性容器之內部並將容器密封。容器為鐵製,容器之容積為15 m3 。作為炸藥,使用0.50 kg之TNT(Trinitrotoluene,2,4,6-三硝基甲苯)與RDX(Research Department explosive,黑索金)之混合物。該炸藥中之TNT與RDX之質量比(TNT/RDX)為50/50。然後,起爆電雷管,於容器內使炸藥爆轟(生成爆轟法奈米金剛石)。然後,於室溫放置24小時,藉此使容器及其內部降溫。放冷後,利用刮刀對附著於容器內壁之奈米金剛石粗產物(包含利用上述爆轟法生成之奈米金剛石粒子之凝附體及煤)進行刮取作業,從而回收奈米金剛石粗產物。(Fabrication of Nanodiamond by Detonation Method) First, a step of generating nanodiamond by the detonation method is performed. In this step, first, a "conical explosive (shaped charge) with an electric detonator installed" is installed inside the pressure-resistant container for detonation, and the container is sealed. The container is made of iron, and the volume of the container is 15 m 3 . As an explosive, a mixture of 0.50 kg of TNT (Trinitrotoluene, 2,4,6-trinitrotoluene) and RDX (Research Department explosive, Hexogen) was used. The mass ratio of TNT to RDX in the explosive (TNT/RDX) is 50/50. Then, the electric detonator is detonated, and the explosive is detonated in the container (detonation method nanodiamond is generated). Then, it was left to stand at room temperature for 24 hours, thereby cooling the container and its inside. After cooling, use a scraper to scrape the rough nano-diamond product (including the agglomerates of nano-diamond particles and coal generated by the above-mentioned detonation method) attached to the inner wall of the container, so as to recover the rough nano-diamond product .
然後,進行氧化處理步驟。對複數次進行如上所述之生成步驟而獲得之奈米金剛石粗產物進行氧化處理步驟。具體而言,向所獲得之奈米金剛石粗產物中添加6 L之98質量%硫酸及1 L之69質量%硝酸而製成漿料後,於常壓條件之回流對該漿料進行48小時之加熱處理。該氧化處理中之加熱溫度為140~160℃。然後進行冷卻,然後藉由傾析法對固形物成分(包含奈米金剛石凝附體)進行水洗。水洗最初之上清液是有色的,於該情況,利用傾析法反覆對該固形物成分進行水洗,直至上清液於目視為透明。然後,進行乾燥,從而以粉體形式獲得包含一次粒子及奈米金剛石凝附體(二次粒子)之奈米金剛石粒子。進而,於以流速20 L/min吹入氧約8體積%、氮約92體積%之氣體之旋轉窯中,於400℃加熱6小時,從而獲得奈米金剛石之乾燥粉體。Then, an oxidation treatment step is performed. The oxidation treatment step is performed on the rough nanodiamond product obtained by performing the above-mentioned generation step for a plurality of times. Specifically, 6 L of 98 mass % sulfuric acid and 1 L of 69 mass % nitric acid were added to the obtained crude nanodiamond to prepare a slurry, and the slurry was refluxed under normal pressure conditions for 48 hours. the heat treatment. The heating temperature in the oxidation treatment is 140 to 160°C. After cooling, the solid content (including nanodiamond agglomerates) was washed with water by a decantation method. The supernatant liquid was colored at first in the water washing, and in this case, the solid content was repeatedly washed with water by the decantation method until the supernatant liquid was visually transparent. Then, by drying, nanodiamond particles including primary particles and nanodiamond agglomerates (secondary particles) are obtained in powder form. Furthermore, in a rotary kiln in which a gas of about 8 vol % of oxygen and about 92 vol % of nitrogen was blown at a flow rate of 20 L/min, it was heated at 400° C. for 6 hours to obtain a dry powder of nano-diamond.
使用X射線繞射裝置(商品名「SmartLab」,Rigaku股份有限公司製造)對所獲得之奈米金剛石乾燥粉體進行晶體結構解析。結果,於金剛石之繞射峰位置,即來自金剛石結晶之(111)面之繞射峰位置,觀察到強繞射峰,所算出之微晶尺寸為4.5 nm。又,使用X射線繞射裝置(商品名「SmartLab」、Rigaku股份有限公司製造)對所獲得之乾燥粉體進行小角度X射線散射測定,使用粒徑分佈解析軟體(商品名「NANO-Solver」、Rigaku股份有限公司製造),針對散射角度1°~3°之區域估算奈米金剛石之一次粒徑。於該估算中,假設奈米金剛石一次粒子為球形且粒子密度為3.51 g/ cm3 。結果,本測定所獲得之奈米金剛石一次粒子平均粒徑為5.5 nm,一次粒子分佈相關之相對標準偏差(RSD:relative standard deviation)為30.2。The crystal structure of the obtained dry nanodiamond powder was analyzed using an X-ray diffraction apparatus (trade name "SmartLab", manufactured by Rigaku Co., Ltd.). As a result, a strong diffraction peak was observed at the diffraction peak position of diamond, that is, the diffraction peak position derived from the (111) plane of the diamond crystal, and the calculated crystallite size was 4.5 nm. The obtained dry powder was subjected to small-angle X-ray scattering measurement using an X-ray diffraction apparatus (trade name "SmartLab", manufactured by Rigaku Co., Ltd.), and particle size distribution analysis software (trade name "NANO-Solver") was used. , manufactured by Rigaku Co., Ltd.), the primary particle size of nanodiamond is estimated for the region of scattering angle of 1° to 3°. In this estimation, the nanodiamond primary particles are assumed to be spherical and have a particle density of 3.51 g/cm 3 . As a result, the average particle size of the primary particles of the nano-diamond obtained by this assay was 5.5 nm, and the relative standard deviation (RSD: relative standard deviation) of the primary particle distribution was 30.2.
(切刀之製作) 使用青銅作為金屬黏結劑之黏合劑,且相對於黏合劑100體積份,摻合10體積份之微米金剛石粉體(#800,切削加工用研磨粒,D50:18~25 μm)而製成組成物,於其中摻合相對於黏合劑100體積份為6.4體積份之上述奈米金剛石乾燥粉體,於氮氣環境,於溫度750℃燒結為片狀。然後,沖裁成環狀,藉此製成金屬切刀(外徑:56 mm、內徑:40 mm、刀厚0.13 mm)。(The making of the cutter) Bronze is used as the binder of the metal binder, and 10 parts by volume of micron diamond powder (#800, abrasive grain for cutting, D50: 18-25 μm) is mixed with 100 parts by volume of the binder to make a composition. 6.4 parts by volume of the above-mentioned dry nano-diamond powder with respect to 100 parts by volume of the binder was mixed therein, and sintered in a nitrogen atmosphere at a temperature of 750° C. to form a sheet. Then, it was punched into a ring shape, thereby producing a metal cutter (outer diameter: 56 mm, inner diameter: 40 mm, blade thickness 0.13 mm).
再者,使用X射線繞射裝置(商品名「SmartLab」、Rigaku股份有限公司製造)對上述微米金剛石粉體進行晶體結構解析,結果,於金剛石之繞射峰位置,即來自金剛石結晶之(111)面之繞射峰位置,觀察到強繞射峰,所算出之微晶尺寸為20 μm。Furthermore, the crystal structure of the above-mentioned micro-diamond powder was analyzed using an X-ray diffraction apparatus (trade name "SmartLab", manufactured by Rigaku Co., Ltd.). As a result, the diffraction peak position of diamond was (111) derived from the diamond crystal. ) surface diffraction peak position, a strong diffraction peak was observed, and the calculated crystallite size was 20 μm.
比較例1 除了未摻合奈米金剛石乾燥粉體以外,以與實施例1相同之方式製作金屬切刀。Comparative Example 1 A metal cutter was fabricated in the same manner as in Example 1, except that the nanodiamond dry powder was not blended.
(玻璃切斷試驗) 對實施例及比較例中製作之金屬切刀進行玻璃切斷試驗。將實施例及比較例中獲得之金屬切刀安裝於切割裝置中,並使用上述金屬切刀將玻璃板(長7.5 cm×寬7.5 cm×厚0.4 mm)切斷,確認切斷後之玻璃板之正面及背面之切屑尺寸。玻璃板之切斷係以如下方式進行:主軸轉速為20 rpm,進給速度分別為1 mm/秒2次、2 mm/秒2次、3 mm/秒2次、4 mm/秒2次、5 mm/秒2次、6 mm/秒25次(合計35次),於長度方向上進行切斷。又,將主軸轉速設為20 rpm,將進給速度設為6 mm/秒72次,於寬度方向上進行切斷(合計107次)。切斷後,利用光學顯微鏡觀察玻璃板正面及背面之切斷線上之切屑,於正面及背面分別抽選尺寸較大之9處。針對正面及背面所抽選之各9處,將背面之切屑尺寸評價結果示於圖2及表1中,將正面之切屑尺寸評價結果示於圖3及表2中。再者,一面以1.0 L/分鐘之量供給去離子水,一面進行切斷。(glass cutting test) A glass cutting test was performed on the metal cutters produced in the examples and comparative examples. The metal cutters obtained in the examples and comparative examples were installed in the cutting device, and the glass plates (length 7.5 cm × width 7.5 cm × thickness 0.4 mm) were cut with the metal cutting blades, and the glass plate after cutting was confirmed. Chip size front and back. The cutting of the glass plate is carried out in the following way: the spindle speed is 20 rpm, the feed speed is 1 mm/sec twice, 2 mm/sec twice, 3 mm/sec twice, 4 mm/sec twice, 2 times at 5 mm/sec, 25 times at 6 mm/sec (35 times in total), and cut in the longitudinal direction. Moreover, the spindle rotation speed was set to 20 rpm, and the feed rate was set to 6 mm/sec 72 times, and cutting was performed in the width direction (107 times in total). After cutting, use an optical microscope to observe the chips on the cutting line on the front and back of the glass plate, and select 9 places with larger sizes on the front and back respectively. Figure 2 and Table 1 show the evaluation results of the chip size on the back surface, and the evaluation results of the chip size on the front surface are shown in Fig. In addition, cutting was performed while supplying deionized water in an amount of 1.0 L/min.
[表1]
[表2]
如圖2及表1所示,於使用比較例1中獲得之金屬切刀之情形時,玻璃板背面之切屑尺寸為13~30 μm,又,平均值為21 μm。另一方面,於使用實施例1中獲得之金屬切刀之情形時,玻璃板背面之切屑尺寸為11~20 μm,又,平均值為14 μm。如此,相對於比較例1而言,實施例1之切屑尺寸總體較小,平均值亦較小,又,標準偏差小,且變動亦較小。又,如圖3及表2所示,可知玻璃板之正面亦同樣地,相對於比較例1,實施例1之切屑尺寸總體較小。As shown in FIG. 2 and Table 1, when the metal cutter obtained in Comparative Example 1 was used, the size of the chips on the back surface of the glass plate was 13 to 30 μm, and the average value was 21 μm. On the other hand, when the metal cutter obtained in Example 1 was used, the chip size of the back surface of the glass plate was 11 to 20 μm, and the average value was 14 μm. In this way, compared with Comparative Example 1, the chip size of Example 1 is generally smaller, the average value is also smaller, the standard deviation is smaller, and the variation is smaller. Moreover, as shown in FIG.3 and Table 2, it turns out that the chip size of Example 1 is small as a whole compared with the comparative example 1 similarly to the front surface of a glass plate.
以下,記載本公開之發明之其他實施型態。
[備註1]一種金屬組成物,其含有金屬、奈米金剛石粒子及微米金剛石粒子。
[備註2]如備註1中記載之金屬組成物,其中,上述奈米金剛石粒子及上述微米金剛石粒子分散於由上述金屬構成之金屬基質中。
[備註3]如備註1或2中記載之金屬組成物,其中,相對於上述金屬之總量100體積份,上述奈米金剛石粒子之含量為0.05~50體積份(較佳為0.1~20體積份,更佳為1~10體積份)。
[備註4]如備註1至3中任一項記載之金屬組成物,其中,上述金屬為上述金屬組成物中之黏合劑。
[備註5]如備註1至4中任一項記載之金屬組成物,其中,上述金屬係藉由燒結法而成形之金屬黏結劑。
[備註6]如備註1至5中任一項記載之金屬組成物,其中,上述金屬包含含銅之合金(較佳為青銅)。
[備註7]如備註1至6中任一項記載之金屬組成物,其含有上述奈米金剛石粒子之二次粒子。
[備註8]如備註1至7中任一項記載之金屬組成物,其中,上述奈米金剛石粒子包含爆轟法奈米金剛石。
[備註9]如備註1至7中任一項記載之金屬組成物,其中,上述奈米金剛石粒子包含空氣冷卻式爆轟法奈米金剛石。
[備註10]如備註1至9中任一項記載之金屬組成物,其中,上述奈米金剛石粒子之一次粒子平均粒徑為1~240 nm(較佳為2~100 nm,更佳為3~50 nm,進而較佳為4~20 nm,尤佳為4~10 nm)。
[備註11]如備註1至10中任一項記載之金屬組成物,其中,上述微米金剛石粒子之平均粒徑為1~600 μm(較佳為5~300 μm,更佳為7~100 μm,進而較佳為10~50 μm)。
[備註12]如備註1至11中任一項記載之金屬組成物,其中,上述金屬組成物中之上述微米金剛石的含量相對於上述金屬之總量100體積份,為1~30體積份(較佳為5~20體積份,更佳為8~15體積份)。
[備註13]如備註1至12中任一項記載之金屬組成物,其中,上述金屬組成物中之金屬、奈米金剛石粒子及微米金剛石粒子的合計含有比率相對於上述金屬組成物之總量100質量%,為90質量%以上(95質量%以上、98質量%以上或99質量%以上)。
[備註14]如備註1至13中任一項記載之金屬組成物,其中,上述金屬組成物中之金屬、奈米金剛石粒子及微米金剛石粒子的合計含有比率相對於上述金屬組成物之總量100體積%,為90體積%以上(95體積%以上、98體積%以上或99體積%以上)。
[備註15]如備註1至14中任一項記載之金屬組成物,其為切削構件。
[備註16]一種如請求項1至14中任一項記載之金屬組成物之用途,其係用作切削構件。Hereinafter, other embodiments of the invention of the present disclosure will be described.
[Note 1] A metal composition containing a metal, nano-diamond particles, and micro-diamond particles.
[Note 2] The metal composition according to
1:金屬組成物 2:金屬(金屬基質) 3:奈米金剛石粒子 4:微米金剛石粒子1: Metal composition 2: Metal (metal matrix) 3: Nanodiamond Particles 4: Micron diamond particles
[圖1]係本發明之一實施方式之金屬組成物之放大示意圖。 [圖2]係表示實施例及比較例中之玻璃切削試驗之背面切屑尺寸評價結果的圖表。 [圖3]係表示實施例及比較例中之玻璃切削試驗之正面切屑尺寸評價結果的圖表。Fig. 1 is an enlarged schematic view of a metal composition according to an embodiment of the present invention. [ Fig. 2] Fig. 2 is a graph showing the results of back chip size evaluation in the glass cutting test in Examples and Comparative Examples. [ Fig. 3] Fig. 3 is a graph showing the evaluation results of the front chip size of the glass cutting test in Examples and Comparative Examples.
1:金屬組成物 1: Metal composition
2:金屬(金屬基質) 2: Metal (metal matrix)
3:奈米金剛石粒子 3: Nanodiamond Particles
4:微米金剛石粒子 4: Micron diamond particles
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- 2021-02-08 TW TW110104684A patent/TW202202251A/en unknown
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WO2021161911A1 (en) | 2021-08-19 |
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