JP4503541B2 - Silicon nitride powder and use thereof - Google Patents
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- JP4503541B2 JP4503541B2 JP2006039341A JP2006039341A JP4503541B2 JP 4503541 B2 JP4503541 B2 JP 4503541B2 JP 2006039341 A JP2006039341 A JP 2006039341A JP 2006039341 A JP2006039341 A JP 2006039341A JP 4503541 B2 JP4503541 B2 JP 4503541B2
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims description 46
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 46
- 239000000843 powder Substances 0.000 title claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 230000001186 cumulative effect Effects 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 238000000790 scattering method Methods 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 description 10
- 230000007797 corrosion Effects 0.000 description 10
- 238000011049 filling Methods 0.000 description 8
- 238000000465 moulding Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は窒化珪素粉末及びその用途に関する。 The present invention relates to silicon nitride powder and uses thereof.
窒化珪素粉末は、その耐摩耗、高強度、低熱膨張等の優れた性質を利用し、樹脂充填材やエンジニアリングセラミックス焼結体の製造原料等に使用されている。近年、非鉄金属の溶湯用部材、特にアルミニウム又はアルミニウム合金の溶湯用部材の需要が伸びており、具体的には熱電対の保護管、ラドル、湯面検知棒、ロール、タイル等の耐摩耗材料、軸受、バルブ等の産業機械部品である。 Silicon nitride powder is used as a raw material for producing resin fillers and engineering ceramics sintered bodies because of its excellent properties such as wear resistance, high strength, and low thermal expansion. In recent years, there has been an increasing demand for non-ferrous metal melt members, particularly aluminum or aluminum alloy melt members. Specifically, wear-resistant materials such as thermocouple protection tubes, ladles, hot water level detection rods, rolls and tiles. Industrial machinery parts such as bearings and valves.
非鉄金属溶湯用部材への要求特性は、高温強度と耐食性がいずれも高いことである。これを解決するため、従来、数多くの技術改良（特許文献１）がなされているが、まだまだ改善の余地があった。
本発明の目的は、高温強度と耐食性がいずれも高い窒化珪素焼結体、それを用いた非鉄金属溶湯用部材、及びそれを製造するための窒化珪素粉末を提供することである。本発明の目的は、窒化珪素粉末の粒度特性と、エタノール吸液量で示される窒化珪素粉末の充填性とを最適化した窒化珪素粉末を提供することによって達成することができる。なお、本明細書において、「高温強度」とは８００℃における４点曲げ強さであり、「耐食性」とは７５０℃の溶融アルミニウムに試験片を２４時間浸漬したときの侵食深さのことであり、「窒化珪素粉末の充填性」とは焼結前の窒化珪素粉末成形体の密度のことである。 An object of the present invention is to provide a silicon nitride sintered body having high high-temperature strength and high corrosion resistance, a nonferrous metal molten member using the same, and a silicon nitride powder for producing the same. The object of the present invention can be achieved by providing a silicon nitride powder in which the particle size characteristics of the silicon nitride powder and the filling property of the silicon nitride powder indicated by the ethanol absorption amount are optimized. In this specification, “high temperature strength” is the 4-point bending strength at 800 ° C., and “corrosion resistance” is the erosion depth when the test piece is immersed in molten aluminum at 750 ° C. for 24 hours. “Fillability of silicon nitride powder” means the density of the silicon nitride powder compact before sintering.
本発明は、ｄ５０が１．１５〜１．２７μｍ、ｄ７５／ｄ２５が４．５〜５．６であり、エタノール吸液量が粉末５ｇ当たり２．１２〜２．１８ｍｌである窒化珪素粉末。ここで、ｄ５０とはレーザー回折散乱法で測定された粒度分布における累積５０体積％径、ｄ７５とは累積７５体積％径、ｄ２５とは累積２５体積％径のことである。また、本発明は、本発明の窒化珪素粉末の焼結体からなる窒化珪素焼結体である。さらに、本発明は、本発明の窒化珪素焼結体で構成された非鉄金属の溶湯用部材であり、好ましくはアルミニウム又はアルミニウム合金溶湯用部材である。 The present invention provides a silicon nitride powder having a d50 of 1.15 to 1.27 μm, a d75 / d25 of 4.5 to 5.6 , and an ethanol absorption of 2.12 to 2.18 ml per 5 g of powder. . Here, d50 is a cumulative 50 volume% diameter in the particle size distribution measured by the laser diffraction scattering method, d75 is a cumulative 75 volume% diameter, and d25 is a cumulative 25 volume% diameter. Moreover, this invention is a silicon nitride sintered compact which consists of a sintered compact of the silicon nitride powder of this invention. Furthermore, the present invention is a non-ferrous metal melt member composed of the silicon nitride sintered body of the present invention, preferably an aluminum or aluminum alloy melt member.
本発明によれば、例えばアルミニウム、マグネシウム、ニッケル等の非鉄金属の溶湯用部品を製造するのに好適な、高温強度と耐食性がいずれも高い窒化珪素焼結体が提供される。 ADVANTAGE OF THE INVENTION According to this invention, the silicon nitride sintered compact with high high temperature intensity | strength and corrosion resistance both suitable for manufacturing the components for molten metal of nonferrous metals, such as aluminum, magnesium, nickel, is provided.
本発明の窒化珪素粉末のｄ５０は０．９〜１．５μｍ、好ましくは、１．１〜１．３μｍである。ｄ５０が０．９μｍ未満であると、ｄ２５も小さくなるのでｄ７５／ｄ２５の条件を満たさせることが困難となる。その結果、窒化珪素粉末の充填性を十分に高めることができなくなり、高温強度と耐食性がいずれも顕著に向上しない。一方、ｄ５０が１．５μｍをこえると、粗粉になりすぎてこれまた高温強度と耐食性が顕著に向上しない。 The d50 of the silicon nitride powder of the present invention is 0.9 to 1.5 μm, preferably 1.1 to 1.3 μm. If d50 is less than 0.9 μm, d25 also becomes small, so it is difficult to satisfy the condition of d75 / d25. As a result, the filling property of the silicon nitride powder cannot be sufficiently increased, and neither the high temperature strength nor the corrosion resistance is remarkably improved. On the other hand, if d50 exceeds 1.5 μm, it becomes too coarse and the high temperature strength and corrosion resistance are not significantly improved.
窒化珪素粉末のｄ７５／ｄ２５は３〜８、好ましくは４〜６である。ｄ７５／ｄ２５が３未満であると、粒度分布がシャープになりすぎて窒化珪素粉末の充填性が高まらず、またこの比が８をこえると、逆に粒度分布がブロードになりすぎて粗粉が増え、これまた窒化珪素粉末の充填性が高まらない。これらの結果、窒化珪素焼結体の焼結密度が大きくならず、高温強度と耐食性が顕著に向上しない。普通に入手できる市販品等の窒化珪素粉末のｄ７５／ｄ２５は、２未満又は１３以上であるので、本発明に係る３〜８は特異的である。 D75 / d25 of the silicon nitride powder is 3 to 8, preferably 4 to 6. If d75 / d25 is less than 3, the particle size distribution becomes too sharp and the filling property of the silicon nitride powder does not increase. On the other hand, if this ratio exceeds 8, the particle size distribution becomes too broad and coarse powder is formed. This also increases the filling ability of the silicon nitride powder. As a result, the sintered density of the silicon nitride sintered body is not increased, and the high temperature strength and corrosion resistance are not significantly improved. Since d75 / d25 of commercially available silicon nitride powder such as commercially available products is less than 2 or 13 or more, 3 to 8 according to the present invention is specific.
窒化珪素粉末の粒度の調整は、例えば金属珪素の直接窒化法で製造した窒化インゴットを粗砕、中砕、粉砕した後、気流分級して窒化珪素粉末を製造する際、分級条件を制御することによって行うことができる。具体的には、一次エアー量やガイドベーン、ルーバー等の自由渦の制御、二次エアー風量等による半自由渦の制御、更にはローター等の回転数による強制渦の制御等によって行うことができる。これらの操作方法は当業者に熟知されている。 For adjusting the particle size of the silicon nitride powder, for example, after pulverizing, intermediately pulverizing, and pulverizing a nitride ingot produced by the direct nitridation method of metal silicon, the classification conditions are controlled when the silicon nitride powder is produced by air classification. Can be done by. Specifically, it can be performed by controlling the free vortex of the primary air amount, guide vanes, louvers, etc., controlling the semi-free vortex by the secondary air flow rate, etc., and controlling the forced vortex by the rotational speed of the rotor, etc. . These methods of operation are well known to those skilled in the art.
粒度の測定は、レーザー回折散乱法による粒度分布測定機（例えばＬＥＥＤＳ＆ＮＯＲＴＨＲＵＰ社製商品名「ＭＩＣＲＯＴＲＡＣ−ＩＩ ＳＰＡ：ＭＯＤＥＬ７９７７−２０」）によって行うことができる。測定は試料粉末６０ｍｇをヘキサメタリン酸ナトリウム０．２質量％水溶液２００ｇに１０分間超音波分散させてから行う。 The particle size can be measured by a particle size distribution measuring instrument (for example, trade name “MICROTRAC-II SPA: MODEL 7777-20” manufactured by LEEDS & NORTH SUP) by a laser diffraction scattering method. The measurement is performed after ultrasonically dispersing 60 mg of the sample powder in 200 g of a 0.2 mass% aqueous solution of sodium hexametaphosphate for 10 minutes.
本発明の窒化珪素粉末は、エタノール吸液量が粉末５ｇ当たり２．０〜２．３ｍｌ、好ましくは２．１〜２．２ｍlである。普通に入手できる市販品等の窒化珪素粉末のエタノール吸液量が１．９ｍl未満又は４ｍl以上であることを踏まえると、数値範囲が厳選されていることが特徴である。エタノール吸液量は窒化珪素粉末の充填性の良否を示す指標であり、粒子同士の隙間が多くなるほど（すなわち最密充填に近くなるほど）小さくなるが、いくら小さくても良いということではなく、窒化珪素粉末の充填性を最大化させる下限値がある。一方、上記粒度範囲にあっては、平均粒子径が大きいほどエタノール吸液量は大きくなる。これらの事実を突き止め、更なる検討を加えて、エタノール吸液量が上記のように特定された。エタノール吸液量が粉末５ｇ当たり２．０ｍl未満であると、窒化珪素粉末の充填性の著しい向上はなく、また２．３ｍｌをこえると、粒子同士の隙間が大きすぎるため、これまた窒化珪素粉末の充填性の著しい向上はない。エタノール吸液量の増減は、上記粒度範囲において、ｄ５０を０．９〜１．５μｍの範囲内で制御することによって行うことができる。 The silicon nitride powder of the present invention has an ethanol absorption of 2.0 to 2.3 ml, preferably 2.1 to 2.2 ml per 5 g of powder. In view of the fact that the amount of ethanol absorption of commercially available silicon nitride powder such as commercially available products is less than 1.9 ml or 4 ml or more, the numerical range is carefully selected. The amount of ethanol absorbed is an index indicating the quality of filling of silicon nitride powder, and the smaller the gap between particles (that is, the closer to the closest packing), the smaller the amount, but this does not mean that it can be as small as possible. There is a lower limit that maximizes the fillability of the silicon powder. On the other hand, in the above particle size range, the ethanol absorption becomes larger as the average particle size is larger. Ascertaining these facts and further studies, the ethanol absorption was determined as described above. If the amount of ethanol absorbed is less than 2.0 ml per 5 g of powder, there is no significant improvement in the filling properties of the silicon nitride powder, and if it exceeds 2.3 ml, the gap between particles is too large. There is no significant improvement in the filling property. The ethanol absorption can be increased or decreased by controlling d50 within the range of 0.9 to 1.5 μm in the above particle size range.
エタノール吸液量の測定は、試料５ｇを秤量して１００ｍｌビーカーに入れ、ビュレットから約０．０２ｍｌずつエタノールを滴下しガラス棒で混合する、この滴下・混合を繰り返して行い、試料の全量がガラス棒にまとわりついたエタノール量を測定することによって行った。 The ethanol absorption is measured by weighing 5 g of a sample into a 100 ml beaker, dropping 0.02 ml of ethanol from the burette and mixing with a glass rod. This dripping / mixing is repeated until the total amount of the sample is glass. This was done by measuring the amount of ethanol clinging to the rod.
本発明の窒化珪素焼結体は、本発明の窒化珪素粉末を含む原料を、常圧焼結又はホットプレス焼結することによって製造することができる。すなわち、本発明の窒化珪素粉末をそのまま、又は例えばＹ２Ｏ３、Ａｌ２Ｏ３、ＭｇＯ等の希土類元素、３ａ族元素等の酸化物からなる焼結助剤を混合し、例えばプレス成形、射出成形、押出成形、鋳込み成形等によって成形した後、例えば窒素、アルゴン等の非酸化性雰囲気下、例えば温度１６５０〜１８００℃、４〜１２時間焼成することによって製造することができる。 The silicon nitride sintered body of the present invention can be produced by subjecting a raw material containing the silicon nitride powder of the present invention to atmospheric pressure sintering or hot press sintering. That is, the silicon nitride powder of the present invention is used as it is or mixed with a sintering aid made of oxides of rare earth elements such as Y 2 O 3 , Al 2 O 3 , MgO, and group 3a elements, for example, press molding, After molding by injection molding, extrusion molding, casting molding, or the like, it can be produced by firing at a temperature of 1650 to 1800 ° C. for 4 to 12 hours, for example, in a non-oxidizing atmosphere such as nitrogen or argon.
本発明の窒化珪素焼結体は、高温強度が８００ＭＰａ以上で、耐食性はほとんど侵食せずであるので非金属溶湯部材に適しており、特にこれらの特性が高度に要求されるアルミニウム又はアルミニウム合金の溶湯部材に最適となる。 Since the silicon nitride sintered body of the present invention has a high-temperature strength of 800 MPa or more and hardly erodes corrosion resistance, it is suitable for a non-metallic molten metal member. Optimal for molten metal parts.
実施例２〜４ 比較例１〜４ 参考例１〜２
金属珪素粉末の直接窒化法（例えば特開平２−４４０１７号公報の実施例１参照）にてα
率９０％以上の窒化珪素インゴットを製造した後、それをジョークラッシャーにて粗砕、
更にチューブミルと振動ミルで中砕・微粉砕した後、気流式分級機で分級し、表１に示さ
れる窒化珪素粉末を製造した。窒化珪素粉末の粒度調整は、振動ミルのフィード量、分級
機の一次エアー量と二次エアー量の制御によって行った。得られた窒化珪素粉末につき、
上記方法に従い、ｄ５０、ｄ７５／ｄ２５及びエタノール吸液量を測定した。また、窒化
珪素粉末の充填性として、窒化珪素粉末を金型プレス成形後９８ＭＰａの圧力でＣＩＰ成
形し、アルキメデス法によりＣＩＰ成形体の相対密度を測定した。それらの結果を表１に
示す。
Examples 2-4 Comparative Examples 1-4 Reference Examples 1-2
Α can be obtained by direct nitridation of metal silicon powder (for example, see Example 1 of JP-A-2-44017).
After producing a silicon nitride ingot having a rate of 90% or more, it is roughly crushed with a jaw crusher.
Further, the mixture was crushed and finely pulverized with a tube mill and a vibration mill, and then classified with an airflow classifier to produce silicon nitride powder shown in Table 1. The particle size adjustment of the silicon nitride powder was performed by controlling the feed amount of the vibration mill and the primary air amount and secondary air amount of the classifier. About the obtained silicon nitride powder,
According to the above method, d50, d75 / d25, and ethanol absorption were measured. Further, as a filling property of the silicon nitride powder, the silicon nitride powder was subjected to CIP molding at a pressure of 98 MPa after die press molding, and the relative density of the CIP compact was measured by Archimedes method. The results are shown in Table 1.
窒化珪素粉末９２質量部、アルミナ粉末３質量部、イットリア粉末５質量部及び水１５質量部を加え、ボールミルで湿式混合した。これをスプレードライヤーで造粒・乾燥し、金型プレス成形後２４５ＭＰａの圧力でＣＩＰ成形してから、窒素雰囲気中、温度１７５０℃で４時間焼結し、窒化珪素焼結体を製造した。 92 parts by mass of silicon nitride powder, 3 parts by mass of alumina powder, 5 parts by mass of yttria powder, and 15 parts by mass of water were added and wet mixed by a ball mill. This was granulated and dried with a spray dryer, CIP-molded at a pressure of 245 MPa after mold press molding, and then sintered at a temperature of 1750 ° C. for 4 hours in a nitrogen atmosphere to produce a silicon nitride sintered body.
得られた窒化珪素焼結体について、高温強度（ＪＩＳ Ｒ１６０４による８００℃の４点曲げ強さ）と耐食性を測定した。耐食性は、黒鉛ルツボ内に温度７５０℃の溶融アルミニウムを形成させ、高温強度測定と同じ試験片を２４時間浸し、侵食深さをマイクロメータで計測した。それらの結果を表１に示す。 About the obtained silicon nitride sintered compact, high temperature strength (800 degreeC 4-point bending strength by JISR1604) and corrosion resistance were measured. Corrosion resistance was obtained by forming molten aluminum at a temperature of 750 ° C. in a graphite crucible, immersing the same specimen as the high-temperature strength measurement for 24 hours, and measuring the erosion depth with a micrometer. The results are shown in Table 1.
本発明の窒化珪素粉末は、非鉄金属の溶湯用部品の製造用原料や樹脂充填材等として使用することができる。 The silicon nitride powder of the present invention can be used as a raw material for manufacturing non-ferrous metal molten metal parts, a resin filler, and the like.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0193470A (en) * | 1987-09-30 | 1989-04-12 | Toshiba Corp | Ceramic sintered material |
| JPH03159907A (en) * | 1989-11-16 | 1991-07-09 | Denki Kagaku Kogyo Kk | Silicon nitride powder |
| JPH06322457A (en) * | 1993-05-13 | 1994-11-22 | Hitachi Metals Ltd | Silicon nitride parts for melting and casting of aluminum and melting and casting equipment using the same |
| JPH08119743A (en) * | 1994-10-19 | 1996-05-14 | Hitachi Metals Ltd | Silicon nitride sintered compact excellent in strength at high temperature and its production and member for metal-melting bath |
| JPH11322311A (en) * | 1998-05-18 | 1999-11-24 | Shin Etsu Chem Co Ltd | Silicon nitride powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0193470A (en) * | 1987-09-30 | 1989-04-12 | Toshiba Corp | Ceramic sintered material |
| JPH03159907A (en) * | 1989-11-16 | 1991-07-09 | Denki Kagaku Kogyo Kk | Silicon nitride powder |
| JPH06322457A (en) * | 1993-05-13 | 1994-11-22 | Hitachi Metals Ltd | Silicon nitride parts for melting and casting of aluminum and melting and casting equipment using the same |
| JPH08119743A (en) * | 1994-10-19 | 1996-05-14 | Hitachi Metals Ltd | Silicon nitride sintered compact excellent in strength at high temperature and its production and member for metal-melting bath |
| JPH11322311A (en) * | 1998-05-18 | 1999-11-24 | Shin Etsu Chem Co Ltd | Silicon nitride powder |
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| US10611898B2 (en) | 2015-07-31 | 2020-04-07 | Nippon Sheet Glass Company, Limited | Glass flakes and resin composition |
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