TW200804228A - Molding die for glass hard disk substrate - Google Patents

Molding die for glass hard disk substrate Download PDF

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Publication number
TW200804228A
TW200804228A TW096119362A TW96119362A TW200804228A TW 200804228 A TW200804228 A TW 200804228A TW 096119362 A TW096119362 A TW 096119362A TW 96119362 A TW96119362 A TW 96119362A TW 200804228 A TW200804228 A TW 200804228A
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Taiwan
Prior art keywords
glass
hard disk
disk substrate
molding die
carbon
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TW096119362A
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Chinese (zh)
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TWI408119B (en
Inventor
Mikio Sakaguchi
Hiroki Ueyama
Keisaku Inoue
Moriji Nozaki
Toshiaki Yoshida
Tetsuya Aoki
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Kao Corp
Ohara Kk
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • C03B11/06Construction of plunger or mould
    • C03B11/08Construction of plunger or mould for making solid articles, e.g. lenses
    • C03B11/084Construction of plunger or mould for making solid articles, e.g. lenses material composition or material properties of press dies therefor
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • C03B11/06Construction of plunger or mould
    • C03B11/08Construction of plunger or mould for making solid articles, e.g. lenses
    • C03B11/088Flat discs
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/575Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering
    • C04B35/5755Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering obtained by gas pressure sintering
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2215/00Press-moulding glass
    • C03B2215/02Press-mould materials
    • C03B2215/05Press-mould die materials
    • C03B2215/07Ceramic or cermets
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2215/00Press-moulding glass
    • C03B2215/72Barrel presses or equivalent, e.g. of the ring mould type
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3817Carbides
    • C04B2235/3821Boron carbides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/604Pressing at temperatures other than sintering temperatures

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)

Abstract

Disclosed is a molding die for glass hard disk substrates which is hardly reactive with glasses, while having high wear resistance and high durability. A glass molded therein can be easily released from the surface of the molding die. Specifically disclosed is a molding die for glass hard disk substrates, which contains a silicon carbide-carbon composite ceramic. The silicon carbide-carbon composite ceramic contains 15-50 parts by weigh of carbon per 100 parts by weight of silicon carbide, and the average particle diameter of the carbon is within the range of 0.3-100 μm.

Description

200804228 九、發明說明: 【發明所屬之技術領域】 本發明係關於玻璃製硬碟基板用成形模,更詳細而言, 係關於含有碳化矽-碳複合陶瓷之玻璃製硬碟基板用成形 模,以及利用其之玻璃製硬碟基板之製造方法。 【先前技術】 玻璃製硬碟基板係適合使用於資訊記錄裝置之磁性記錄 媒體用基板。通常,該玻璃製硬碟基板於成形模之上模及 下模之間配置有玻璃原料,利用熱壓而成形為所需形狀, 進而,根據須要,對表面進行研磨以製品化。 作為用以成形上述玻璃製硬碟基板之成形模之材料而 言,由於陶瓷之熱穩定性優異,因此使用有各種陶究(JP 2002-230747)。 另一方面,於JP 2004-67432中揭示有,將特定粒徑之陶 兗材料(碳化矽等)與特定粒徑之碳以特定比例調配而形成 之陶瓷複合燒結體,作為對陶瓷、玻璃、金屬等進行成形 加工時之成形模之原料。 然而,於玻璃製硬碟基板之製造中,伴隨成形之高速 化、高頻化,對於上述JP 2002-230747所記載之成形模材 料’其表面易磨耗’玻璃成分與成形模表面在高溫下反 應,因此而出現所成形之玻璃之表面精度下降之問題。 又,對於JP 2004-67432所記載之陶瓷複合燒結體,由於其 所含有之碳粒子之粒徑微小,故玻璃成分與成形模表面牢 固地密著而難以從上述成形模剝離,因此出現難以連續成 121126.doc 200804228 形之問題。 【發明内容】 本發明係關於一種玻璃製硬碟基板用成形模(以下,亦 稱為「本發明之成形模」),其係含有碳化矽_碳複合陶瓷 之成形模,其中上述碳化矽-碳複合陶瓷中,對於重量 份之碳化矽,含有15重量份〜50重量份之碳粒子,且上述 石反粒子之平均粒徑為〇·3 μπι〜1〇〇㈣之範圍。 本發明係關於一種玻璃製硬碟基板之製造方法,其係包 _ &於成形模巾配置破璃原料,並對上述玻璃原料進行加壓 成形之步驟,且上述成形模係本發明之玻璃製硬碟基板用 成形模。 【實施方式】 (玻璃製硬碟基板用成形模) 如上所述,本發明之成形模含有碳化矽_碳複合陶瓷(以 下,亦稱為「複合陶瓷」),該碳化矽_破複合陶瓷中,對 _ 於100重量份之碳化矽,含有15重量份〜50重量份之碳粒 子,且上述碳粒子之平均粒徑為〇·3 μιη〜1〇〇 μηι之範圍。 如上所述,對於本發明之成形模而言,於上述複合陶瓷 中,對於100重量份之碳化矽,含有15重量份〜50重量份之 石厌粒子’與先前技術中例如上述專利文獻1之碳化矽複合 陶曼之製造中作為燒結助劑而使用之碳量相比,該含有量 為較多量。藉由使其具有上述含有量,而可於玻璃成形時 抑制與破璃之反應性,由此成為呈現高耐磨耗性與耐久性 之成形模。又’亦可確保如專利文獻2之對於碳含量非常 121126.doc 200804228 南之陶瓷所無法達成之充分之耐久性。 ^ ’本發明之成形模中,上述複合㈣所含有之碳粒子 之平均粒徑為0.3 μηι〜100 μιη,與專利文獻2之陶瓷中之碳 粒子相比’該平均粒徑為非常大之粒徑。使用上述大録 之碳粒子,可降低所成形之玻璃與成形模表面之密著性, 以實現良好之脫模性。[Technical Field] The present invention relates to a molding die for a glass hard disk substrate, and more particularly to a molding die for a glass hard disk substrate containing a tantalum carbide-carbon composite ceramic. And a method of manufacturing a glass hard disk substrate using the same. [Prior Art] A glass hard disk substrate is suitable for a substrate for a magnetic recording medium used in an information recording device. Usually, the glass hard disk substrate is placed between the upper mold and the lower mold of the forming mold, and is formed into a desired shape by hot pressing, and further, the surface is polished to be processed as necessary. As a material for forming a molding die of the above-described glass hard disk substrate, since ceramics are excellent in thermal stability, various ceramics (JP 2002-230747) are used. On the other hand, JP 2004-67432 discloses a ceramic composite sintered body formed by blending a ceramic material of a specific particle size (such as tantalum carbide) with carbon of a specific particle size in a specific ratio, as a ceramic, glass, or the like. A raw material of a molding die when forming a metal or the like. However, in the manufacture of a glass hard disk substrate, the molding die material described in JP 2002-230747 has a surface that is easy to wear, and the glass component reacts with the surface of the molding die at a high temperature. Therefore, there is a problem that the surface precision of the formed glass is lowered. Further, in the ceramic composite sintered body described in JP 2004-67432, since the particle diameter of the carbon particles contained therein is small, the glass component and the surface of the molding die are strongly adhered to each other, and it is difficult to peel off from the molding die, so that it is difficult to continuously In the form of 121126.doc 200804228 shape. The present invention relates to a molding die for a glass hard disk substrate (hereinafter also referred to as "the molding die of the present invention"), which is a molding die containing a ruthenium carbide-carbon composite ceramic in which the above-described ruthenium carbide is- In the carbon composite ceramic, 15 parts by weight to 50 parts by weight of carbon particles are contained in parts by weight of the cerium carbide, and the average particle diameter of the stone antiparticles is in the range of 〇·3 μπι 1 to (4). The present invention relates to a method for producing a glass hard disk substrate, which comprises the steps of: arranging a glass raw material in a molding die, and subjecting the glass raw material to press forming, and the forming die is the glass of the present invention. A forming die for a hard disk substrate. [Embodiment] (Forming Die for Glass Hard Disk Substrate) As described above, the molding die of the present invention contains a ruthenium carbide-carbon composite ceramic (hereinafter also referred to as "composite ceramic"), and the ruthenium carbide-breaking composite ceramic is used. And 100 parts by weight of carbonized ruthenium containing 15 parts by weight to 50 parts by weight of carbon particles, and the average particle diameter of the carbon particles is in the range of 〇·3 μιη to 1〇〇μηι. As described above, in the above-mentioned composite ceramic, the above-mentioned composite ceramic contains 15 parts by weight to 50 parts by weight of the stone-reactive particles for 100 parts by weight of cerium carbide, and the prior art, for example, the above-mentioned Patent Document 1 The amount of carbon used as a sintering aid in the production of tantalum carbide composite taman is relatively large compared to the amount of carbon used as a sintering aid. By having the above content, the reactivity with the glass can be suppressed during the molding of the glass, whereby the molding die exhibits high abrasion resistance and durability. Further, it is also possible to ensure sufficient durability such as the patent document 2 for a carbon content of 121126.doc 200804228. In the molding die of the present invention, the average particle diameter of the carbon particles contained in the composite (four) is 0.3 μηι to 100 μηη, which is a very large particle size compared with the carbon particles in the ceramic of Patent Document 2. path. By using the above-mentioned large-sized carbon particles, the adhesion between the formed glass and the surface of the molding die can be lowered to achieve good mold release property.

又,從確保更良好之脫模性之觀點而言,上述複合陶究 所含有之碳粒子之平均粒徑較好的是〇5卿以上,更好的 疋0.7 μιη以上,進而好的是i μιη以上。同樣,從確保更良 好之脫板性之觀點而言,上述複合陶究所含有之碳粒子之 平均粒徑較好的是25 μ誠下,更好的是5叫以下。具體 而言,碳粒子之平均粒徑較好的是〇5 μιη〜25 pm,更好的 是〜5卿’進而好的是i㈣〜5 _。上述碳粒子之平 均粒徑係藉由雷射繞射/散射式粒徑分 ^,掘場製作所社製)而敎之體積平均粒徑== 相同)。 再者’本發明之成形模係錢製硬碟基板之製造中所使 用之成形模,但玻璃製硬碟基板可為非晶性玻璃€非晶質 玻璃)製基板’亦可為#晶化玻璃(玻璃陶幻製基板,只要 為玻璃系基板,則無特別限制。 從確保更高之耐磨耗性及耐久性之觀點^,上述複合 陶瓷所含有之碳粒子之含有量較好的是,相對於ι〇〇重量 份之碳化矽,為15重量份〜45重量份,更好的是重量份 〜30重量份。 121126.doc 200804228 作為上述碳化石夕之原料,可為α、β之任—結 碳化矽原料之純度並無特別限 曰曰 推而担一#命士 处以更南密度燒結, 耗性及耐久性之觀點而言,較好的是9。重量 ^ 是95重量%以上。碳化石夕原料(粒子)之平 :徑並無特別限制’但從燒結性更良好之觀點而言,上 述原料較好的是〇.10„1〜1〇^1111之粉末。 上Moreover, from the viewpoint of ensuring better release property, the average particle diameter of the carbon particles contained in the composite ceramics is preferably 〇5 qing or more, more preferably 疋0.7 μηη or more, and further preferably i Ιιη or more. Similarly, from the viewpoint of ensuring better release properties, the average particle size of the carbon particles contained in the above composite ceramics is preferably 25 μC, and more preferably 5 or less. Specifically, the average particle diameter of the carbon particles is preferably 〇5 μιη to 25 pm, more preferably ~5 qing' and further preferably i(four) 〜5 _. The average particle diameter of the carbon particles is determined by the laser diffraction/scattering particle diameter, which is manufactured by the company, and the volume average particle diameter of the crucible is the same. Further, the molding die used in the production of the hard disk substrate of the present invention may be a substrate made of a hard glass substrate, but the glass hard disk substrate may be a non-crystalline glass. The glass (glass phantom substrate) is not particularly limited as long as it is a glass substrate. From the viewpoint of ensuring higher abrasion resistance and durability, the content of the carbon particles contained in the composite ceramic is preferably It is 15 parts by weight to 45 parts by weight, more preferably ~30 parts by weight, based on the weight of the cerium carbide. 121126.doc 200804228 As the raw material of the above-mentioned carbonized stone, it can be α, β The purity of the —-junction 碳 矽 并无 并无 并无 并无 并无 并无 并无 担 担 担 # # # # # # # # # # 处 处 处 处 处 处 处 处 更 更 更 更 更 更 更 更 更 更 更 更 更 更The flatness of the carbonaceous raw material (particles): the diameter is not particularly limited', but from the viewpoint of better sinterability, the above-mentioned raw material is preferably a powder of 10.10 „1~1〇^1111.

㈣兮闹曼所含有之碳粒子較好的是碳之單體,由社 :相、非晶相、或者結晶相與非晶相之混合相而組成。該 專单體之結晶相較好的是,於藉由雷射拉曼分光法所 之測定光譜中’在以1580 (^附近為中心之14〜:〜 1700咖·1之範圍内,具有結晶相之峰。該結晶構造並無特 別限制,但較好的[可舉出石墨型平面六角形構造、菱 面體形構造等。又’非晶相較好的是,於藉由雷射拉曼分 光法所獲得之測定光譜中,在以136G W附近為中心之 1300 cm· i〜145〇 cm-i之範圍内,具有結晶相之峰。 上述複合陶瓷所含有之碳粒子,從確保更高之耐摩耗性 及耐久性之觀點,進而從達成更高強度及破壞韌性之觀點 而言,結晶相與非晶相之雷射拉曼分光強度之峰面積比 (結晶相7非晶相)較好的是1〜1〇,更好的是1〜5。通常,可 認為上述峰面積比相當於碳之石墨化度,只要該值為上述 範圍,則可達成更良好之強度及破壞韌性。再者,上述光 譜之測定可使用氬雷射拉曼分光裝置(NEC社製)。為成為 上述峰面積比,亦可較好地選擇殘碳率30重量%〜95重量 /〇 ’更好地選擇殘碳率40重量%〜90重量%之烧基改質紛樹 121126.doc 200804228 脂、煤焦油瀝青作為碳源。再者,所謂殘碳率,係指根據 JISK 2425而測定之碳源中固定碳之重量百分比。(4) The carbon particles contained in the noisy man are preferably carbon monomers, which are composed of a phase, an amorphous phase, or a mixed phase of a crystalline phase and an amorphous phase. The crystal phase of the specific monomer is preferably in the range of the spectrum measured by the Raman spectroscopy method, which is in the range of 1480::1 to 1700 ga. The crystal structure is not particularly limited, but is preferably a graphite-type planar hexagonal structure, a rhombohedral structure, etc. The amorphous phase is preferably obtained by laser Raman. The measurement spectrum obtained by the spectroscopic method has a peak of a crystal phase in the range of 1300 cm·i to 145 cm-i centered around 136 G W. The carbon particles contained in the composite ceramic are higher in ensuring From the viewpoint of abrasion resistance and durability, the peak area ratio (crystal phase 7 amorphous phase) of the laser Raman spectroscopic intensity of the crystal phase and the amorphous phase is higher from the viewpoint of achieving higher strength and fracture toughness. It is preferably 1 to 1 Torr, more preferably 1 to 5. In general, it is considered that the peak area ratio corresponds to the degree of graphitization of carbon, and if the value is in the above range, more excellent strength and fracture toughness can be achieved. Furthermore, the above spectrum can be measured using an argon laser Raman spectroscopic device (NEC Corporation). In order to achieve the above peak area ratio, it is also possible to better select a residual carbon ratio of 30% by weight to 95% by weight/〇 to better select a residual carbon ratio of 40% by weight to 90% by weight. Doc 200804228 Grease and coal tar pitch are used as carbon sources. Further, the carbon residue ratio refers to the weight percentage of fixed carbon in the carbon source measured according to JIS K 2425.

從確保更高之耐磨耗性及耐久性之觀點而言,上述複合 陶究所含有之礙化石夕之平均粒徑較好的是G3 _以上。同 樣’從確保更高之耐磨耗性及耐久性之觀點而言,上述複 合陶竟所含有之碳切之平均粒徑較好的是⑽叫以下, 更好的是50叫以下’進而好的是4 _以下。具體而言, 碳化石夕之平均粒徑較好的是G·3帥〜⑽㈣,更好的是〇3 μΓΠ ’進而好的是〇·3 _〜4 μιη。再者,碳化石夕之平 均粒徑可藉由與上述碳粒子之平均粒徑相同之方法而測 定。碳化石夕係於上述複合陶兗中成為基質者,其結晶型可 為α、β之任一者。 上述複合㈣較好的是由上述碳切與碳而構成,但在 不損及本發明之效果之範圍内,亦可進而含有除碳化石夕以 外之碳化物等任意成分。 本發明之複合陶瓷含有粒徑較大之碳粒子,並且較好地 含有,徑較大之碳化矽’因而為確保複合陶莞之強度,較 好的是’空隙直徑較小。冑大空隙直徑較好的是鳩㈣以 下,更好的是0叫〜100㈣,進而好的是5〇 μιη以下進 而更好的是25 μπ1以下。再者,最大空隙直徑可以如下方 式而測定。即,對於複合陶莞表面之空隙1,可藉由 key:nce社製之VH-8〇〇〇型而獲得空隙孔之像(照片),並對 所獲得之像特畫像解析而求丨。於畫像解析時,測定隨 機定向之空隙孔之長軸徑(mm)與短㈣(職),求出(長轴 121126.doc 200804228 徑+短軸徑)/2’並對於上述VH__型倍率為刚倍時之 視野中每-空隙孔’將各自所獲得之值之最大值作為最大 空隙直徑。所謂長軸徑與短軸徑,係分別以如下方式而定 義。當以2條平行線夾持空隙孔時,將該踢平行線之間隔 為最小之空隙孔之寬度稱為短軸#,另—方面,當以與該 平行線成直角方向上之2條平行線來夾持空隙孔時,將該2 條平行線之間隔稱為長軸徑。再者,於模且成形、From the viewpoint of ensuring higher abrasion resistance and durability, the above-mentioned composite ceramics contains an average particle size of G3 _ or more. Similarly, from the viewpoint of ensuring higher wear resistance and durability, the average particle size of the carbon cut contained in the above composite ceramics is preferably (10) below, and more preferably 50 or less. It is 4 _ or less. Specifically, the average particle diameter of the carbonized stone is preferably G·3 handsome ~ (10) (four), more preferably 〇 3 μΓΠ ' and further preferably 〇 · 3 _ ~ 4 μιη. Further, the average particle diameter of the carbonized stone can be measured by the same method as the average particle diameter of the above carbon particles. The carbonized stone is a matrix in the above composite ceramic pot, and its crystal form may be either α or β. The above-mentioned composite (4) is preferably composed of the above-mentioned carbon cut and carbon. However, it may further contain an optional component such as a carbide other than the carbonaceous stone in the range which does not impair the effects of the present invention. The composite ceramic of the present invention contains carbon particles having a large particle diameter, and preferably contains a ruthenium carbide having a large diameter, thereby ensuring the strength of the composite ceramics, and it is preferable that the diameter of the void is small. The larger diameter of the larger void is preferably 鸠(4) or less, more preferably 0 is less than 100 (four), and further preferably 5 〇 μιη or less and more preferably 25 μπ1 or less. Further, the maximum void diameter can be measured as follows. In other words, for the void 1 on the surface of the composite pottery, the image of the void hole (photograph) can be obtained by the VH-8〇〇〇 type manufactured by Key: nce, and the obtained image can be analyzed. In the image analysis, the long axis diameter (mm) and the short (four) (job) of the randomly oriented void are measured, and the long axis 121126.doc 200804228 diameter + short axis diameter/2' is obtained and the above VH__ type magnification is obtained. The maximum value of each value obtained for each void hole in the field of view at the time of the double magnification is taken as the maximum void diameter. The long axis diameter and the short axis diameter are defined as follows. When the gap hole is held by two parallel lines, the width of the gap hole which minimizes the interval between the kick parallel lines is referred to as the short axis #, and on the other hand, when two holes are perpendicular to the parallel line When the wire is used to hold the void hole, the interval between the two parallel lines is referred to as a long axis diameter. Furthermore, it is molded and formed.

CIp(C〇LD IS〇STATIC PRESS,冷等靜壓)、Hip(酣 ISOSTATK: PRESS,熱等靜壓)等中,若以〇 5 心2 之壓力而成形’則可使複合陶兗之最大空隙直徑為 _ 以下。 本發明之成形模由於對於玻璃之脫模性高,因而較好的 是,在玻璃成形時玻璃所接觸之表面之至少一部分由上述 複合陶究而構成,進而好的是,上述接觸表面全部由上述 複合陶竞而構成。X,上述成形模之全體亦可由上述複合 陶竟而構成。其具體例為,當本發明之成形模由模具與沖 頭而組成時,模具及沖頭之任—者或二者可*上述複合陶 甍所構成。又,對於模具及沖頭之任—者或二者,其與玻 璃之接觸面之-部分或者整個面亦可由上述複合陶究所構 成0 本發明之成形模之形狀可舉出與先前眾所周知之成形模 相同之形狀。本發明之成形模之特徵為,含有上述複合陶 瓷,且如上所述,若玻璃所接觸之表面之至少一部分含有 上述複合陶£’則可提高對玻璃之脫模性,因而該形狀本 121126.doc 200804228 身無任何限制。 當使用本發明之成形模來盤生 、求i造玻璃製硬碟基板時,上述 成形模中與玻璃之接觸表面之 两灸形狀可轉印至成形後之玻璃 表面㈣乂好的疋’上述接觸表面儘可能平滑。具體而 言:從成形後之基板研磨效率之觀點以及上述接觸表面之 平滑性之觀點而言’上述接觸本 I钱觸表面之中心線平均粗度Ra較CIp (C〇LD IS〇STATIC PRESS, cold isostatic pressing), Hip (酣ISOSTATK: PRESS, hot isostatic pressing), etc., if formed by the pressure of 〇5 core 2, the largest compound ceramic scorpion The void diameter is _ or less. Since the mold of the present invention has high mold release property to glass, it is preferred that at least a part of the surface contacted by the glass during glass forming is composed of the above composite ceramics, and it is preferable that the contact surfaces are all The above composite Tao Jing constitutes. X, the entire molding die may be composed of the above composite ceramic. Specifically, when the molding die of the present invention is composed of a die and a punch, either or both of the die and the punch may be composed of the above composite ceramic. Further, for the mold or the punch, the part or the whole surface of the contact surface with the glass may be composed of the above composite ceramics. The shape of the molding die of the present invention may be exemplified as previously known. The shape of the forming die is the same. The molding die of the present invention is characterized in that it comprises the above composite ceramic, and as described above, if at least a part of the surface contacted by the glass contains the composite ceramic, the release property to the glass can be improved, and thus the shape is 121126. Doc 200804228 There are no restrictions. When the molding die of the present invention is used to form a glass hard disk substrate, the two moxibustion shapes of the contact surface with the glass in the molding die can be transferred to the surface of the formed glass (4). The contact surface is as smooth as possible. Specifically, from the viewpoint of the substrate polishing efficiency after molding and the smoothness of the above-mentioned contact surface, the average thickness Ra of the center line of the above-mentioned contact surface is higher.

好的是請1 _〜10叫,更好的是_ μΓη〜9.5㈣,進而 好的是0.02叫。再者,中心線平均粗度以可利用 m B〇651而求出。中心線平均粗度以可藉由提高燒結體 之密度而設^上述範圍,因此使用下述假燒之粉末(複 合陶資*)即可。 (複合陶瓷之製造方法) 本發月之玻璃製硬碟基板用成形模中之複合陶瓷,可以 如下方式而製備。 上述複合陶瓷可藉由將含有碳化矽及碳源之原料混合物 根據須要假燒之後,成形為所需形狀,並將其燒成而製 造。以下將描述,當以該複合陶瓷構成本發明之成形模全 體時,可成形為所需成形模形狀,又,當以該複合陶瓷構 成本發明之成形模之一部分時,可成形為成形模零件之所 需形狀。 上述複合陶瓷較好的是,含有如上所述碳之單體,但該 碳之單體較好的是由製造過程中適當之碳源所生成。具體 而言’可將碳化矽、下述碳源、以及所需之先前眾所周知 之添加劑進行濕式混合後假燒。於該假燒步驟中,通常碳 121126.doc -12- 200804228 源之碳轉變為單體。上述各原料之混合比例可適當設定 為’所獲得之複合陶竟中’料⑽重量份之碳化石夕,含 有15重量份〜50重量份之碳粒子。 上述添加劑並無特別限制,可舉出眾所周知之硼化合 物、鈦化合物、銘、氧化銀化合物等之燒結助劑等。 上述漁式此σ可使用球磨機、振動式球磨機及行星式球 磨機等進行混合。X,濕式混合所使用之溶劑並無特別限 制’較好的是’苯、甲苯、二f苯等料㈣溶劑;甲 醇、乙醇等醇系溶劑;以及甲基乙基酮等酮系溶劑等有機 溶劑。作為其他溶劑’亦可使用水、水與上述有機溶劑之 混合溶劑等。 濕式混合後之混合物之假燒並無特別限制,可以先前眾 所周知之方法而進行,但從使所使用之碳源更充分地轉換 為碳單體’並且維持良好分散性之觀點而言,較好的是, 於n性%境氣體(氮氣、氬氣等環境氣體)下,於 150 C〜800°C進行熱處理。 上述碳源並無特別限制,可使用於濕式混合所使用之上 述有機溶劑中具有可溶性或分散性者,且在上述假燒條件 下可轉換為碳者。當碳源為固體粉末時,從其分散性之觀 點而吕,較好的是平均粒徑為〇1 μιη〜1〇〇 左右之材 料。又,為使上述碳源於假燒後轉換為碳之轉換率高,故 、芳香知反化氫較佳,具體而言,可舉出呋喃樹脂、酚樹 月曰及煤焦油瀝青等,其中更好的是酴樹脂及煤焦油遞青。 又,可將假燒後之上述物質作為碳源而使用。 12I126.doc -13- 200804228 :、逃反化矽原料(粒子),如上所述,可為α、β之任 一結晶型。又,分& 、^ 孩奴化矽原料之純度並無特別限制,但從 以更高密度捧& 、# f , ^ 儿、、、σ,進而提高耐磨耗性及而ί久性之觀點而 幸乂好的疋90重量%以上,更好的是95重量%以上。碳 夕原料(粒子)之平均粒徑並無特別限制,但從燒結性更 ^好之觀點而言’較好的是G.1 μπι〜1G μπι之粉末。再者, 句、2原料(粒子)之平均粒徑係藉由雷射繞射/散射光式粒 徑分布測定裝番,f 、置(商nu*LA72〇,堀場製作所社製)而測 之體積平均粒徑D5。(以下相同)。 +二人對飯燒後之混合物依所需進行造粒後,成形為所 :形狀。成形方法並無特別限制,只要以模具成形法、射 、二 P(冷等靜壓)法等形成塊,並根據須要對上述塊 進仃機械加工以製作所需形狀之成形體即可。 繼而’將所獲得之成形體提供於燒成步驟。燒成方法並 、特%限制’可以眾所周知之方法而進行,但較好的是, 於[月性%境氣體下或真空中,^18〇(rc〜23〇(rCT進行處 =在i述燒成溫度下進行處理時,彳獲得燒結體之密 、又強度及硬度等機械特性更良好。為達成高密度化,上 :燒成方法進而好的是,採用熱壓、HIP(熱等靜壓)法 寻〇 ’Ok, please call 1 _~10, and better _ μΓη~9.5 (4), and then 0.02 is good. Furthermore, the average thickness of the center line can be obtained by using m B 〇 651. The average thickness of the center line can be set to the above range by increasing the density of the sintered body. Therefore, the following calcined powder (combined ceramics *) can be used. (Manufacturing method of composite ceramic) The composite ceramic in the molding die for a glass hard disk substrate of this month can be prepared as follows. The above composite ceramics can be produced by forming a raw material mixture containing cerium carbide and a carbon source into a desired shape after firing according to the necessity of firing. As will be described below, when the composite mold of the present invention is constituted by the composite ceramic, it can be formed into a desired shape of a molding die, and when the composite ceramic is used as a part of the molding die of the present invention, it can be formed into a molding die part. The desired shape. The above composite ceramic is preferably a monomer containing carbon as described above, but the monomer of the carbon is preferably produced by a suitable carbon source in the production process. Specifically, the cerium carbide, the following carbon source, and the previously known additives as required may be subjected to wet mixing and then sintered. In the sintering step, the carbon of the carbon 121126.doc -12-200804228 is usually converted to a monomer. The mixing ratio of each of the above-mentioned raw materials can be appropriately set to [10 parts by weight of carbonaceous stone in the composite ceramic material obtained, and contains 15 parts by weight to 50 parts by weight of carbon particles. The above-mentioned additives are not particularly limited, and examples thereof include sintering aids such as a well-known boron compound, a titanium compound, and a silver oxide compound. The above-described fishing type σ can be mixed using a ball mill, a vibrating ball mill, a planetary ball mill or the like. The solvent to be used for the wet mixing is not particularly limited. It is preferably a solvent such as benzene, toluene or di-f-benzene, or an alcohol-based solvent such as methanol or ethanol; and a ketone solvent such as methyl ethyl ketone. Organic solvents. As the other solvent, water, a mixed solvent of water and the above organic solvent, or the like can be used. The pseudo-sintering of the mixture after the wet mixing is not particularly limited and can be carried out by a previously known method, but from the viewpoint of more fully converting the carbon source used to a carbon monomer' and maintaining good dispersibility, Preferably, the heat treatment is carried out at 150 C to 800 ° C under an n-% gas (ambient gas such as nitrogen or argon). The above carbon source is not particularly limited, and it can be used for wet mixing in which the organic solvent is soluble or dispersible, and can be converted into carbon under the above-mentioned calcination conditions. When the carbon source is a solid powder, it is preferably a material having an average particle diameter of about 1 μm to about 1 Å from the viewpoint of dispersibility. Further, in order to convert the carbon source into a carbon after the calcination, the conversion rate is high, and therefore, the aromatic hydrogen halide is preferably used, and specific examples thereof include a furan resin, a phenol tree, and a coal tar pitch. More preferably, the resin and coal tar are blue. Further, the above-mentioned substance after the sinter can be used as a carbon source. 12I126.doc -13- 200804228: The anti-chemical raw material (particle), as described above, may be any crystal form of α or β. In addition, there is no particular limitation on the purity of the raw materials of the sub-&, ^ children, but from the higher density, &, #f, ^, 、, σ, to improve wear resistance and longevity Fortunately, 90% by weight or more, more preferably 95% by weight or more. The average particle diameter of the carbonaceous material (particles) is not particularly limited, but a powder of G.1 μπι to 1G μπι is preferable from the viewpoint of better sinterability. In addition, the average particle diameter of the two materials (particles) is measured by the laser diffraction/scattering light particle size distribution, and is measured by f, and quotient (commercial nu*LA72〇, manufactured by Horiba, Ltd.). Volume average particle diameter D5. (the same below). + The mixture of the two people after the rice is granulated as needed, and formed into a shape. The molding method is not particularly limited as long as it is formed by a die forming method, an injection, a two-P (cold isostatic pressing) method, or the like, and it is necessary to machine the above-mentioned block to form a molded body having a desired shape. Then, the obtained molded body is supplied to the firing step. The calcination method is particularly limited to the method which can be well known, but it is preferred that it is in the case of [monthly % gas or vacuum, ^ 18 〇 (rc~23〇 (rCT is performed = in i) When the treatment is carried out at the firing temperature, the sintered body is dense, and the mechanical properties such as strength and hardness are further improved. In order to achieve higher density, the upper: firing method is preferably hot pressing or HIP (hot isostatic). Pressure method

该腹合H除了容易地加工成形以外,依存於該特性, 對賦予本發明欲解決之問題之—的成形模所要求之特性具 ::::貢獻,該等特性具體而言’為相對於高溫玻璃之化 予穩疋性(耐氧化性、耐則生、對玻璃之惰性)或耐摩耗 121126.doc 200804228In addition to the ease of processing, the web H is dependent on the characteristics required for the forming mold to which the problem to be solved by the present invention is:::: contribution, which is specifically relative to The high temperature glass is stabilized (oxidation resistance, resistance to life, inert to glass) or abrasion resistance 121126.doc 200804228

又,對於碳化矽,較好的是, 當範圍内調整碳原料之殘碳 不過度地進行原料之溶解。 調整其燒成條件使結晶性提 高,並適當地進行粒子成長。 (本發明之成形模之製造方法) 其次,將說明I發明之成形模之較佳製造方《,但本發 明之成形模之製造方法並非限定於該等方法。當由上述複 合陶瓷構成本發明之成形模全體時,可於上述複合陶瓷之 製k步驟中,將假燒之混合物成形為所需成形模形狀,並 燒成。又,當由上述複合陶瓷構成本發明之成形模之一部 为a守,如上所述,可製作由複合陶瓷而組成之零件,並將 其作為成形模之一部分而組裝,以製造本發明之成形模。 本發明之成形模較好的是,於玻璃製硬碟基板之製造中 與玻璃接觸之表面係如上所述之平滑面。因此較好的是, 根據須要,研磨與上述玻璃之接觸表面。研磨方法並無特 別限制,但當上述複合陶瓷為高硬度材料時,由於以鑽石 以外之研磨料進行研磨時所需之時間變長,因而較好的 是,利用鑽石研磨料進行研磨。從充分確保本發明之成形 模中與玻璃之接觸表面之表面平滑性之觀點而言,所使用 之鑽石研磨料之平均粒徑較好的是2 μπι以下。 當構成本發明之成形模之上述複合陶瓷係以HIP法燒成 121126.doc •15- 200804228 時,可獲得非常高密度之燒結體。藉由所成形之玻璃之表 面而賦予更良好之平滑性,故成形模之相對密度較高較 佳。具體而言’成形模之相對密度較好的是95%以上,更 好的是98%以上。該相對密度可以體積密度除以理論密度 (真比重)來計算,體積密度可根據JIS R1634而測定。再 者,當陶瓷由複數成分構成時,計算各成分之理論密度X 各成分之含有量(重量%^100,並將所獲得之各成分之計 算值之和,作為上述陶瓷全體之理論密度。 (玻璃製硬碟基板之製造方法) 如上所述,本發明之玻璃製硬碟基板之製造方法係包括 下述步驟者,即,將玻璃原料配置於成形模中,並根據須 要於加熱條件下,對上述玻璃原料進行加壓成形之步驟, 上述成形模係本發明之玻璃製硬碟基板用成形模。如上所 述本發明之製造方法中,只要使用本發明之成形模作為成 形模,則其他步驟及處理條件等無任何限制。 對於本發明之玻璃製硬碟基板之製造方法之一例,將使 用圖1進行說明,但本發明並非限制於此。 圖1係表示本發明之玻璃製硬碟基板用成形模之一例之 剖面圖。如該圖所示,成形模具備對向之上模i 〇a與下模 10b,以及將該等上模及下模以可上下移動之方式而連結 之外周部12,101 a係上模l〇a之加工面(與玻璃之接觸面), l〇lb係下模10b之加工面(與玻璃之接觸面)。並且,成形模 中,至少上模10a之加工面l〇la與下模1〇b之加工面1〇1]3係 由上述複合陶瓷而構成。再者,成形模亦可不具備外周 121126.doc -16- 200804228 部。Further, in the case of niobium carbide, it is preferred to adjust the residual carbon of the carbon raw material within the range to dissolve the raw material. The firing conditions are adjusted to increase the crystallinity, and the particles are appropriately grown. (Manufacturing Method of Forming Die of the Present Invention) Next, a preferred manufacturing method of the forming die of the first invention will be described. However, the method of producing the forming die of the present invention is not limited to these methods. When the entire composite mold of the present invention is composed of the above composite ceramics, the pseudo-fired mixture can be formed into a desired mold shape and fired in the k-step of the composite ceramic. Further, when the composite mold of the present invention constitutes a part of the forming mold of the present invention, as described above, a component composed of a composite ceramic can be produced and assembled as a part of the forming mold to manufacture the present invention. Forming die. Preferably, the molding die of the present invention has a smooth surface as described above in contact with the glass in the manufacture of a glass hard disk substrate. Therefore, it is preferred to grind the contact surface with the above glass as needed. The polishing method is not particularly limited. However, when the composite ceramic is a high-hardness material, since the time required for polishing with an abrasive other than diamond is long, it is preferred to use a diamond abrasive for polishing. From the viewpoint of sufficiently ensuring the surface smoothness of the contact surface with the glass in the molding die of the present invention, the average particle diameter of the diamond abrasive to be used is preferably 2 μm or less. When the above composite ceramic constituting the molding die of the present invention is fired by the HIP method 121126.doc • 15 - 200804228, a sintered body of a very high density can be obtained. Since the surface of the formed glass is imparted with better smoothness, the relative density of the forming mold is preferably higher. Specifically, the relative density of the forming die is preferably 95% or more, more preferably 98% or more. The relative density can be calculated by dividing the bulk density by the theoretical density (true specific gravity), which can be measured in accordance with JIS R1634. Further, when the ceramic is composed of a plurality of components, the theoretical density X of each component is calculated (% by weight of 100%, and the sum of the calculated values of the obtained components is used as the theoretical density of the entire ceramic. (Manufacturing Method of Glass Hard Disk Substrate) As described above, the method for producing a glass hard disk substrate of the present invention includes the steps of disposing a glass raw material in a forming mold and, if necessary, under heating conditions. The step of press molding the glass raw material, wherein the forming die is a molding die for a glass hard disk substrate of the present invention. As described above, in the manufacturing method of the present invention, if the molding die of the present invention is used as a molding die, Other steps, processing conditions, and the like are not limited. An example of a method for producing a glass hard disk substrate of the present invention will be described with reference to Fig. 1. However, the present invention is not limited thereto. Fig. 1 is a view showing the glass hard of the present invention. A cross-sectional view of an example of a forming die for a disk substrate. As shown in the figure, the forming die has a facing upper die i 〇a and a lower die 10b, and the upper die and the lower die The outer peripheral portion 12, 101a can be connected to the processing surface (contact surface with the glass) of the upper mold l〇a, and the processing surface (contact surface with the glass) of the lower mold 10b can be moved up and down. In the forming mold, at least the processing surface 10a and the lower surface 1b of the upper mold 10a are formed of the above composite ceramic. Further, the forming mold may not have the outer circumference 121126.doc - 16- 200804228 Department.

首先’於成形模之上模l〇a及下模l〇b之間配置玻璃材料 11(例如,配置於下模10b之加工面⑺讣上)。其次,使上模 l〇a與下模l〇b移動,以此對玻璃材料η加壓,此後,將其 冷卻以成形為玻璃製硬碟基板。繼而,將該成形之玻璃製 硬碟基板從上述成形模中脫模,獲得玻璃製硬碟基板。再 者’本發明之玻璃製硬碟基板用成形模之製造方法之特徵 為使用本發明之成形模,而温度及加重條件等無任何限 制,可如先前眾所周知之方式設定。 玻璃材料11中,可將未加熱之玻璃原料(室溫左右)配置 於上模10a及下模10b之間,並且一邊加熱一邊進行加壓加 工,亦可預先將玻璃原料丨!加熱至特定溫度而成為熔融玻 璃,並使其從熔融玻璃槽通過流出管而向下模l〇b之加工 面流下。加熱處理之溫度並無特別限制,但從成形性之觀 點而言,較好的是2〇〇。〇〜15〇〇〇c ,更好的是 400°C〜1500°C,進而好的是50(rc〜14〇(rc,進而更好的是 峨〜1400。。。又’熔融玻璃之溫度只要可使玻璃原料: 融即可,其並無特別限制,但從成形性之觀點而言,較好 的是200°C〜1500°C,更好的是400。〇〜15〇〇<t,進而 500。〇1400。(:,進而更好的是 6〇(rc〜14〇(rc。 疋 加壓時所施加之壓力並無特別限制,但較好的是0.2 MPa〜50 MPa,由於可進一步縮短加壓時間,故更好的是 0.3 MPa〜40 MPa,進而好的是〇 4 Mpa〜3〇 Mpa。再者,= 使上模10a與下模l〇b之二者移動而進行加壓,亦可如圖】 121126.doc -17- 200804228 之前頭所示,對上模1 (^施加壓力而進行加壓。 上述破璃原料之種類亦無任何限制,可為成形後之形態 為非晶質玻璃之原料,亦可為成形後之形態為結晶化玻璃 (玻璃陶瓷)之原料。 (資訊記錄媒體) 根據本發明,可提供具備上述玻璃製硬碟基板之資訊記 錄媒體。於此情形時,只要使用以上述方法而製作之玻璃 製硬碟基板即可,資訊記錄媒體之其他構成等無任何限 制。 [實施例] 將下述表1所示之碳源、平均粒徑為05 p_碳化矽 粒子(純度98重量%)、以及燒結助劑b4C(2重量%)’於振動 式球磨機中以乙醇進行濕式混合,乾燥後,於5〇代下假 燒2小% ’並將該假燒物藉由乙醇進行濕式粉碎而聚料 化:利用噴霧乾燥機對該漿料進行造粒以獲得顆粒。使用 i等顆粒以CIP法形成為塊,並利用 c〇r〇i)加卫機對所獲得之塊進行加工,以成形為玻璃成 形叙’進而’於氯氣環境下’於2200T:下燒成4小時。再 者,藉由該燒成而形成本發明之碳化石夕_碳複合陶究。對 於燒成後之成形模,以平均粒徑為2 _之鑽石研磨料對鱼 玻璃接觸之表面進行研磨,最終獲得破璃製硬碟基板用成 开> 模。再者,於下述表1巾 厌S有置表示相對於1 重量 份之碳化矽,燒成後之碳含有量。 以下述測定方法對所獲得之成形模之各特性進行評價。 121126.doc 200804228 該等結果一併顯示於下表i中。 (1) 雷射拉曼比 所謂雷射拉曼比,係指碳粒子之結晶相與非晶相之雷射 拉曼分光強度之峰面積比(結晶相/非晶相),其藉由氬雷射 拉曼分光裝置(NEC社製)而測定。 (2) 表面粗度 使用粗度計(小坂技研製),根據JIS B 0651而測定上述 成形模之與玻璃接觸之表面之中心線平均粗度Ra。 (3) 脫模性 使用所製作之成形模,於以下條件製作硬碟基板,並以 下述方式評價上述硬碟基板之硬碟基板成形模之脫模性。 即’於上述成形模中,投入作為原料之玻璃凝塊(G〇b 塊)(黏度logr| : 1〜4),並施加20 MPa之壓力,以此製造玻 璃製硬碟基板。進而,使用相同成形模,連續製造1〇〇〇個 玻璃製硬碟基板,並根據下述評價標準而評價各玻璃製硬 碟基板之脫模性。 (硬碟基板之製作條件) 玻璃成分:Si〇2、Li2〇、A1203、B2〇3、Na20、K20 即將加壓前之玻璃溫度:^(^^〜^(^^(由放射溫度計 測定) 加壓方法:以直接加壓法,使特定重量之熔融玻璃之溫 度降溫至成形溫度區域(1〇§”=7〜1〇)為止,並利用成形模 進行玻璃塊之加壓成形。 冷卻條件··加壓中以熱交換用流體(水)來吸收加壓品之 121126.doc -19 - 200804228 熱量。藉此’加壓面冷卻,因而可捭 又传南品質且局效率之 玻璃成形品。 (評價標準) ◎:表示1000個均脫模良好 〇:表示1000個中有1個脫模不良 △ ··表示1000個中有2〜4個脫模不良 X :表示1000個中有5個以上脫模不良 其中’所謂脫模良好’係指加壓後隨即使成形模之上模 脫離加壓品時’加壓品未移動則為良好,所謂脫模不良, 係指加壓後隨即使成形模之上模離開加壓品時,加壓品移 動,或者加壓品黏附於上模。 (4)耐久性 成形模之耐久性係對上述(3)之脫模性測試後之成形 模,進行表面外觀及其粗度目視之觀察,以及中心線平均 粗度Ra之測定,並根據下述評價標準而進行評價。中心線 平均粗度Ra係分別測定成形模(上模)之與玻璃之接觸面(加 壓面)的中心部及外周部之一點,並求出兩個測定值之 差。圖2中示意性表示成形模之上模。圖2中,圖2(A)係成 形模之上模之剖面圖,圖2(B)係成形模之上模之平面圖。 如圖2(B)所示,對於上述中心部,測定以成形模(上模)之 加壓面之中心點為中心之2 (圖中之箭頭χ),對於上述 外周部’測定自外周(該圖2(B)中闪側之實線)向内側i 〇 mm之更内侧2 mm(圖中之箭頭γ)。下述評價標準中,所謂 粗度變化」’係指上述中心部與外周部之差的粗度差 121126.doc 200804228 異,即,指上述中心部與外周部之差於脫模性測試前後所 產生之變化量。再者,當成形模之耐久性評價較高時,同 樣可認為耐磨耗性亦良好。 (評價標準) ◎:無粗度變化 〇:認為有若干粗度變化 Ra Δ10%以下 △:認為有粗度變化 Ra Δ20%以下 X :認為有較大粗度變化 Ra Δ30%以下 (表1) 碳源 碳 碳化矽 陶瓷 含有量 重量份 平均粒 徑μιη 雷射拉 曼比 含有量 重量份 平均粒 徑μιη 最大空 隙直徑 脫模性測試前 之 Ra(pm) 脫模性 财久性 比較例1 酚樹脂 25 0.25 0.6 100 0.05 11 0.03 X Δ 實施例1 酚樹脂 25 0.4 1.1 100 0.2 5 0.03 〇 ◎ 實施例2 酚樹脂 25 U 1.5 100 0.7 13 0.05 ◎ ◎ 實施例3 酚樹脂 25 3.7 1.9 100 3.9 17 0.2 ◎ ◎ 實施例4 煤焦油瀝青 25 9.9 2.8 100 38 29 0.9 ◎ 0 實施例5 酴樹脂 25 28 2.1 100 5 93 1.1 〇 〇 實施例6 酚樹脂 25 71 1.7 100 1.7 210 3.3 〇 〇 比較例2 酚樹脂 25 150 1 100 13.5 15 0.02 Δ X 比較例3 酚樹脂 25 1.1 1.5 100 110 355 11.7 Δ X 實施例7 酚樹脂 17 5.3 1.7 100 0.7 19 0.1 ◎ ◎ 實施例8 酚樹脂 48 69 1.8 100 0.7 39 0.5 〇 〇 比較例4 酚樹脂 15 0.1 0.4 100 0.05 49 0 Δ Δ 比較例5 酚樹脂 52 7.7 1.1 100 0.7 420 16.9 Δ X 比較例6 紛樹脂 8 1.6 1.2 100 1.3 14 0.09 Δ Δ 實施例9 煤焦油瀝青 25 27 5.8 100 0.7 77 8.9 〇 〇First, a glass material 11 is disposed between the upper mold 〇a and the lower mold 〇b (for example, disposed on the processing surface (7) of the lower mold 10b). Next, the upper mold 10a and the lower mold 10b are moved to pressurize the glass material η, and thereafter, it is cooled to be formed into a glass hard disk substrate. Then, the formed glass hard disk substrate was released from the molding die to obtain a glass hard disk substrate. Further, the manufacturing method of the molding die for a glass hard disk substrate of the present invention is characterized by using the molding die of the present invention, and the temperature and the weighting conditions are not limited, and can be set as previously known. In the glass material 11, the unheated glass raw material (at room temperature or so) can be disposed between the upper mold 10a and the lower mold 10b, and can be pressurized while being heated, or the glass raw material can be smashed in advance! The glass is heated to a specific temperature to be molten glass, and flows from the molten glass tank through the outflow pipe to the processing surface of the lower mold lb. The temperature of the heat treatment is not particularly limited, but from the viewpoint of formability, it is preferably 2 Å. 〇~15〇〇〇c, more preferably 400°C~1500°C, and even better 50(rc~14〇(rc, and more preferably 峨~1400...and the temperature of the molten glass) The glass raw material may be melted, and it is not particularly limited, but from the viewpoint of moldability, it is preferably 200 ° C to 1500 ° C, more preferably 400. 〇 15 15 ° < t, and further 500. 〇 1400. (:, and further preferably 6 〇 (rc 〜 14 〇 (rc. 疋. The pressure applied during pressurization is not particularly limited, but preferably 0.2 MPa to 50 MPa, Since the pressurization time can be further shortened, it is more preferably 0.3 MPa to 40 MPa, and further preferably 〇4 Mpa to 3 〇Mpa. Further, = moving both the upper mold 10a and the lower mold 10b Pressurize, as shown in the previous figure, 121126.doc -17- 200804228, pressurize the upper mold 1 (^ pressure is applied. There is no restriction on the type of the above-mentioned glass raw materials, but it can be formed. The material in the form of amorphous glass may be a raw material in the form of crystallized glass (glass ceramic) after molding. (Information recording medium) According to the present invention, it is possible to provide The information recording medium of the glass hard disk substrate. In this case, the glass hard disk substrate produced by the above method may be used, and other configurations of the information recording medium and the like are not limited. [Examples] The carbon source shown in 1 and the average particle diameter of 05 p_barium carbide particles (purity: 98% by weight) and the sintering aid b4C (2% by weight) were wet-mixed in ethanol in a vibratory ball mill, and dried. Sintering 2% by % under 5 ' generation and polymerizing the smoltar by wet pulverization with ethanol: granulating the slurry with a spray dryer to obtain granules. Using i particles to CIP The method is formed into a block, and the obtained block is processed by a c〇r〇i) adding machine to form a glass forming mold and then fired at 2200T: for 4 hours in a chlorine atmosphere. The carbonized stone-carbon composite ceramic of the present invention is formed by the firing. For the forming mold after firing, the surface of the fish glass contact is ground with a diamond abrasive having an average particle diameter of 2 mm, and finally the broken surface is obtained. The glass hard disk substrate is used to open the > mold. Again, The amount of carbon after firing was measured with respect to 1 part by weight of niobium carbide in the following Table 1. The properties of the obtained molding die were evaluated by the following measurement methods. 121126.doc 200804228 The results are shown together in the following table i. (1) Laser Raman ratio The so-called laser Raman ratio refers to the peak area ratio of the laser Raman splitting intensity of the crystalline phase and the amorphous phase of the carbon particles (crystalline phase /Amorphous phase, which was measured by an argon laser Raman spectroscopic device (manufactured by NEC Corporation). (2) The surface roughness was measured using a roughness meter (developed by Kogyo Co., Ltd.), and the above-mentioned forming mold was measured in accordance with JIS B 0651. The centerline average roughness Ra of the surface in contact with the glass. (3) Mold release property Using the formed mold, the hard disk substrate was produced under the following conditions, and the mold release property of the hard disk substrate forming mold of the hard disk substrate was evaluated as follows. In the above-mentioned molding die, a glass clot (G〇b block) (viscosity logr|: 1 to 4) as a raw material was placed, and a pressure of 20 MPa was applied to produce a glass hard disk substrate. Further, one glass hard disk substrate was continuously produced by using the same molding die, and the mold release property of each glass disk substrate was evaluated in accordance with the following evaluation criteria. (Production conditions of hard disk substrate) Glass composition: Si〇2, Li2〇, A1203, B2〇3, Na20, K20 Glass temperature immediately before pressurization: ^(^^~^(^^(measured by radiation thermometer) Pressurization method: The temperature of the molten glass of a specific weight is cooled to the molding temperature region (1 〇 § = 7 〜 1 〇) by a direct press method, and the glass block is press-formed by a molding die. · During the pressurization, the heat exchange fluid (water) is used to absorb the heat of the pressurized product 121126.doc -19 - 200804228. By this, the 'pressure surface is cooled, so that the glass quality of the south quality and the efficiency can be transmitted. (Evaluation Criteria) ◎: Indicates that 1000 pieces are all released well 〇: indicates that one of the 1000 pieces has a mold release defect △ ·· indicates that there are 2 to 4 pieces of die release in 1000. X: 5 out of 1000 In the above mold release failure, "good mold release" means that the pressurization product does not move even when the mold is removed from the press mold after pressurization, and the mold release is good. When the upper mold of the forming mold leaves the pressing product, the pressing product moves, or the pressing product adheres to the upper portion. (4) Durability of the durable molding die is a visual observation of the surface appearance and the thickness thereof after the mold release test of the above (3), and the measurement of the center line average roughness Ra, and The evaluation was carried out according to the following evaluation criteria: The center line average roughness Ra was measured at one of the center portion and the outer peripheral portion of the contact surface (pressure surface) of the molding die (upper mold) with the glass, and two measurements were determined. The difference between the values. The upper mold of the forming mold is schematically shown in Fig. 2. In Fig. 2, Fig. 2(A) is a cross-sectional view of the upper mold of the forming mold, and Fig. 2(B) is a plan view of the upper mold of the forming mold. As shown in Fig. 2(B), in the center portion, 2 (centered arrow χ) centered on the center of the pressing surface of the forming die (upper die) is measured, and the outer peripheral portion is measured from the outer periphery (this In Fig. 2(B), the solid line on the flash side is 2 mm on the inner side of the inner side 〇mm (the arrow γ in the figure). In the following evaluation criteria, the "thickness change" means the center portion and the outer peripheral portion. The difference in thickness is 121126.doc 200804228, that is, the difference between the center portion and the outer portion is before and after the release test. In addition, when the durability evaluation of the forming mold is high, the abrasion resistance is also considered to be good. (Evaluation criteria) ◎: No change in thickness 〇: There are some roughness changes Ra Δ10% The following △: It is considered that there is a change in roughness Ra Δ20% or less X: It is considered that there is a large thickness change Ra Δ30% or less (Table 1) Carbon source Carbon carbide 矽 Ceramic content Weight part average particle size μιη Laser Raman ratio Weight fraction average particle size μιη Maximum void diameter La (pm) before mold release test Demolding property Comparative example 1 Phenolic resin 25 0.25 0.6 100 0.05 11 0.03 X Δ Example 1 Phenolic resin 25 0.4 1.1 100 0.2 5 0.03 〇 ◎ Example 2 Phenolic resin 25 U 1.5 100 0.7 13 0.05 ◎ ◎ Example 3 Phenolic resin 25 3.7 1.9 100 3.9 17 0.2 ◎ ◎ Example 4 Coal tar pitch 25 9.9 2.8 100 38 29 0.9 ◎ 0 Example 5 酴Resin 25 28 2.1 100 5 93 1.1 〇〇 Example 6 Phenolic resin 25 71 1.7 100 1.7 210 3.3 〇〇 Comparative Example 2 Phenolic resin 25 150 1 100 13.5 15 0.02 Δ X Comparative Example 3 Phenolic resin 25 1.1 1.5 100 110 355 11.7 Δ X Example 7 Phenolic Resin 17 5.3 1.7 100 0.7 19 0.1 ◎ ◎ Example 8 Phenolic Resin 48 69 1.8 100 0.7 39 0.5 〇〇 Comparative Example 4 Phenolic Resin 15 0.1 0.4 100 0.05 49 0 Δ Δ Comparative Example 5 Phenolic Resin 52 7.7 1.1 100 0.7 420 16.9 Δ X Comparative Example 6 Resin 8 1.6 1.2 100 1.3 14 0.09 Δ Δ Example 9 Coal tar pitch 25 27 5.8 100 0.7 77 8.9 〇〇

如上所述,根據本發明之玻璃製硬碟基板用成形模,其 與玻璃之反應性少,耐磨耗性耐久性優異,且成形後之玻 璃從上述成形模表面之脫模性良好。因此,即使連續且長 期地使用本發明之成形模,亦可抑制成形模加工表面之粗 糙或脫模不良,且可高頻率地製造玻璃製硬碟基板。又, -21 · 121126.doc 200804228 所獲得之玻璃製硬碟基板之良率亦提高,故可實現於成形 後實質上無需研磨之表面平滑性。因此,根據本發明之成 形模,可降低玻璃製硬碟基板之成形成本。 【圖式簡單說明】 圖1係表示本發明之玻璃製硬碟基板用成形模之一例之 剖面圖。 圖2係本發明之實施例之玻璃製硬碟基板用成形模之上 棋圖’圖2 A係上述上模之剖面圖,圖2 B係上述上模之平 面圖。 【主要元件符號說明】 上模 下模 材料 外周部 加工面 加工面As described above, the molding die for a glass hard disk substrate according to the present invention has less reactivity with glass and is excellent in abrasion resistance durability, and the release property of the glass after molding from the surface of the molding die is good. Therefore, even if the molding die of the present invention is used continuously and for a long period of time, it is possible to suppress the roughening or mold release failure of the surface of the molding die, and to manufacture the glass hard disk substrate at a high frequency. Moreover, the yield of the glass hard disk substrate obtained by -21 · 121126.doc 200804228 is also improved, so that the surface smoothness which is substantially unnecessary after polishing can be realized. Therefore, according to the molding die of the present invention, the forming cost of the glass hard disk substrate can be reduced. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a cross-sectional view showing an example of a molding die for a glass hard disk substrate of the present invention. Fig. 2 is a cross-sectional view of the upper mold of Fig. 2A, and Fig. 2B is a plan view of the upper mold, in a forming mold for a glass hard disk substrate according to an embodiment of the present invention. [Description of main component symbols] Upper die Lower die material Outer peripheral part Processing surface Processing surface

10 a 10b 11 12 101a 101b 121126.doc -22-10 a 10b 11 12 101a 101b 121126.doc -22-

Claims (1)

200804228 十、申請專利範圍: 1 · 一種玻璃製硬碟基板用成形模,其係含有碳化矽_碳複合 陶瓷者, 其中上述碳化矽-碳複合陶瓷中,對於10()重量份之碳 化石夕,含有15〜50重量份之碳粒子,且上述碳粒子之平 • 均粒徑為0·3 μηι〜100 μιη之範圍。 ' 2.如請求項1之玻璃製硬碟基板用成形模,其中上述碳化 矽-碳複合陶瓷中碳化矽之平均粒徑為〇3 μηι〜1〇〇 μηΐ2 _ 範圍。 3·如請求項1或2之玻璃製硬碟基板用成形模,其中上述碳 粒子之結晶相與非晶相之雷射拉曼分光強度之峰值面積 比(結晶相/非晶相)為1〜10。 4. 如請求項1或2之玻璃製硬碟基板用成形模,其中上述複 合陶瓷之最大空隙直徑為300 μηι以下。 5. 如請求項丨或2之玻璃製硬碟基板用成形模,其中於玻璃 製硬碟基板成形時,與玻璃接觸之上述成形模表面之中 # 心線平均粗度“為0.001 μ^η以上、10μιη以下。 6. -種玻璃製硬碟基板之製造方法,其係包括於成形模中 配置玻璃原料並對上述玻璃原料進行加壓成形之玻璃成 形步驟,且上述成形模係請求項丨〜5中任一項之玻璃製 硬碟基板用成形模。 ^ 7. 如請求項6之玻璃製硬碟基板之製造方法,#中於上述 =〇^。成$、步驟中’在將上述玻璃原料加熱至200°c〜 1500 C之狀態下,對上述玻璃原料施加〇·2〜50 MPa之壓 力而成形。 121126.doc200804228 X. Patent application scope: 1 . A molding die for a glass hard disk substrate, which comprises a cerium carbide-carbon composite ceramic, wherein the carbonized cerium-carbon composite ceramic has 10 () parts by weight of carbonized fossil eve And containing 15 to 50 parts by weight of carbon particles, and the carbon particles have a flat average particle diameter ranging from 0·3 μηι to 100 μιη. 2. The molding die for a glass hard disk substrate according to claim 1, wherein the average particle diameter of the niobium carbide in the niobium carbide-carbon composite ceramic is in the range of 〇3 μηι to 1〇〇 μηΐ2 _. 3. The molding die for a glass hard disk substrate according to claim 1 or 2, wherein a peak area ratio (crystalline phase/amorphous phase) of the laser Raman spectral intensity of the crystal phase of the carbon particles to the amorphous phase is 1 ~10. 4. The molding die for a glass hard disk substrate according to claim 1 or 2, wherein the composite ceramic has a maximum void diameter of 300 μη or less. 5. The molding die for a glass hard disk substrate according to claim 2 or 2, wherein in the surface of the forming die which is in contact with the glass during molding of the glass hard disk substrate, the mean diameter of the core line is "0.001 μ? The above-mentioned method of manufacturing a glass hard disk substrate includes a glass forming step of disposing a glass raw material in a molding die and press-molding the glass raw material, and the above-mentioned forming die request item A molding die for a glass hard disk substrate according to any one of the above-mentioned items. ^ 7. The method for producing a glass hard disk substrate according to claim 6, wherein the above-mentioned = 〇 ^. The glass raw material is heated to a temperature of 200 ° C to 1500 C, and a pressure of 〇 2 to 50 MPa is applied to the glass raw material to form.
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