JPH03503158A - Method and apparatus for producing boron carbide crystals - Google Patents
Method and apparatus for producing boron carbide crystalsInfo
- Publication number
- JPH03503158A JPH03503158A JP90503055A JP50305590A JPH03503158A JP H03503158 A JPH03503158 A JP H03503158A JP 90503055 A JP90503055 A JP 90503055A JP 50305590 A JP50305590 A JP 50305590A JP H03503158 A JPH03503158 A JP H03503158A
- Authority
- JP
- Japan
- Prior art keywords
- furnace
- boron carbide
- nitrogen
- section
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/36—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using oxygen or mixtures containing oxygen as gasifying agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/991—Boron carbide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。 (57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】 炭化硼素結晶を製造するための方法および装置本発明は、炭化硼素結晶を製造す るための方法および装置に関する。より詳細には、本発明は、サブミクロンサイ ズの炭化硼素結晶の製造に向けられている。[Detailed description of the invention] Method and apparatus for producing boron carbide crystals The present invention relates to methods and apparatus for producing boron carbide crystals. TECHNICAL FIELD The present invention relates to a method and apparatus for. More specifically, the present invention It is aimed at the production of boron carbide crystals.
炭化硼素（Ｂ、Ｃ）は、高い硬度、高温での良好な構造保全性、および化学的不 活性を有するセラミック材料である。これらの特性により、炭化硼素は、装置、 例えば、外装めっき、サンドプラスチングノズル、軸受、ダイ、原子炉用コント ロールロッド、および耐熱ライナーを二次加工するために有用な材料となる。多 くのこれらの適用において、結晶が１ミクロメートルより小さいサイズである、 高純度で単分散の炭化硼素粉末を用いることが望ましい。狭い粒度の分散は、生 成物にある利益を与える。１つの利益は、最適な反応性である。Boron carbide (B, C) has high hardness, good structural integrity at high temperatures, and chemical resistance. It is an active ceramic material. These properties make boron carbide suitable for equipment, For example, exterior plating, sand plasting nozzles, bearings, dies, nuclear reactor controls. It is a useful material for fabricating roll rods and heat-resistant liners. Many In many of these applications, the crystals are less than 1 micrometer in size, It is desirable to use highly pure, monodisperse boron carbide powder. Narrow particle size dispersion confer a certain benefit on a product. One benefit is optimal reactivity.
他は、材料を熱圧し、細孔、過剰な炭素および低融点の金属炭化物の不純物を含 まない均一な微粒材料を得ることができることである。Others hot-press the material to remove pores, excess carbon, and low-melting metal carbide impurities. Therefore, it is possible to obtain a uniform fine grain material with no grains.
炭化硼素結晶を製造するための通常の方法は、酸化硼素化合物および炭素化合物 の粒状混合物をるつぼに置き、るつぼを高温炉の熱区分に通らせることである。The usual method for producing boron carbide crystals is to use boron oxide compounds and carbon compounds The granular mixture is placed in a crucible and the crucible is passed through the thermal section of a high temperature furnace.
この方法の主な問題は、極めて広範囲なミクロンサイズの範囲の結晶のみを製造 し、本質的に１ミクロメートルより小さいサイズの結晶を製造しない速度でその 反応温度まで混合物を加熱することである。The main problem with this method is that it only produces crystals in a very wide micron size range. and at a rate that does not produce crystals essentially smaller than 1 micrometer in size. by heating the mixture to reaction temperature.
本発明は、大部分の結晶がサブミクロメートルサイズである炭化硼素結晶を製造 するための装置および方法に向けられている。The present invention produces boron carbide crystals in which most of the crystals are submicrometer-sized. The present invention is directed to an apparatus and method for.
本発明の実施において用いる装置は、極めて高温で操作する改良変事炭素抵抗押 込型炉である。炉ユニットは、床部材および屋根部材を含み、これら２部材の間 のスペースは、熱区分と定める。熱は、屋根部材に隣接した炉ユニット内に位置 するヒータ一手段により熱区分に加えられる。The apparatus used in the practice of this invention is a modified carbon resistance press operating at extremely high temperatures. It is a built-in furnace. The furnace unit includes a floor member and a roof member, with a space between these two members. The space is defined as the thermal division. Heat is located in a furnace unit adjacent to the roof member Heat is applied to the section by means of a heater.
炉ユニットの他の部材は、炉の熱区分の上に位置する垂直供給管である。供給管 は、酸化硼素化合物および炭素化合物の窒素を含まない粒状混合物を供給するた めに設計されている。冷却液を供給管のまわりに循環させ、酸化硼素供給化合物 をその融点より低い温度に保つに十分に管を冷却する。炉ユニットは、供給管の 下を直接通る路中を炉の熱区分の床に沿って移動するように設計された一群のボ ート部材をも含む。Another member of the furnace unit is the vertical feed pipe located above the heat section of the furnace. supply pipe to provide a nitrogen-free granular mixture of boron oxide and carbon compounds. It is designed for Circulate the coolant around the supply tube to remove the boron oxide supply compound. Cool the tube sufficiently to keep it below its melting point. The furnace unit is connected to the supply pipe. A group of balls designed to move along the floor of the furnace's thermal section in a path that passes directly underneath. Also includes seat members.
炉ユニットの典型的な操作において、粒状混合物が供給管から炉の熱区分を通り 落下している間は、熱区分の温度を１５７０℃より高い温度に保持する。この温 度で酸化硼素化合物は炭素化合物と反応し、炭化硼素結晶を形成する。各ボート 部材が供給管の下を移動するので、ボートは炭化硼素結晶の積荷で充填され、こ れは炉の熱区分の外部の集積点にボートで移送される。In typical operation of a furnace unit, a granular mixture is passed from the feed pipe through the heat section of the furnace. During the drop, the temperature of the thermal section is maintained above 1570°C. This temperature At a certain temperature, boron oxide compounds react with carbon compounds to form boron carbide crystals. each boat As the parts move down the feed pipe, the boat is filled with a cargo of boron carbide crystals, which This is transported by boat to a collection point outside the thermal section of the furnace.
第４図は、本発明に従い炭化硼素と製造するにおいて用いられる高温炉の、はぼ 図式的な正両立面図である。FIG. 4 shows a schematic diagram of a high temperature furnace used in producing boron carbide according to the present invention. It is a schematic elevational view.
第２図は、炭化硼素のための出発材料を炉中に供給するために用いられる、第１ 図に示した炉の部材の、部分的に図式的な、詳細な図である。FIG. 2 shows the first 1 is a detailed, partially diagrammatic view of parts of the furnace shown in the figure; FIG.
図中、特に第１図に関して、本発明の高温炉を一般に文字Ｆで示す。炉の外部を 金属殻１０と定める。炉の内部を一般に屋根部材および床部材と定める。屋根部 材は、３部のデツキ、すなわち上部デツキ１１、中間デツキ１２、および下部デ ツキ１３からなり、床部材１４は、デツキ１３の下に位置する。屋根部材のデツ キおよび床部材はグラファイトから構成される。殻と屋根部材、および殻と床部 材の間のスペースは、断熱部１５を与える。In the figures, and with particular reference to FIG. 1, the high temperature furnace of the present invention is generally designated by the letter F. the outside of the furnace It is defined as a metal shell 10. The interior of the furnace is generally defined as a roof member and a floor member. roof part The material is divided into three decks: an upper deck 11, an intermediate deck 12, and a lower deck. It consists of a deck 13, and a floor member 14 is located below the deck 13. Depths of roof components The key and floor members are constructed of graphite. Shell and roof members, and shell and floor parts The spaces between the materials provide insulation 15.
ここで説明する炉において、断熱部１５は、ランプブラックで充填されている。In the furnace described here, the insulation section 15 is filled with lamp black.
デツキ１２と床部材１４の間のスペースは、炉の熱区分１７と定める。二次加工 されたグラファイトである、ヒーターボード１８は、熱区分１７の直接上の、上 部デツキ１１と中間デツキ１２０間のスペース１９中に位置する。直流電流は、 加熱媒質として各ボード中を流れる。The space between the deck 12 and the floor member 14 defines the thermal section 17 of the furnace. Second processing The heater board 18 , which is made of graphite, is located directly above the thermal section 17 . It is located in the space 19 between the partial deck 11 and the intermediate deck 120. The direct current is It flows through each board as a heating medium.
炉の熱区分１７の上には、３部からなる垂直シュート構造を有する。シュートの 低部は、スリーブ２０で定められ、これはデツキ１２中で留まり、デツキ１１を 通り、伸びている。シュートの上部は、スリーブ２０より小さい直径の、スリー ブ２１と定める。スリーブ２１の下端は、転移部２２によりスリーブ２０の上端 と連結している。スリーブ２１の最上端２１は、パツキングランド２３およびグ ランドナツト２３ａと嵌められており、密閉の組み立てを与える。Above the thermal section 17 of the furnace there is a three-part vertical chute structure. of the shoot The lower part is defined by a sleeve 20, which remains in the deck 12 and holds the deck 11. The street is growing. The upper part of the chute has a sleeve of smaller diameter than the sleeve 20. 21. The lower end of the sleeve 21 is connected to the upper end of the sleeve 20 by the transition part 22. It is connected with. The uppermost end 21 of the sleeve 21 is connected to the packing gland 23 and the gland 23. It is fitted with a rand nut 23a to provide a hermetic assembly.
特に第２図において示されるように、冷却ジャケットはシュートのスリーブ２１ 内に縦に組み立てられている。ジャケットは内部管２４と定められ、これは外部 管２５内に取り囲まれている。垂直供給管２６は、管２４内に縦に組み立てられ ており、これら管の間の環は、供給管の外部に沿い冷却液を循環させるための通 路２７と定める。冷却液は、入口部２８を通り通路２７に入る。管２４の外部と 管２５の内部の間の他の環は、出口部３０を通りジャケットを去る冷却液のため の通路２９と定める。As shown in particular in FIG. It is assembled vertically inside. The jacket is defined as an inner tube 24, which is It is surrounded within tube 25. Vertical feed pipe 26 is vertically assembled within pipe 24. The ring between these tubes is a conduit for circulating the coolant along the outside of the supply tube. 27. Coolant enters passage 27 through inlet 28 . the outside of the tube 24 and Another ring between the interior of the tube 25 is for the cooling liquid leaving the jacket through the outlet section 30. It is defined as passage 29.
本発明の実施において、炭化硼素を製造するための出発材料は、酸化硼素化合物 および炭素化合物の粒状混合物である。In the practice of the present invention, the starting material for producing boron carbide is a boron oxide compound. and a granular mixture of carbon compounds.
供給管２６中に粒状混合物を供給するための装置は、供給管の上端の上に位置す る。第２図において示されるように、用いることのできるある種の供給装置は、 スクリュー供給装置３１である。スクリュー供給装置上の流し出口３１ａは、撓 み継手３３でガラス見逸管３２の最上端に連結している。その底端で、見逸管は 、他の撓み継手３４で供給管２６の最上端に連結している。A device for feeding the granular mixture into the feed pipe 26 is located above the upper end of the feed pipe. Ru. As shown in FIG. 2, some feeding devices that can be used include: This is a screw feeding device 31. The sink outlet 31a on the screw feeder is It is connected to the uppermost end of the glass stop tube 32 with a joint 33. At its bottom end, the Miitsu tube is , is connected to the uppermost end of the supply tube 26 by another flexible joint 34.
操作 本発明の実施に従う炭化硼素結晶の製造を説明するために典型的な例を与えよう 。粒状混合物は、工業銘柄硼酸（Ｕ、Ｓ。operation Let us give a typical example to illustrate the production of boron carbide crystals according to the practice of the present invention. . The granular mixture was made of technical grade boric acid (U,S).
Ｂｏｒａｘ） 、サイズ−２００メツシユ（７４ミクロメートルよりも小さい） 、および５０％圧縮アセチレンカーボンブラック（ＧｕｌｆＯｉｌ ［：ｏ、） の物理的配合物からなる。混合物をエポキシ塗膜で塗布された改良乳鉢ミキサー 中で３０分間配合する。次反応化学量論に基づきおよそ２０％の炭素を超える過 剰の硼素を与えるだめの混合物を製造する。Borax), size - 200 mesh (smaller than 74 micrometers) , and 50% compressed acetylene carbon black (GulfOil [:o,) Consists of a physical formulation of. Improved mortar mixer with mixture coated with epoxy coating Blend for 30 minutes inside. Based on the following reaction stoichiometry, approximately 20% excess carbon A stock mixture is prepared which provides excess boron.
２ Ｂ２Ｏ３＋ ７ Ｃ−＋Ｂ、Ｃ＋ ６ ＣＤ４モルのＢニアモルのＣ＝１０ ０％ ４ Ｘ １．２モルのＢニアモルのＣ＝２０過剰のＢ混合物を３５０℃で３．５ 時間チタン皿中で加熱し、それを８２０３＋ Ｃに脱水する。皿は２インチの高 さ×２４インチの幅Ｘ７２インチの長さく ５ ｃｍ Ｘ ６１ｃｍ Ｘ １８ ３ａｎ）と測定され、 １７２インチ（１３ｃｍ）の直径の細孔を有するチタン 被覆で遮断し、水蒸気を加熱の間に混合物から出させる。冷却後、乾燥させた混 合物をゆるく凝集させるが、これは容易に＜１０メツシユ（１，６８ｍｍ）の凝 集体に分解させることができる。2 B2O3+ 7 C-+B, C+ 6 CD4 mol B near mol C=10 0% 4 X 1.2 mol of B near mol of C = 20 excess B mixture at 350°C by 3.5 Heat in a titanium dish for an hour and dehydrate it to 8203+C. The plate is 2 inches high x 24 inches wide x 72 inches long 5 cm x 61 cm x 18 3an) with pores measuring 172 inches (13 cm) in diameter. A cover is used to allow water vapor to escape from the mixture during heating. After cooling, dry the mixture. The mixture is loosely agglomerated, but this easily results in a coagulation of <10 mesh (1.68 mm). Can be broken down into aggregates.
製造のこの時点で、実質的な量の閉じ込められた空気を有するので、混合物は約 １！Ｍｂｓ／ｃｕ、ｆｔ（２４０，３ｋｇ／ｍ”）の嵩密度を有する。閉じ込め られた空気は約８０％のＮ２を有するが、これは反応し、窒化硼素を形成するの で望ましくない。問題を解決するために、混合物を真空に引き、それを脱泡し、 アルゴンを排気した供給混合物を満たすために用いる。従って、脱泡工程で炭化 硼素生成物中のＮ２濃度が約０．３〜０．４％に減少する。供給混合物が脱泡さ れていない状態において、サブミクロメートルの炭化硼素結晶の窒素含有量は、 １〜３％もの高さとなりうる。At this point in production, with a substantial amount of trapped air, the mixture is approximately 1! It has a bulk density of Mbs/cu, ft (240,3 kg/m”). Confinement The collected air has about 80% N2, which reacts to form boron nitride. and undesirable. To solve the problem, pull a vacuum on the mixture to degas it, Argon is used to fill the evacuated feed mixture. Therefore, carbonization occurs during the defoaming process. The N2 concentration in the boron product is reduced to about 0.3-0.4%. Feed mixture is defoamed In the untreated state, the nitrogen content of submicrometer boron carbide crystals is It can be as high as 1-3%.
脱泡工程の次に、粒状混合物３５はホッパー３６中に装填され、これはスクリュ ーコンベヤー３１に流し出口３１ａと反対の端で連結している。製造操作の間、 パージ用ガスとしてのアルゴンをパージライン３７を通してホッパー中にそして 、パージライン３８を通してスクリューコンベヤー中に向ける。コンベヤー中の スクリューシャツ）３１ｂは可変速度駆動を有するモーター３９で駆動する。ア ルゴンパージガスは、混合物３５中の酸化硼素および炭素化合物の反応に不活性 雰囲気を与える。Following the defoaming step, the granular mixture 35 is loaded into a hopper 36, which is - Connected to the conveyor 31 at the end opposite to the outlet 31a. During manufacturing operations, Argon as a purge gas is passed through purge line 37 into the hopper and , through purge line 38 and into the screw conveyor. in the conveyor The screw shirt) 31b is driven by a motor 39 with variable speed drive. a The rugone purge gas is inert to the reaction of boron oxide and carbon compounds in mixture 35. Gives the atmosphere.
混合物３５がコンベヤー３１から供給管２６中に移動する間、それはガラス見逸 管３２を通る。従って、見逸管は、炉中への反応混合物の流れを定期的に見て、 必要ならば調整的な処理を行うための「窓」を炉の操作員に与える。スクリュー コンベヤーから、混合物を０．３１１ ｂｓ／分（０，７ｋｇ／分）、好ましく は０．１〜０．２１ ｂｓ／分（０，２〜０．４ ｋｇ／分）の速度で供給管中 に移送する。混合物が供給管を通り落下する間、水（あるいは他の適当な冷却液 ）を連続的に冷却ジャケットの通路２７および２９を通して循環させる。While the mixture 35 moves from the conveyor 31 into the supply tube 26, it passes through the glass Passes through tube 32. Therefore, the lookout tube periodically watches the flow of the reaction mixture into the furnace and Gives the furnace operator a "window" to take corrective action if necessary. screw From the conveyor, the mixture is preferably is in the supply pipe at a rate of 0.1 to 0.21 bs/min (0.2 to 0.4 kg/min). Transfer to. Water (or other suitable cooling liquid) is used as the mixture falls through the supply tube. ) is continuously circulated through passages 27 and 29 of the cooling jacket.
ここで記載したように供給管を冷却することにより、管内の温度を無水硼酸の軟 化点である３００℃より低い温度に保つ。By cooling the supply pipe as described here, the temperature inside the pipe can be lowered to soften the boric acid anhydride. The temperature is kept below the oxidation point of 300°C.
粒状混合物が供給管を通して移動する間に冷却されないならば、それはすぐに半 液体相に変化し、管をふさぐであろう。If the granular mixture is not cooled while moving through the feed pipe, it will quickly become semi- It will change to a liquid phase and block the tube.
供給管２６から、粒状混合物３５は、炉下の熱区分１７を通り、生成物ボート４ ０中に下方落下し、炉の床１４に押し進む。第１図において示したように、生成 物ボートには連続脈理があり、それらは適当なコンベヤーシステム（示していな い）により動いている。From the feed pipe 26, the granular mixture 35 passes through the thermal section 17 below the furnace and into the product boat 4. It falls downward into the air and pushes forward onto the floor 14 of the furnace. As shown in Figure 1, generation The material boat has continuous striae, which are transported by a suitable conveyor system (not shown). ).
ボートは、約２インチ〜３インチ／分（５〜１８ｃｍ／分）の速度で熱区分１７ を通り押し込まれる。粒子３５が供給管２６の排出端２６ａで熱区分１７に入る 間、温度は約１５００℃である。温度は、粒子が生成物ボート中に落下する点で 約２０００℃に増大する。各生成物ボート４０が供給管の排出端の下を直接通る とき、それは炭化硼素結晶の積荷で充填され、生成物は熱区分の外部の集積点く 示していない）に移送される。The boat is in thermal section 17 at a speed of approximately 2 inches to 3 inches per minute (5 to 18 cm per minute). is pushed through. Particles 35 enter thermal section 17 at discharge end 26a of supply pipe 26 During this period, the temperature is approximately 1500°C. The temperature at which the particles fall into the product boat is The temperature increases to about 2000°C. Each product boat 40 passes directly under the discharge end of the feed pipe. When it is filled with a cargo of boron carbide crystals, the product is deposited at an accumulation point outside the thermal section. (not shown).
製造操作の間、熱区分１７は一酸化炭素およびアルゴンガスで充填され、炭化硼 素への出発材料の反応に望ましい不活性雰囲気を与える。第１図において示した ように、アルゴンは２点く１点は供給入口管２６を通り、他点は矢印４２で示し たように、区分の左端である）で熱区分中に導入される。左端から熱区分に入る アルゴン流は他の目的にもかなう。この流体は、熱区分を去るように生成物ボー ト４０が続く路に対して直向流で移動する。従って、ガス流は、混合物３５中の 粒子が炭化硼素の反応が完了する前に熱区分を押し流されることを防ぐためのバ リヤーとして作用する。During manufacturing operations, thermal section 17 is filled with carbon monoxide and argon gas and provides the desired inert atmosphere for the reaction of the starting materials to the reactants. Shown in Figure 1 As shown, argon passes through the supply inlet pipe 26 at two points, and the other points are indicated by arrows 42. is introduced into the thermal section at the left end of the section). Enter the heat section from the left end Argon flow also serves other purposes. This fluid is directed to the product bowl as it leaves the thermal section. 40 moves in a direction perpendicular to the path it follows. Therefore, the gas flow in the mixture 35 A barrier to prevent particles from being swept through the thermal compartment before the boron carbide reaction is complete. Acts as a rear.
サブミクロメートルサイズの炭化硼素結晶を得るかぎは、その開始反応温度より 高い温度で極めて速く出発材料を加熱し得ることである。従って、本発明の実施 において、熱区分の温度を１５７０℃より高い温度に保持することが重要である 。The key to obtaining submicrometer-sized boron carbide crystals is the starting reaction temperature. It is possible to heat the starting material very quickly at high temperatures. Therefore, implementation of the present invention It is important to maintain the temperature of the thermal section above 1570°C. .
他の重要な要因は、反応温度より高い温度で粒子を加熱するためにかかる時間で ある。ここで記載した操作において、熱区分の温度は１６００℃〜２１．００℃ であり、粒子が熱区分を通り移動する間に加熱される速度は少なくとも２００℃ ／秒である。Another important factor is the time it takes to heat the particles above the reaction temperature. be. In the operation described here, the temperature of the thermal section is between 1600°C and 21.00°C. and the rate at which the particles are heated while moving through the thermal section is at least 200°C. /second.
生成した炭化硼素の量は、約１ボンド／時間（０，４６ｋｇ／時間）であり、約 ９０重量％の結晶がサブミクロメートルサイズであった。実際のサイズは０．１ 〜０．３ミクロメートルであった。The amount of boron carbide produced is approximately 1 bond/hour (0,46 kg/hour) and approximately 90% by weight of the crystals were submicrometer sized. Actual size is 0.1 ~0.3 micrometer.
国際調査報告 −International search report -
Claims (1)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US29568289A | 1989-01-11 | 1989-01-11 | |
| US295,682 | 1989-01-11 | ||
| PCT/US1989/005871 WO1990008102A1 (en) | 1989-01-11 | 1989-12-27 | Method and apparatus for producing boron carbide crystals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03503158A true JPH03503158A (en) | 1991-07-18 |
Family
ID=23138787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP90503055A Pending JPH03503158A (en) | 1989-01-11 | 1989-12-27 | Method and apparatus for producing boron carbide crystals |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP0429557A4 (en) |
| JP (1) | JPH03503158A (en) |
| KR (1) | KR910700196A (en) |
| AU (1) | AU621989B2 (en) |
| CA (1) | CA2007460A1 (en) |
| FI (1) | FI904446A0 (en) |
| IL (1) | IL93018A0 (en) |
| WO (1) | WO1990008102A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106810261A (en) * | 2017-04-12 | 2017-06-09 | 郑州嵩山硼业科技有限公司 | A kind of method that use intermediate frequency furnace smelts boron carbide |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO20010929D0 (en) * | 2001-02-23 | 2001-02-23 | Norsk Hydro As | A method for conducting thermal reactions between reactants and an oven for the same |
| CN110357106B (en) * | 2019-08-26 | 2022-07-29 | 燕山大学 | Method for preparing nano twin crystal boron carbide powder |
| CN113880093A (en) * | 2021-11-24 | 2022-01-04 | 郑州嵩山硼业科技有限公司 | Boron carbide production process |
| CN114506846B (en) * | 2022-02-15 | 2023-06-06 | 厦门金鹭特种合金有限公司 | Production method and production device of superfine carbide |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1897214A (en) * | 1930-05-14 | 1933-02-14 | Norton Co | Boron carbide and method of making the same |
| US2155682A (en) * | 1935-11-21 | 1939-04-25 | Norton Co | Method of making abrasive metal carbides |
| US3377141A (en) * | 1964-08-26 | 1968-04-09 | Cabot Corp | Process for producing metal carbides utilizing a solution treatment prior to reaction |
| US3379647A (en) * | 1966-05-04 | 1968-04-23 | Carborundum Co | Metal carbide and boride production |
| US3535080A (en) * | 1969-02-18 | 1970-10-20 | Norton Co | Apparatus and method for the continuous furnacing of borides,carbides and silicides |
| US4017587A (en) * | 1969-10-03 | 1977-04-12 | The United States Of America As Represented By The Secretary Of The Navy | Boron carbide |
| US4137295A (en) * | 1977-04-20 | 1979-01-30 | Tamers Murry A | Carbide production using molten metals as heat source |
| JPS55113609A (en) * | 1979-02-21 | 1980-09-02 | Ibiden Co Ltd | Manufacturing apparatus for beta crystallbase silicon carbide |
| JPS5825044B2 (en) * | 1979-05-23 | 1983-05-25 | 安藤 義則 | Method and device for producing ultrafine carbide powder |
| US4529575A (en) * | 1982-08-27 | 1985-07-16 | Ibiden Kabushiki Kaisha | Process for producing ultrafine silicon carbide powder |
| US4804525A (en) * | 1986-04-14 | 1989-02-14 | The Dow Chemical Company | Producing boron carbide |
| JPS63166709A (en) * | 1986-12-26 | 1988-07-09 | Ibiden Co Ltd | Production of carbide |
-
1989
- 1989-12-27 AU AU50364/90A patent/AU621989B2/en not_active Ceased
- 1989-12-27 WO PCT/US1989/005871 patent/WO1990008102A1/en not_active Application Discontinuation
- 1989-12-27 EP EP19900902739 patent/EP0429557A4/en not_active Withdrawn
- 1989-12-27 JP JP90503055A patent/JPH03503158A/en active Pending
- 1989-12-27 KR KR1019900701997A patent/KR910700196A/en not_active Application Discontinuation
-
1990
- 1990-01-09 IL IL93018A patent/IL93018A0/en unknown
- 1990-01-10 CA CA002007460A patent/CA2007460A1/en not_active Abandoned
- 1990-09-10 FI FI904446A patent/FI904446A0/en not_active IP Right Cessation
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106810261A (en) * | 2017-04-12 | 2017-06-09 | 郑州嵩山硼业科技有限公司 | A kind of method that use intermediate frequency furnace smelts boron carbide |
Also Published As
| Publication number | Publication date |
|---|---|
| WO1990008102A1 (en) | 1990-07-26 |
| AU5036490A (en) | 1990-08-13 |
| EP0429557A4 (en) | 1992-04-22 |
| AU621989B2 (en) | 1992-03-26 |
| FI904446A0 (en) | 1990-09-10 |
| CA2007460A1 (en) | 1990-07-11 |
| KR910700196A (en) | 1991-03-14 |
| IL93018A0 (en) | 1990-11-05 |
| EP0429557A1 (en) | 1991-06-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Weimer et al. | Rapid process for manufacturing aluminum nitride powder | |
| EP0414803B1 (en) | Method of producing boron carbide | |
| EP0734362B1 (en) | Firing fines | |
| JPH05333B2 (en) | ||
| EP0753491A1 (en) | Process for treatment of reactive fines | |
| JPS5841708A (en) | Preparation of graphite fluoride and its device | |
| NO174694B (en) | Apparatus and method for producing uniform, fine, boron-containing ceramic powders | |
| EP0582571B1 (en) | Process for preparing aluminium nitride powder via controlled combustion nitridation | |
| EP2014617A2 (en) | Process For Melting Silicon Powders | |
| CA1175238A (en) | Method and apparatus for the thermal production of metal carbides and metals | |
| JPH03503158A (en) | Method and apparatus for producing boron carbide crystals | |
| IE921931A1 (en) | Process for the preparation of aluminium nitride | |
| US3347958A (en) | Process for preparing granular ferroselenium | |
| JPH0118005B2 (en) | ||
| JPH0138042B2 (en) | ||
| CN112756619A (en) | Production method of submicron CuSn alloy powder with controllable element proportion | |
| JPH0135773B2 (en) | ||
| JP3006843B2 (en) | Method for producing metal complex containing silicon carbide powder | |
| JPH0224781B2 (en) | ||
| Bruno | Production of aluminum-silicon alloy and ferrosilicon and commercial purity aluminum by the direct reduction process. Second annual technical report for the period 1978 September 1-1979 December 31 | |
| JPS59146941A (en) | Method for fluidizing and chlorinating zirconium oxide | |
| JPS5820708A (en) | Production of superfine powder of silicon carbide mainly composed of beta-type crystal | |
| JPS63166709A (en) | Production of carbide | |
| JPS59141411A (en) | Production of ultrafine powder of silicon carbide | |
| TW201319003A (en) | Components of plant, such as reduction furnace body and/or electrode, in particular for a reduction furnace |