WO2012060211A1 - アルミナ質焼結体、砥粒、及び砥石 - Google Patents
アルミナ質焼結体、砥粒、及び砥石 Download PDFInfo
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- WO2012060211A1 WO2012060211A1 PCT/JP2011/073898 JP2011073898W WO2012060211A1 WO 2012060211 A1 WO2012060211 A1 WO 2012060211A1 JP 2011073898 W JP2011073898 W JP 2011073898W WO 2012060211 A1 WO2012060211 A1 WO 2012060211A1
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- sintered body
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- alumina
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- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
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Definitions
- the present invention relates to an alumina sintered body, an abrasive grain using the alumina sintered body, and a grindstone using the abrasive grain.
- Alumina sintered bodies are used in various industrial fields by taking advantage of their high hardness, high strength, high heat resistance, high wear resistance, and high chemical resistance. In particular, it is used as a raw material (abrasive grain) for heavy grinding wheels in the steel industry.
- the grinding ratio of the grindstone affects the "hardness” and "fracture toughness” of the abrasive grains used in the grindstone. Is done. It is considered that the following relationship exists between “grinding ratio and hardness” and “grinding ratio and fracture toughness”. (1) As the hardness of the abrasive grains increases, the grinding amount increases, so the grinding ratio increases. (2) When the fracture toughness increases, the amount of abrasive wear decreases, so the grinding ratio increases.
- the numerator portion in the grinding ratio equation is affected by the grinding amount, and the denominator portion is affected by the wear amount.
- abrasive grains for conventional heavy grinding wheels abrasive grains obtained by sintering an alumina fine powder raw material (for example, see Patent Documents 1 to 3) and fused alumina zirconia abrasive grains (for example, see Patent Document 4).
- Abrasive grains obtained by adding a crystal grain growth inhibitor such as magnesium oxide to high-purity fine-grained alumina powder see, for example, Patent Document 5
- a crystal grain growth inhibitor such as magnesium oxide
- Patent Document 6 a sintered material in which aluminum oxide is the main material and TiO 2 is added has been proposed. Furthermore, as an alumina sintered body having high hardness and high fracture toughness and excellent wear resistance, an alumina sintered body to which a metal compound such as Ti, Mg, Fe, etc., which can be dissolved in an alumina crystal, has been proposed. (For example, see Patent Document 7).
- Patent Documents 1 to 5 do not specifically disclose abrasive grains having high hardness and low fracture toughness, or low hardness and high fracture toughness, and high hardness and high fracture toughness.
- the sintered material of Patent Document 6 has been evaluated for hardness, no consideration is given to fracture toughness.
- the alumina sintered body of Patent Document 7 discloses only a combination of Ti and Mg and a combination of Fe and Mg, and other combinations are not specifically disclosed.
- the present invention has been made under such circumstances, an alumina sintered body that gives abrasive grains having high hardness and excellent fracture toughness, abrasive grains using the alumina sintered body, and the abrasive grains It aims at providing the grindstone which uses this.
- the present inventors have made titanium compounds (particularly titanium oxides) and iron compounds (particularly iron oxides) as compounds to be contained in the alumina sintered body. It was noticed and it was found that the characteristics of the alumina sintered body can be improved by controlling the total amount thereof (the total amount of contents converted into oxides). The present invention has been completed based on such findings.
- the present invention is as follows.
- An alumina sintered body containing a titanium compound and an iron compound wherein the total amount of the titanium compound content converted to TiO 2 , the iron compound content converted to Fe 2 O 3 and the alumina content is 98 mass% or more, the total amount of the content of the titanium compound converted to TiO 2 and the content of the iron compound converted to Fe 2 O 3 is 5 to 13 mass%, and the content of the titanium compound converted to TiO 2 and mass ratio of the iron compound calculated as Fe 2 O 3 was the content (TiO 2: Fe 2 O 3 ) is 0.85: 1.15 to 1.15: alumina sintered body is 0.85.
- an alumina sintered body that gives abrasive grains having high hardness and excellent fracture toughness, an abrasive grain using the alumina sintered body, and a grindstone using the abrasive grain. it can.
- the alumina-based sintered body of the present invention contains a titanium compound and an iron compound, and the content obtained by converting the titanium compound to TiO 2 (hereinafter sometimes referred to as “TiO 2 converted content”) and the iron compound are Fe 2 O 3.
- TiO 2 converted content the content obtained by converting the titanium compound to TiO 2
- Fe 2 O 3 converted content the content obtained by converting the titanium compound to TiO 2
- the total amount of the three components of the converted content (hereinafter sometimes referred to as “Fe 2 O 3 converted content”) and the alumina content is 98% by mass or more.
- the total amount of the two components of the TiO 2 equivalent content and the Fe 2 O 3 equivalent content is 5 to 13% by mass, and preferably 7 to 10% by mass.
- the mass ratio (TiO 2 : TiO 2 : content converted to TiO 2 content and Fe 2 O 3 content) Fe 2 O 3 ) is 0.85: 1.15 to 1.15: 0.85.
- the ratio (TiO 2 : Fe 2 O 3 ) is preferably 0.90: 1.10 to 1.10: 0.90, and 0.95: 1.05 to 1.05: 0.95. More preferably.
- the hardness decreases as the total amount increases. If it is in the range of the invention, the average Vickers hardness, which is an index of hardness, is, for example, 16 GPa or more, and the hardness is practically excellent.
- the relationship between the total amount of the two components and the fracture toughness is not related to the above-mentioned hardness, but the present inventors have found that the fracture toughness is remarkably increased in the specific range of the two components. It was. That is, if the total amount of the two components is within the range of the present invention, the fracture toughness value is, for example, 3.0 MPa ⁇ m 1/2 or more.
- FIG. 3 shows the way of propagation of cracks in the direction of arrow Y along the grain boundaries of the alumina particles 12.
- FIG. 4B shows the SEM photograph of a sintered body according to Comparative Example 1 described later.
- FIG. 4 (A) shows the state of the crystal structure before applying an impact
- FIG. 4 (B) applied the impact. The state of subsequent crack propagation is shown.
- a crystal phase for example, FeTiAlO 5 particles 10
- a crystal phase for example, FeTiAlO 5 particles 10
- the presence of the FeTiAlO 5 particles 10 at the grain boundaries of the alumina particles 12 causes the cracks to deviate in the direction of the arrow X starting from the particles 10 even when cracks that occur when an impact is applied are advanced. Therefore, the impact force is dispersed and relaxed instead of in one direction. Therefore, it is considered that the fracture toughness value as a whole increases. This can also be seen from SEM photographs showing the results of the impact test shown in FIG.
- FIG. 2 is an SEM photograph of a sintered body according to Example 3 to be described later.
- the gray portion (light-colored portion) located at the triple point at the grain boundary of alumina particles is FeTiAlO 5 particles. Equivalent to.
- ilmenite titanium oxide
- FeTiO 3 a raw material containing Ti and Fe.
- the presence of the FeTiAlO 5 particles provides an alumina sintered body that provides abrasive grains having high hardness and excellent fracture toughness.
- the FeTiAlO 5 particles can obtain an alumina sintered body having high hardness and excellent fracture toughness due to an action such that the fracture toughness is higher than that of the corundum phase.
- the presence of the crystal phase composed of FeTiAlO 5 particles and the average crystal size can be confirmed by the method described in Examples below.
- the average crystal size of the crystal phase (FeTiAlO 5 particles) of the composite metal oxide containing Ti, Fe and Al is preferably 3.4 to 7.0 ⁇ m from the viewpoint of achieving high fracture toughness. More preferably, it is 6.5 ⁇ m.
- the thickness is 3.4 to 7.0 ⁇ m, the effect of suppressing the progress of cracks generated at the time of breakage is increased. This is because if the average crystal size is in this range, the effect of deflecting cracks by the FeTiAlO 5 particles can be kept good.
- the alumina sintered body of the present invention is a silicon compound and / or calcium which is a metal compound other than TiO 2 , Fe 2 O 3 and Al 2 O 3. It is preferable to contain a compound.
- SiO 2 converted content Sum of content of silicon compound converted to SiO 2 (hereinafter sometimes referred to as “SiO 2 converted content”) and content of calcium compound converted to CaO (hereinafter also referred to as “CaO converted content”)
- the amount is preferably 2% by mass or less, and more preferably 0.5 to 2% by mass.
- Silicon compounds and calcium compounds act as grain growth agents, and when they are present in an amount of 2% by mass or less in terms of oxide, the shape and size of the corundum crystals of alumina are considered to be non-uniform and cause crack deflection. It is done. In other words, due to the presence of specific amounts of titanium and iron compounds, and specific amounts of silicon and calcium compounds, the respective actions combine to effectively generate crack deflection, resulting in higher fracture toughness effects. Conceivable.
- the content of alumina, TiO 2 equivalent content, Fe 2 O 3 equivalent content, SiO 2 equivalent content, CaO equivalent content, metal oxide equivalent content of other metal compounds are fluorescent X-rays It can be determined by elemental analysis. Specifically, it is obtained as follows. First, in order to perform the measurement, a wet analysis of a standard oxide sample having a known element composition is performed. A calibration curve necessary for measurement is created using the obtained wet analysis value as a reference value. The sample is quantitatively analyzed based on the created calibration curve. As a measuring instrument, “PW2400 type” manufactured by Panallytical can be used. The measurement is preferably carried out under the conditions of tube: rhodium tube, characteristic X-ray: K ⁇ ray.
- the tube voltage and tube current are preferably measured under different conditions for each element.
- An example of tube voltage and tube current conditions is shown in Table 1 below.
- requiring each metal oxide conversion content becomes the quantity which converted and totaled all the metal elements contained in an alumina sintered body.
- alumina sintered body [Production method of alumina sintered body] Next, the manufacturing method of the alumina sintered body of the present invention described above will be described.
- material In the method for producing an alumina sintered body of the present invention, alumina, a titanium compound, and an iron compound are used as raw materials. If necessary, a silicon compound and / or a calcium compound is further used. These may be composite oxides containing two or more.
- the cumulative mass 50% diameter (d 50 ) of alumina powder, titanium compound powder, iron compound powder, silicon compound powder, and calcium compound powder is 3 ⁇ m or less in order to obtain a homogeneous mixed powder. It is preferable that it is 1 ⁇ m or less.
- the cumulative mass 50% diameter (d 50 ) of various powders can be measured by a laser diffraction method.
- the alumina powder is a raw material for forming a main crystal phase composed of corundum crystals in the obtained alumina sintered body, it is preferably a high-purity one.
- alumina formed by the Bayer method is used. Is preferred.
- the titanium compound powder and the iron compound powder may be high-purity TiO 2 powder and high-purity Fe 2 O 3 powder, respectively, or all of titanium, iron, and alumina, or two of them may be complex oxidation.
- An object may be formed.
- the composite oxide include ilmenite (titanite: FeTiO 3 ) powder, aluminum titanate powder, FeTiAlO 5 powder, and the like. Since ilmenite powder is less expensive than high-purity TiO 2 powder and high-purity Fe 2 O 3 powder, the production cost of abrasive grains can be reduced. Therefore, it is preferable to use ilmenite powder.
- ilmenite is also called titanium iron ore, which is a naturally occurring iron and titanium oxide mineral and has a composition represented by FeTiO 3 .
- the production areas are Australia, Norway, Russian Urals, India, Canada, USA, Malaysia, etc., and the chemical composition differs depending on the production area.
- part of Fe 2+ is replaced with Mg 2+ .
- Table 2 shows the respective chemical compositions of the alumina component and the iron compound, titanium compound, silicon compound, and calcium compound converted into oxides among the components constituting ilmenite (from Queensland, Australia).
- the mass mixing ratio of ilmenite powder to alumina powder is preferably 0.05: 0.95 to 0.16: 0.84, and 0.08: 0 .92 to 0.12: 0.88 is more preferable.
- the mass mixing ratio is preferably 0.05: 0.95 to 0.16: 0.84, the total amount of the two components of the TiO 2 equivalent content and the Fe 2 O 3 equivalent content is 5 to 13 mass%. can do.
- the total content of the silicon compound in terms of SiO 2 and the content of the calcium compound in terms of CaO is 2% by mass or less, preferably 0.5 to 2% by mass.
- the silicon compound powder and calcium compound powder may be high-purity SiO 2 powder, high-purity CaO powder, calcium carbonate powder, etc., or all of silica, calcium oxide, and alumina, or two of them. May form a complex oxide.
- the composite oxide include powders such as mullite, zeolite, bentonite, gehlenite, and anorthite.
- the method for preparing the mixture of raw materials is not particularly limited, but for example, the following method can be preferably employed.
- predetermined amounts of alumina powder and ilmenite powder (or TiO 2 powder and Fe 2 O 3 powder) obtained by the Bayer method are respectively added to an aqueous medium containing polyvinyl alcohol.
- a homogenous slurry using a disperser using a medium such as an ultrasonic disperser, a planetary ball mill, a ball mill, or a sand mill, or a medialess disperser such as an optimizer (trade name) or a nanomizer (trade name).
- this slurry is dried and then pulverized to prepare a mixture (powder) having a cumulative mass 50% diameter (d 50 ) of 3 ⁇ m or less, preferably 1 ⁇ m or less.
- the molded body of the mixture of raw materials prepared as described above is sintered to obtain the alumina sintered body of the present invention having a relative density of 95% or more, preferably 97% or more.
- the relative density can be obtained by dividing the sintered bulk density measured by the Archimedes method by the true density.
- a known molding means such as a die press, cold isostatic pressing, cast molding, injection molding, extrusion molding, or the like is formed into an arbitrary shape.
- the sintering is performed by various sintering methods such as a hot press method, a normal pressure firing method, a gas pressure firing method, and a microwave heating firing method.
- the alumina sintered body of the present invention thus obtained has high hardness and excellent fracture toughness, for example, grinding, cutting, polishing tools such as abrasives, cutting materials, abrasives, etc., Furthermore, it is suitable as abrasive grains for heavy grinding wheels in the steel industry.
- the abrasive grain of the present invention comprises the alumina sintered body of the present invention.
- the alumina sintered body of the present invention can be obtained by sequentially performing a pulverization process, a kneading process, a forming process, a drying process, and a sintering process.
- the grindstone of the present invention has the layer of the abrasive grains of the present invention on the working surface.
- the method for fixing the abrasive grains to the working surface in the grindstone of the present invention include resin bond, vitrified bond, metal bond, and electrodeposition.
- the base metal material include steel, stainless steel alloy, and aluminum alloy.
- Resin bonds have good sharpness but low durability. Vitrified bonds have good sharpness and good wear resistance, but internal stress is generated in the abrasive grains, and the abrasive grains tend to crack or chip. Electrodeposition has a large degree of freedom in shape and good sharpness. In view of the above, in the grindstone, a method for fixing the abrasive grains is selected according to the application.
- a resin bond grindstone powder of a binder such as phenol resin or polyimide resin and abrasive grains are mixed, or the binder is coated on the abrasive grains, filled in a mold and press-molded.
- the method of the present invention wherein the abrasive layer is fixed to the working surface of the base metal by mixing the abrasive particles with a liquid binder such as epoxy resin or unsaturated polyester resin, and pouring into a mold and curing.
- a grindstone is obtained.
- K IC 0.026 * E1 / 2 * P1 / 2 * a / c3 / 2 K IC : Fracture toughness value (MPa ⁇ m 1/2 )
- E Young's modulus (Pa)
- N Maximum load
- a Indentation dimension
- c Crack size (m)
- the Young's modulus E is an alumina value (3.9 ⁇ 10 11 Pa).
- composition analysis of metal oxide crystal phase containing Ti, Fe and Al of alumina-based sintered body Using “X'pert PRO” manufactured by Panallytical as a device, characteristic X-ray: CuK ⁇ ray, tube voltage
- the composition analysis of the metal oxide crystal phase was performed under the conditions of 40 kV and tube current of 40 mA.
- examples of the form of the raw material of the sintered body include powder, metal powder, slurry, and aqueous solution.
- a powder raw material it was considered preferable to use a powder raw material from the viewpoint of ease of handling during work, and the powder raw material was used.
- the chemical composition of alumina powder, ilmenite powder, iron oxide powder and titanium oxide powder used as raw materials (alumina content, TiO 2 equivalent content, Fe 2 O 3 equivalent content, SiO 2 equivalent content, CaO
- the converted content is shown in Tables 3 to 6 below.
- the alumina powder is “AL-160SG-3” manufactured by Showa Denko KK, and its cumulative mass 50% diameter (d 50 ) is 0.6 ⁇ m.
- the above-mentioned ilmenite powder was produced in Australia, and was manufactured by CRL (Consolidated Rutile Limited) of Australia and pulverized to a cumulative mass of 50% diameter (d 50 ): 0.75 ⁇ m.
- the iron oxide powder is Benegara SR-570 manufactured by Tone Sangyo Co., Ltd., and its cumulative mass 50% diameter (d 50 ) is 0.5 ⁇ m.
- the titanium oxide powder is “Super Titania (registered trademark) G series” manufactured by Showa Titanium Co., Ltd., and its cumulative mass 50% diameter (d 50 ) is 0.6 ⁇ m.
- Examples 1 to 5 and Comparative Examples 1 to 7 The alumina powder having a cumulative mass of 50% diameter (d 50 ) of 0.6 ⁇ m and the ilmenite powder having a cumulative mass of 50% diameter (d 50 ) of 0.75 ⁇ m are mixed with TiO 2 in the formed alumina sintered body and Various mixtures were obtained by mixing so that each content of Fe 2 O 3 was a value shown in Table 7.
- the various slurries were each dried at 120 ° C. for 24 hours, and then pulverized with a mortar to obtain various pulverized products having a cumulative mass 50% diameter (d 50 ) of 300 ⁇ m or less.
- the various pulverized products were each molded with a pressure of 100 MPa and then subjected to a hydrostatic pressure treatment with a pressure of 150 MPa to prepare various molded products.
- Example 6 and 7 and Comparative Examples 8 and 9 Alumina powder with cumulative mass 50% diameter (d 50 ) 0.6 ⁇ m, iron oxide powder with cumulative mass 50% diameter (d 50 ) 0.5 ⁇ m, and oxidation with cumulative mass 50% diameter (d 50 ) 0.6 ⁇ m Titanium powder was mixed so that the contents of TiO 2 and Fe 2 O 3 in the formed alumina sintered body would be the values shown in Table 7, and various mixtures were obtained.
- the metal oxide crystal phase containing Ti, Fe and Al present at the grain boundaries of the main crystal phase composed of corundum crystals is FeTiAlO 5.
- the crystal phase was confirmed by X-ray diffraction measurement.
- Example 4 the result of the X-ray diffraction measurement of the alumina sintered body of Example 4 is shown in FIG.
- Data analysis of the X-ray diffraction measurement was performed using analysis software “X'Pert High Score Plus” manufactured by PANalytical.
- analysis software “X'Pert High Score Plus” manufactured by PANalytical.
- the structure of FeAlTiO 5 was determined based on the literature published by Tiedemann et al. The pattern obtained thereby was compared with the result of the experimental sample, and it was determined that the peak was due to FeAlTiO 5 .
- FeAlTiO 5 particle 12 FeAlTiO 5 particle 12: Alumina particle X: Arrow indicating the progress direction of crack Y: Arrow indicating the progress direction of crack
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Abstract
Description
研削比=被削材が削られた量(研削量)/砥石の摩耗量
(1)砥粒の硬度が高くなると研削量が増えるため研削比は大きくなる。
(2)破壊靱性が高くなると砥粒の摩耗量が少なくなるため研削比は大きくなる。
[1] チタン化合物及び鉄化合物を含むアルミナ質焼結体であって、チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量とアルミナの含有量との合計量が98質量%以上であり、チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量との合計量が5~13質量%であり、チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量との質量比(TiO2:Fe2O3)が、0.85:1.15~1.15:0.85であるアルミナ質焼結体。
[2] チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量との合計量が7~10質量%である上記[1]に記載のアルミナ質焼結体。
[3] 上記[1]又は[2]に記載のアルミナ質焼結体からなる砥粒。
[4] 上記[3]に記載の砥粒の層を作用面に有する砥石。
本発明のアルミナ質焼結体は、チタン化合物及び鉄化合物を含み、チタン化合物をTiO2換算した含有量(以下、「TiO2換算含有量」ということがある)と鉄化合物をFe2O3換算した含有量(以下、「Fe2O3換算含有量」ということがある)とアルミナの含有量との3成分合計量が98質量%以上となっている。
また、TiO2換算含有量とFe2O3換算含有量との2成分合計量は5~13質量%となっており、7~10質量%となっていることが好ましい。
上記比(TiO2:Fe2O3)は、0.90:1.10~1.10:0.90であることが好ましく、0.95:1.05~1.05:0.95であることがより好ましい。
まず、アルミナだけからなる焼結体の場合は、図3に示すように、クラックの伝わり方は、アルミナ粒子12の粒界に沿って矢印Y方向に進行することになる。そして、衝撃の大きさによっては、図4(B)のSEM写真に示すように、粒界に沿って直線的に亀裂が生じることになる。なお、図4は、後述の比較例1に係る焼結体のSEM写真であり、図4(A)は衝撃を加える前の結晶組織の様子を示し、図4(B)は衝撃を加えた後のクラック伝播の様子を示す。
このことは、図2に示す衝撃試験の結果を示すSEM写真からもわかる。すなわち、図2(A)のSEM写真のようにアルミナ粒子の粒界にFeTiAlO5粒子が存在する状態で衝撃を加えると、図2(B)のようにクラックはFeTiAlO5粒子を起点にこれを迂回するように進行する。
なお、図2は後述の実施例3に係る焼結体のSEM写真であり、当該図中、アルミナ粒子の粒界にある三重点に位置する灰色部分(色の薄い部分)がFeTiAlO5粒子に相当する。
ケイ素化合物をSiO2換算した含有量(以下、「SiO2換算含有量」ということがある)とカルシウム化合物をCaO換算した含有量(以下、「CaO換算含有量」ということがある)との合計量は2質量%以下となっていることが好ましく、0.5~2質量%となっていることがより好ましい。
ケイ素化合物及びカルシウム化合物は粒成長剤として作用し、これらが酸化物換算で2質量%以下存在することで、アルミナのコランダム結晶の形状・サイズを不均一にし、クラックの偏向を生じさせるものと考えられる。つまり、特定量のチタン化合物及び鉄化合物、及び特定量のケイ素化合物及びカルシウム化合物の存在により、それぞれの作用が組み合わさってクラックの偏向が効率よく生じ、より高い破壊靭性化の効果が得られると考えられる。
まず測定を行うために、元素の組成が既知の標準酸化物試料の湿式分析を行う。得られた湿式分析値を基準値として、測定の際に必要な検量線を作成する。サンプルの定量分析は、この作成した検量線を基に行う。測定機器としては、Panalytical社製、「PW2400型」を用いることができる。また測定は、管球:ロジウム管球、特性X線:Kα線の条件で実施することが好ましい。管電圧及び管電流は元素ごとに異なる条件で測定を行うことが好ましい。管電圧と管電流の条件の一例を下記表1に示す。
なお、本明細書において、各金属酸化物換算含有量を求める際の分母となる全体量は、アルミナ質焼結体に含まれる全ての金属元素を酸化物に換算して合計した量となる。
次に、既述の本発明のアルミナ質焼結体の製造方法について説明する。
(原料)
本発明のアルミナ質焼結体の製造方法においては、原料としてアルミナ、チタン化合物、鉄化合物を用いる。必要に応じてさらにケイ素化合物及び/又はカルシウム化合物を用いる。これらは2種以上を含む複合酸化物でもよい。
ここで、各種粉末の累積質量50%径(d50)は、レーザー回折法により測定することができる。
ケイ素化合物粉末、カルシウム化合物粉末としては、それぞれ高純度のSiO2粉末及び高純度のCaO粉末、炭酸カルシウム粉末等であってもよいし、シリカ、酸化カルシウム、アルミナの全部あるいはそれらの中の2種が複合酸化物を形成したものであってもよい。複合酸化物としては、ムライト、ゼオライト、ベントナイト、ゲーレナイト、アノーサイト等の粉末が挙げられる。
本発明のアルミナ質焼結体を製造する方法において、原料の混合物を調製する方法に特に制限はないが、例えば下記の方法を好ましく採用することができる。
まず、ポリビニルアルコールを含む水性媒体中に、バイヤー法で得られたアルミナ粉末、イルメナイト粉末(又はTiO2粉末とFe2O3粉末)を、それぞれ所定量を加える。その後、例えば、超音波分散機、遊星ボールミル、ボールミル、サンドミル等のメディアを用いた分散機、アルティマイザー(商品名)、ナノマイザー(商品名)等のメディアレス分散機等を用いて均質なスラリーを得る。次いで、このスラリーを乾燥処理したのち、粉砕して、累積質量50%径(d50)3μm以下、好ましくは1μm以下の混合物(粉末)を調製する。
上記のようにして調製された原料の混合物の成形体を焼結して、相対密度95%以上、好ましくは97%以上である本発明のアルミナ質焼結体を得る。相対密度が95%以上であることで、焼結体中の気孔・空隙に起因する焼結体硬度および破壊靭性の低下を抑制することができる。なお、相対密度はアルキメデス法で測定した焼結嵩密度を真密度で除して求めることができる。
また、焼結に際しては、公知の成形手段、例えば金型プレス、冷間静水圧プレス、鋳込成形、射出成形、押出し成形等により任意の形状に成形し、次いでこの成形体を公知の焼結法、例えば、ホットプレス法、常圧焼成法、ガス加圧焼成法、マイクロ波加熱焼成法等、種々の焼結手法によって焼結する。
本発明の砥粒は、本発明のアルミナ質焼結体からなる。本発明のアルミナ質焼結体は、粉砕処理、混練処理、成形処理、乾燥処理、焼結処理を順次施すことで得られる。
本発明の砥石は、本発明の砥粒の層を作用面に有するものである。
本発明の砥石における砥粒の作用面への固定方法としては、レジンボンド、ビトリファイドボンド、メタルボンド、電着等が挙げられる。
また、台金の材質としては、スチール、ステンレス合金、アルミニウム合金等が挙げられる。
以上に鑑み、砥石においては、その用途に応じて砥粒の固定方法が選択される。
本発明の砥石の形状については特に制限はなく、砥石の用途に応じて、ストレート型やカップ型等の形状から適宜選択すればよい。
なお、各例における諸特性は以下に示す方法に従って求めた。
原料粉末の累積質量50%径(d50)は、レーザー回折法(日機装(株)製マイクロトラック HRA)により測定した。
装置として(株)アカシ製、機種名「MVK-VL、Hardness Tester」を用い、測定は、荷重0.98N、圧子の打ち込み時間10秒の条件とし、15点の測定値の平均値を平均ビッカース硬度とした。平均ビッカース硬度が16GPa以上であれば実用上問題ない。
装置として松沢精機(株)製、機種名「DVK-1」を用い、測定は、最大荷重9.81N、圧子の打ち込み速度50μm/sec、圧子の打ち込み時間15秒の条件にて15点の平均値を平均破壊靱性値とした。計算式は以下の通りである。また、平均破壊靱性値が3.0MPa・m1/2以上であれば実用上問題ない。
KIC = 0.026 * E1/2 * P1/2 * a / c3/2
KIC : 破壊靱性値(MPa・m1/2)
E : ヤング率(Pa)
P : 最大荷重(N)
a : 圧痕寸法(m)
c : クラックの寸法(m)
なお、本発明において上記ヤング率Eは、アルミナの値(3.9×1011Pa)を用いた。
装置として日本電子(株)製、機種名「JSM-6510V」を用いてSEM写真を撮影した。得られたSEM写真から各結晶相の平均結晶サイズを測定した。平均結晶サイズは、各結晶(50個)の同一方向における最大長さを直径法により測定し、平均を算出して求めた。
装置としてPanalytical社製、機種名「X'pert PRO」を用い、特性X線:CuKα線、管電圧40kV、管電流40mAの条件にて上記金属酸化物結晶相の組成分析を行った。
相対密度はアルキメデス法で測定した各焼結体の嵩密度を真密度で除して求めた。
この際、添加した鉄化合物とチタン化合物とは全て反応してFeTiAlO5になったと仮定し、その上で、アルミナの真密度を3.98、FeTiAlO5の真密度を4.28とし、生成され得るFeTiAlO5の割合と残部であるアルミナの割合をもとに真密度を算出した。
累積質量50%径(d50)0.6μmの上記アルミナ粉末と、累積質量50%径(d50)0.75μmの上記イルメナイト粉末とを、形成されるアルミナ質焼結体中のTiO2及びFe2O3の各含有量が表7に示す値となるように混合して各種混合物を得た。
また、図2に実施例3のアルミナ質焼結体に対する衝撃試験前後のSEM写真を、図4に、比較例1のアルミナ質焼結体に対する衝撃試験前後のSEM写真を示す。なお、これらの図中、(A)は衝撃試験前の結晶組織の様子を示し、(B)は衝撃試験後のクラック伝播の様子を示す。
累積質量50%径(d50)0.6μmの上記アルミナ粉末と、累積質量50%径(d50)0.5μmの酸化鉄粉末、及び累積質量50%径(d50)0.6μmの酸化チタン粉末を、形成されるアルミナ質焼結体中のTiO2及びFe2O3の各含有量が表7に示す値となるように混合して各種混合物を得た。
次いで、この各種スラリーを、それぞれ120℃で24時間乾燥処理した後、乳鉢により解砕処理して、累積質量50%径(d50)300μm以下の各種粉砕品を得た。この各種粉砕品を、それぞれ100MPaの圧力で金型成形したのち、さらに150MPaの圧力で静水圧処理を施して各種成形体を作製した。
次に、この各種成形体を相対密度が95%以上になるように、電気炉(大気雰囲気)にて4時間焼成することにより各種のアルミナ質焼結体を得た。これらについて、既述のような試験(評価)を行った。結果を下記表7に示す。
X線回折測定のデータ解析は、PANalytical社製の解析ソフト「X’Pert High Score Plus」を用いて行った。
この解析ソフトでは、FeAlTiO5の構造を、1982年にTiedemann等が発表した文献を基に結晶構造を決定した。
それによって得られたパターンと、実験サンプルの結果を照合して、ピークがFeAlTiO5に起因するものであると判断した。
12:アルミナ粒子
X :クラックの進行方向を示す矢印
Y :クラックの進行方向を示す矢印
Claims (4)
- チタン化合物及び鉄化合物を含むアルミナ質焼結体であって、
チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量とアルミナの含有量との合計量が98質量%以上であり、
チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量との合計量が5~13質量%であり、
チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量との質量比(TiO2:Fe2O3)が、0.85:1.15~1.15:0.85であるアルミナ質焼結体。 - チタン化合物をTiO2換算した含有量と鉄化合物をFe2O3換算した含有量との合計量が7~10質量%である請求項1に記載のアルミナ質焼結体。
- 請求項1に記載のアルミナ質焼結体からなる砥粒。
- 請求項3に記載の砥粒の層を作用面に有する砥石。
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JP2016539889A (ja) * | 2013-10-04 | 2016-12-22 | センター フォア アブラシブズ アンド リフラクトリーズ リサーチ アンド ディベロップメント ツェー アー エァ エァ デー ゲゼルシャフト ミット ベシュレンクテル ハフツング | 増大した靭性を備えた溶融酸化アルミニウムをベースとする、多結晶質の多孔性Al2O3物体およびその使用 |
JP2019527288A (ja) * | 2016-06-22 | 2019-09-26 | イメルテック ソシエテ パル アクシオン サンプリフィエ | ボーキサイト中に存在する酸化物を主成分とした焼結研磨粒子 |
JP2020180020A (ja) * | 2019-04-25 | 2020-11-05 | 京セラ株式会社 | 黒色セラミックス |
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JP4989792B2 (ja) * | 2010-11-01 | 2012-08-01 | 昭和電工株式会社 | アルミナ質焼結体の製造方法、アルミナ質焼結体、砥粒、及び砥石 |
EP3053898B1 (en) | 2015-02-06 | 2018-09-26 | Center for Abrasives and Refractories Research & Development C.A.R.R.D. GmbH | Sintered shaped abrasive grains on basis of aluminum oxide comprising mineralogical phases consisting of mullite, tialite and/or armalcolite, and baddeleyite and/or srilankite and a method for their production |
DE102016100196A1 (de) | 2015-02-06 | 2016-08-11 | Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh | Geformte Sinterschleifkörner auf Basis von Aluminiumoxid mit Anteilen an mineralogischen Phasen bestehend aus Mullit, Tialit und/oder Armalcolit und Baddeleyit und/oder Srilankit sowie ein Verfahren zu ihrer Herstellung |
JP6722518B2 (ja) * | 2016-06-09 | 2020-07-15 | 新光電気工業株式会社 | 焼結体及びその製造方法と静電チャック |
CN114180980B (zh) * | 2021-12-28 | 2023-06-23 | 德阳三环科技有限公司 | 一种自增韧99氧化铝陶瓷基板及其制备方法 |
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KR101316665B1 (ko) | 2013-10-10 |
SI2636655T1 (sl) | 2016-11-30 |
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JPWO2012060211A1 (ja) | 2014-05-12 |
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US8894730B2 (en) | 2014-11-25 |
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