TW313562B - Chromium carbide based ceramics composite block gauge and its preparation - Google Patents

Chromium carbide based ceramics composite block gauge and its preparation Download PDF

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TW313562B
TW313562B TW84103995A TW84103995A TW313562B TW 313562 B TW313562 B TW 313562B TW 84103995 A TW84103995 A TW 84103995A TW 84103995 A TW84103995 A TW 84103995A TW 313562 B TW313562 B TW 313562B
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Taiwan
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powder
chromium carbide
block gauge
tungsten carbide
carbide
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TW84103995A
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Chinese (zh)
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Jong-Pyng Lay
Cherng-Tzuu Fuh
Jia-Ruey Duann
Ay-Gang Lih
Kae-Lih Ger
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Ind Tech Res Inst
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Abstract

A method for preparing chromium carbide ceramic block gauge comprises the steps of: (1) preparing a starting powder of chromium carbide (Cr3C2) base material having diameters of 0.3 to 10.0 (muon)m; (2) adding 10 to 35 percent by volume of tungsten carbide (WC) powder having diameters of 0.1 to 15.0 (muon)m into the chromium carbide base powder and mix thoroughly; (3) adding deionized water in the resultant powder and mixing the same to give a homogeneous slurry; (4) de-watering and drying the resultant slurry followed by press-forming: (5) sintering the formed solid composite by hot pressing; and (6) grinding the resultant composite to desired size.

Description

經濟部中央標準局員工消費合作社印製 313502 A7 B7 五、發明説明(丨) 【發明之應用範疇】 本發明是關於一種複合陶瓷塊規,特別是關於一種碳 化鉻複合陶瓷塊規。本發明之陶瓷塊規,具有比金屬塊規 更優良之抗氧化性及耐腐蝕性,並較一般陶瓷塊規具有更 高之反光度,可利用光干涉技術,作爲校正工具。. 【發明之背景】 標準塊規已廣泛地應用在工業及學術界,作爲長度量 測的標準。現在產業界所使用之標準塊規多以高碳合金所 製作,少數則以陶瓷材料製成(美國專利5,272,120,日 本專利63188701)。在以金屬爲材質之塊規方面,現有之 合金塊規表面容易氧化並極易刮傷。因此使用此類塊規必 須非常小心,以防刮傷;也不可留下指紋以免產生鏽斑。 這種塊規儲存時必須上油,再次使用時必須經過數道的除 油程序,以避免油膜厚度造成量度誤差。然而除油時,由 於油膜表面所附著之大氣灰塵粒子,容易造成塊規表面之 刮傷,進而影響到量器精度。因此使用此類金屬質塊規極 爲不便。 在以陶瓷爲材質(氧化鍩、氧化鋁、碳化矽或氮化矽 )之塊規方面,雖然較金屬材料具有高強度、硬度、不易 氧化等優異之特性,然而由於其反光度不足(請參見表一 ),因此無法以習用之光干涉技術作長度量測與校正。造 成陶瓷塊規在加工製作與校正上的困擾。 另外,也有人利用在碳化物(如碳化鉻或碳化鎢)材 料中,添加入金屬黏結劑(如鈷、鎳或鉻)來製做陶瓷塊 規產品。雖然碳化絡材料具有高感光度,但是由於金屬黏 結劑的添加,造成材料的硬度値下降,抗氧化性及抗腐蝕 > 皆爲之劣化,進而減短產品的使用壽命。因此也不是一種 V Bufl i · (請先閱讀背面之注意事項再填寫本頁) --^裝--- -訂 M tuf it mu —em ml mav fm mu 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 83. 3.10,000 經濟部中央標準局員工消費合作社印製 S13562 A7 B7 五、發明説明(Z ) 有利的解決方式。因此目前業界亟須一種新穎之塊規,該 塊規兼具陶瓷材質塊規高硬度,高抗腐蝕,不易氧化以及 金屬材質塊規適合應用於光干涉技術之優點者。 【發明的目的】 本發明之目的主要提供產品業界一種新穎的陶瓷塊規, 以提供一種兼具陶瓷塊規高硬度、高抗腐蝕,不易氧化等 優點,及金屬塊規適合光干涉技術應用之優點之塊規。 ' 本發明之目的也在提供一新穎的陶瓷基複合材料塊規。 本發明之目的也在提供一種陶瓷基複合材料塊規之製 作方法。 【發明之簡述】 本發明之複合陶瓷塊規乃利用不含金屬添加劑的碳化 鉻(Cr3C2)基體,加入碳化鎢(WC)強化相,經熱壓法燒 結而製成原材,再經切割及硏磨而形成塊規。經本發明之 方法所製成之複合陶瓷塊規,具有之特性包括:高抗腐飩 性;高硬度;優異的材質強度與韌性;近於鋼質材料(特 別是不銹鋼材)之熱膨脹係數,因此溫度變化所引起量器 與被測物之相對誤差較小;及優異的反射率及表面光澤度。 因此習用之光干涉量測工具,可以用來校正本發明之複合 陶瓷塊規。這是一般市售之陶瓷塊規所無法達到的效果。 上述及其他未發明之優點及目的,可經由以下說明並 參照下列圖式,而更形淸楚: 【圖式之簡單說明】 第1圖表示本發明碘化鉻複合陶瓷塊規之製作流程圖。 表一係各習用塊規材料表面反光度測試値。 表二係顯示經由本發明之方法所製成之複合陶瓷塊規 特性測試結果。 -4 - (請先閱讀背面之注意事項再填寫本頁) —f 裝------訂-----' 銀 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 經濟部中央標準局員工消費合作社印製 31S562 A7 B7 五、發明説明(3 ) [發明之詳細說明】 本發明之複合陶瓷塊規原材之詳細製作流程如第1圖 所示。 首先在(101)製備預訂比例的粉體:0〜30M%之碳化 鎢讎,在(102)製備碳化鉻讎,而在(103)將二者混合。 兩者起始粉體的粒徑約在0.2〜10/zm之間,其平均粒徑分 別爲 Q.2 及 1.5#πι。. 接著在(104)將粉體置入去離子水內,經24小時混合 處理後,於(105)將鑄型所得之均質策料再予以去水乾燥》 過篩及加壓成型,並於(106)將鑄型放入石墨模中,以熱 壓方式利用14⑽1至1700°(:之高溫燒結。燒結時所使用之 壓力在0〜50MPa之間,而保持時間在30分至4小時,燒結 氣氛採用還原氣氛(氬氣或氮氣)或眞空。燒結後試片於 (107)經600號石磨輪加工製成略大預訂尺寸之長方體,最 後再在(108)經由多道的精密硏磨而達成預訂的平面度與 尺寸。 由上述方式製成之複合陶瓷塊規基體內含有均質的碳 化鎢與碳化鉻混合相。其材質非常緻密且不須用任何金屬 質之燒結助劑。因此,本發明之碳化鎢/碳化鉻複合陶瓷 塊規成品,不但保有碳化鉻材料所具有之優異特性,諸如 光澤及抗腐飩等特點,其抗折強度與韌度也較純碳化鉻原 材增強了許多。同時硬度也明顯的上昇。. 表2顯示經由本發明之方法所製成之複合陶瓷塊規特 性測試結果。如表所示,本發明之複合陶瓷塊規確具有優 異之特性。. .Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 313502 A7 B7 V. Description of the invention (丨) [Application range of the invention] The present invention relates to a composite ceramic block gauge, in particular to a chromium carbide composite ceramic block gauge. The ceramic block gauge of the present invention has better oxidation resistance and corrosion resistance than the metal block gauge, and has higher reflectance than the general ceramic block gauge, and can use light interference technology as a correction tool. [Background of the invention] Standard block gauges have been widely used in industry and academia as a standard for length measurement. At present, the standard block gauges used in the industry are mostly made of high-carbon alloys, and a few are made of ceramic materials (US Patent 5,272,120, Japanese Patent 63188701). In terms of metal block gauges, the existing alloy block gauges are easily oxidized and scratched. Therefore, the use of such blocks must be very careful to prevent scratches; fingerprints should not be left to avoid rust. This block gauge must be filled with oil when stored, and must go through several degreasing procedures when used again to avoid measurement errors caused by the thickness of the oil film. However, when degreasing, atmospheric dust particles attached to the surface of the oil film can easily cause scratches on the surface of the block gauge, which in turn affects the accuracy of the gauge. Therefore, it is extremely inconvenient to use such metal block gauges. In terms of block gauges made of ceramics (metal oxide, aluminum oxide, silicon carbide, or silicon nitride), although they have higher strength, hardness, and not easy to oxidize than metal materials, due to their insufficient reflectivity (see Table 1) Therefore, the conventional light interference technique cannot be used for length measurement and correction. The difficulties in processing and calibration caused by the ceramic block gauge. In addition, it is also used to add metal binders (such as cobalt, nickel or chromium) to carbide (such as chromium carbide or tungsten carbide) materials to make ceramic block products. Although the carbonized material has high sensitivity, due to the addition of metal binder, the hardness value of the material is reduced, and the oxidation resistance and corrosion resistance are all deteriorated, thereby shortening the service life of the product. Therefore, it is not a kind of V Bufl i. (Please read the precautions on the back before filling in this page)-^ 装 --- -book M tuf it mu —em ml mav fm mu This paper standard is applicable to China National Standard (CNS) A4 specification (210X297 mm) 83. 3.10,000 Printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs S13562 A7 B7 V. Invention description (Z) An advantageous solution. Therefore, there is an urgent need for a novel block gauge in the industry, which combines the advantages of ceramic block gauges with high hardness, high corrosion resistance, not easy to oxidize, and metal block gauges suitable for use in optical interference technology. [Object of the invention] The object of the present invention is to provide a novel ceramic block gauge in the product industry, to provide a combination of ceramic block gauge with high hardness, high corrosion resistance, not easy to oxidize, etc., and metal block gauge suitable for the application of light interference technology The advantages of the block gauge. 'The purpose of the present invention is also to provide a novel ceramic matrix composite block gauge. The object of the present invention is also to provide a method for manufacturing a ceramic matrix composite block gauge. [Brief Description of the Invention] The composite ceramic block gauge of the present invention uses a chromium carbide (Cr3C2) matrix without metal additives, adds a tungsten carbide (WC) strengthening phase, is sintered by hot pressing to make a raw material, and is then cut And grinding to form a block gauge. The composite ceramic block gauge made by the method of the present invention has the following characteristics: high corrosion resistance; high hardness; excellent material strength and toughness; thermal expansion coefficient close to that of steel materials (especially stainless steel), Therefore, the relative error between the measuring instrument and the measured object caused by the temperature change is small; and the excellent reflectance and surface glossiness. Therefore, the conventional optical interference measurement tool can be used to correct the composite ceramic block gauge of the present invention. This is an effect that cannot be achieved by the commercially available ceramic block gauges. The above-mentioned and other uninvented advantages and purposes can be made more obvious by the following description and referring to the following drawings: [Simple description of the drawings] Figure 1 shows the flow chart of the production of the chromium iodide composite ceramic block gauge of the present invention. Table 1 is the surface reflectance test values of various conventional block gauge materials. Table 2 shows the test results of the characteristics of the composite ceramic block gauge manufactured by the method of the present invention. -4-(Please read the precautions on the back before filling in this page) —f Pack ------ ordered ----- 'The size of the silver paper is applicable to the Chinese National Standard (CNS) A4 specification (210X297mm) 31S562 A7 B7 printed by the Staff Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy V. Description of the invention (3) [Detailed description of the invention] The detailed production process of the composite ceramic block gauge raw material of the present invention is shown in Figure 1. First, a predetermined ratio of powder is prepared in (101): 0 to 30 M% tungsten carbide, chromium carbide is prepared in (102), and the two are mixed in (103). The particle size of the starting powder of the two is about 0.2 ~ 10 / zm, and the average particle size is Q.2 and 1.5 # πι. . Then put the powder into deionized water at (104), and after 24 hours of mixing treatment, at (105), the homogeneous material obtained from the casting mold is then dried by dewatering, sieving and press forming, and (106) Put the casting mold into the graphite mold, and sinter it at a high temperature of 14⑽1 to 1700 ° (:. The pressure used during sintering is between 0 ~ 50MPa, and the holding time is 30 minutes to 4 hours. The sintering atmosphere is a reducing atmosphere (argon or nitrogen) or emptiness. After sintering, the test piece is processed by a 600 stone grinding wheel at (107) to form a cuboid with a slightly larger predetermined size, and finally at 108, through multiple precision grinding To achieve the predetermined flatness and size. The composite ceramic block gauge made by the above method contains a homogeneous mixture of tungsten carbide and chromium carbide. The material is very dense and does not require any metal sintering aids. Therefore, The finished tungsten carbide / chromium carbide composite ceramic block gauge of the present invention not only retains the excellent characteristics of the chromium carbide material, such as gloss and anti-corrosion characteristics, but also has higher bending strength and toughness than pure chromium carbide raw materials. Many. At the same time the hardness is also obvious Table 2 shows the increase .. Composite ceramics block Laid test results made by the method of the present invention. As shown in Table, the composite ceramics block indeed present invention have excellent characteristics of ...

雖然不需爲任何理論所拘束,但本發明之複合陶瓷塊 規具有提高之硬度値,顯是基於高楊氏係數(Young’ S -5 - (請先閲讀背面之注意事項再填寫本頁) ---訂 Λ -mu fm Bm nn n^— 1 n^i— 1-11¾ 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 經濟部中央標準局員工消費合作社印製 A7 B7 五、發明説明(4 ) modulus)的碳化鎢添加相所導致(碳化鎢之楊氏係數爲 710GPa,而碳化鉻之楊氏係數約385GPa)。 此外,強度與韌度之增加是由於碳化鎢與碳化鉻之熱 膨脹係數差異(碳化鎢6.9 X10-6/°C而碳化鉻約11.2 X10-6/°C )〇這種熱膨脹係數之差異源於材料燒結緻密後的冷 . 卻過程中,造成碳化鎢/碳化鉻介面產生殘餘應力。這種 殘餘應力造成基材的破壞方式:從單質碳化鉻的沿晶破壞, 變成複合材料之穿晶破壞模式。這種模式轉變促使材料之 強度顯著提昇。 至於本發明之複合陶瓷塊規之所以具有較高之韌度, 主因在於碳化鎢添加相造成之裂痕轉折及橋架的韌化機構 所導致。而本發明之複合陶瓷塊規,其熱膨脹係數 由 11.2xl(H/aC,降至9.5xlO-6/°C (20Vol%之碳化鎢添 加物)。由於一麵質待測物之熱膨腿茅、數約在10X10— 6/°C左右。因此使用本發明之塊規量測一般鋼質待測物時, 可以減少因溫度偏移所造成之量測誤差。 本發明之複合陶瓷塊規,其表面光澤性及光反射率均 較現有之市售陶瓷塊規(如碳化矽、氮化砍、氧化结、及 氧化鋁)高出甚多。近乎於一般市售之鋼質規材料(如表 一中試片14所示)。以完全緻密的單體碳化鉻材料爲例 (如表1試片9),在45度及90度的反射率平均値分别是 47.7%及55%。如加入20Vol%的碳化鎢顆粒於碳化鉻基材 (如表1中試片7),不但其機械獲得顯著提昇,而且仍能 保持優異的反射率特性。在45度及90度的反射率平均値分 別是43.7%及51% 〇此値較之一般常用的陶瓷塊規材料(如 氧化鋁(2.4%)、氧化銷(6.4%、氮化矽(4.1%)及碳化矽 (9.3%)等)的反射率超越甚多。因此,本發明之複合陶瓷 (請先閱讀背面之注意事項再填寫本頁) —f--裝--- 丁 、-& --— 本紙張尺度適用中國國家標準(CNS ) A4規格(210X 297公釐) S13562 A7 B7 五、發明説明(夕) 塊規適合以習用之光干渉法技術校正其尺寸誤差。這是一 般市售陶瓷質塊規所無法達到的。 以上是有關於本發明碳化鉻複合陶瓷塊規之說明。習 於斯藝之人士不難由以上之說明瞭解本發明之精神,並據 以作出不同之變化與引申。唯若不超出本發明之精神,均 在其專利範圍之內。 (請先閱讀背面之注意事項再填寫本頁)Although not bound by any theory, the composite ceramic block gauge of the present invention has an increased hardness value, which is obviously based on the high Young's coefficient (Young 'S -5-(please read the precautions on the back before filling this page) --- Subscribe Λ -mu fm Bm nn n ^ — 1 n ^ i— 1-11¾ This paper scale is applicable to China National Standard (CNS) A4 (210X297mm) A7 B7 printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs V. Description of the invention (4) Modulus) caused by the addition phase of tungsten carbide (Young's coefficient of tungsten carbide is 710 GPa, and the Young's coefficient of chromium carbide is about 385 GPa). In addition, the increase in strength and toughness is due to the difference in the thermal expansion coefficients of tungsten carbide and chromium carbide (tungsten carbide 6.9 X10-6 / ° C and chromium carbide approximately 11.2 X10-6 / ° C). This difference in thermal expansion coefficients originates from The material is cold after sintering and compacting. However, during the process, residual stress is generated in the tungsten carbide / chromium carbide interface. This residual stress causes the destruction of the substrate: from the intergranular destruction of elemental chromium carbide to the transgranular failure mode of the composite material. This mode change has led to a significant increase in the strength of the material. The reason why the composite ceramic block gauge of the present invention has higher toughness is mainly due to the cracking caused by the addition phase of tungsten carbide and the toughening mechanism of the bridge. The composite ceramic block gauge of the present invention has a coefficient of thermal expansion from 11.2xl (H / aC, down to 9.5xlO-6 / ° C (20Vol% tungsten carbide additive). Due to the thermal expansion of the test object on one side The number is about 10X10-6 / ° C. Therefore, when using the block gauge of the present invention to measure general steel objects, the measurement error caused by temperature deviation can be reduced. The composite ceramic block gauge of the present invention The surface gloss and light reflectance are much higher than the existing commercially available ceramic block gauges (such as silicon carbide, nitride cutting, oxide junction, and alumina). It is almost the same as the general commercially available steel gauge materials ( As shown in the test piece 14 in Table 1.) Taking the fully dense single chromium carbide material as an example (see test piece 9 in Table 1), the average reflectance values at 45 degrees and 90 degrees are 47.7% and 55%, respectively. If 20Vol% of tungsten carbide particles are added to the chromium carbide substrate (such as test piece 7 in Table 1), not only its mechanical properties are significantly improved, but it still maintains excellent reflectance characteristics. The average reflectivity at 45 degrees and 90 degrees Values are 43.7% and 51% respectively. This value is compared with the commonly used ceramic block gauge materials (such as alumina (2.4%), oxide sales (6.4%, nitrogen The reflectivity of siliconized silicon (4.1%) and silicon carbide (9.3%) etc. surpasses much. Therefore, the composite ceramic of the present invention (please read the precautions on the back before filling in this page) —f-- 装 --- D,-& --- This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X 297 mm) S13562 A7 B7 V. Description of invention (Xi) The block gauge is suitable for correcting its dimensional error using conventional light interference technology This is beyond the reach of commercially available ceramic block gauges. The above is a description of the chromium carbide composite ceramic block gauge of the present invention. It is not difficult for those who are acquainted with Siyi to understand the spirit of the present invention from the above description and based on it Make different changes and extensions. Only if it does not exceed the spirit of the invention, it is within the scope of its patent. (Please read the precautions on the back before filling this page)

、tT 經濟部中央標準局員工消費合作社印裂 -7 - 本紙張尺度適用中國國家標準(CNS } A4規格(210X297公釐), TT Ministry of Economic Affairs, Central Standards Bureau, Employee Consumer Cooperative Printed Crack -7-This paper size is applicable to the Chinese National Standard (CNS} A4 specification (210X297 mm)

Claims (1)

If, MW 公告本 A8 B8 C8 D8 申請專利範圍 經濟部中央揉準局負工消費合作社印$L 第84103 995號申請專利範圍修正本 1. 一種碳化鉻複合陶瓷塊規之製法,包括: 製備碳化鉻(Cr3C2)基材之起始粉體’粒徑在〇.3 〜10_0/zm間; 在碳化鉻基材粉體中加入體積百分比1 _〇〜3 5之碳化 鎢(WC)粉末,其粒徑則在0.1〜15.0//Π1間,並予充分混 合; 在所得之粉體中加入去離子水,並予混合成爲均質 之漿料; 將所得之漿料去水乾燥,加壓成型; 將成型之固態組成物作熱壓處理,使之燒結;及 將所得之組成物硏磨至所需之尺寸。 2..如申請專利範圍第1項之製法,其中碳化鎢之起始 體積百分比爲14〜25。 3. 一種碳化鉻複合陶瓷塊規,其中包含碳化鉻基材, 其粒徑在〇3〜10.0//m間,及體積百分比爲10〜35之碳化 鎢粉末強化相,其粒徑在0.1〜l5.〇em間;並以包括下列 步驟製得者: 將該碳化路粉體、該碳化鶴粉體,.力Π入去離子水混 合成均質漿料; 將該漿料去水乾燥,加壓成形; 將該成形之組成物作熱壓燒結處理;及 將所得之燒結體硏磨至所需尺寸。 4· 如申請專利範圍第3項之塊規,其中碳化鎢強化相 之增加量爲14〜25體積百分比。 . (請先閣讀背面之注意事項再填寫本頁) 丁 - I J'a A) 本紙張尺度適用中國國家棣準(CNS ) A4規格(210X297公釐)If, MW Announcement A8 B8 C8 D8 Application for Patent Scope The Ministry of Economic Affairs Central Bureau of Accreditation Consumer Cooperatives Printing $ L No. 84103 995 Application for Patent Scope Amendment 1. A method of making chromium carbide composite ceramic blocks, including: preparation of chromium carbide (Cr3C2) The starting powder of the base material has a particle size of 0.3 ~ 10_0 / zm; add vol. 1_〇 ~ 3 5 volume percent tungsten carbide (WC) powder to the chromium carbide base material powder The diameter is between 0.1 ~ 15.0 // Π1, and fully mixed; add deionized water to the obtained powder, and premix to form a homogeneous slurry; dry the resulting slurry to dryness, press molding; The formed solid composition is hot-pressed to sinter it; and the resulting composition is ground to a desired size. 2. The method as claimed in item 1 of the patent application scope, in which the initial volume percentage of tungsten carbide is 14-25. 3. A chromium carbide composite ceramic block gauge, which contains a chromium carbide base material with a particle size of 〇3 ~ 10.0 // m, and a volume percentage of 10 ~ 35 tungsten carbide powder reinforced phase with a particle size of 0.1 ~ l5.〇em room; and made by the following steps: the carbonized road powder, the carbonized crane powder, force Π into deionized water mixed into a homogenous slurry; the slurry was dried to dry, add Compression forming; hot-sintering the formed composition; and grinding the resulting sintered body to a desired size. 4. As the block gauge of item 3 of the patent application scope, the increase of the tungsten carbide strengthening phase is 14 ~ 25 volume percent. (Please read the precautions on the back before filling in this page) Ding-I J'a A) This paper size is applicable to China National Standard (CNS) A4 (210X297mm)
TW84103995A 1995-04-19 1995-04-19 Chromium carbide based ceramics composite block gauge and its preparation TW313562B (en)

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