JPH0722692B2 - Container for hydrothermal synthesis - Google Patents

Container for hydrothermal synthesis

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Publication number
JPH0722692B2
JPH0722692B2 JP19433888A JP19433888A JPH0722692B2 JP H0722692 B2 JPH0722692 B2 JP H0722692B2 JP 19433888 A JP19433888 A JP 19433888A JP 19433888 A JP19433888 A JP 19433888A JP H0722692 B2 JPH0722692 B2 JP H0722692B2
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container
inner
cylindrical
micropores
buffer chamber
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JPH0243939A (en
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康太郎 千葉
政征 河合
基秀 畑中
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株式会社日本製鋼所
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Priority to JP19433888A priority Critical patent/JPH0722692B2/en
Priority to CN 90101411 priority patent/CN1022335C/en
Publication of JPH0243939A publication Critical patent/JPH0243939A/en
Publication of JPH0722692B2 publication Critical patent/JPH0722692B2/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • B01J3/046Pressure-balanced vessels
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL-GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02Apparatus characterised by their chemically-resistant properties
    • B01J2219/0204Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
    • B01J2219/0236Metal based

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、人工水晶の製造等に使用する水熱合成用容器に関する。 BACKGROUND OF THE INVENTION (FIELD OF THE INVENTION) The present invention relates to a hydrothermal synthesis vessel used in the manufacture or the like of artificial quartz.

(従来の技術) 従来の水熱合成用容器の一例を第4図に示す。 Shown in FIG. 4 an example of a (prior art) conventional containers for hydrothermal synthesis. 21は容器本体、22は蓋、23はクランプ、24は対流制御板、25はヒータであり、各26は熱電対である。 21 container body 22 lid, 23 clamp 24 is convection control plate, 25 is a heater, the 26 is a thermocouple. 容器本体21内には種子Aと原料Bとが収容され、ヒータ25にて加熱された強アルカリ溶液内に浸漬されている。 The container body 21 is housed and seed A and the raw material B, and is immersed in a strongly alkaline solution, which is heated by the heater 25. 人工水晶の場合を例にとると、温度350〜400℃、圧力1000〜1500kg/cm 2で使用されるために容器本体21は、高強度、高靭性、かつ耐蝕性に優れた金属材料が使用される。 Taking the case of synthetic quartz as an example, a temperature 350 to 400 ° C., the container body 21 to be used at a pressure 1000~1500kg / cm 2, a high strength, high toughness, and metallic materials used with excellent corrosion resistance It is.

水熱合成で製造される製品は、電子、光学等の分野への用途が多く、今後益々、小型化、薄帯化される傾向にあるが、製品を粗悪化する主要因として異物の混入がある。 Products manufactured in the hydrothermal synthesis, the electronic, many applications in the field of optical, etc., more and more in the future, miniaturization, but tend to be thin fasciated, foreign substances are mainly due to poor the product is there. 特に、容器本体21内面が、強アルカリ溶液によつて侵蝕され、アクマイトなる鉄化合物を生じ、Fe+イオンが製品へ混入するのが最大の問題点であり、種々の対策がとられている。 In particular, the container body 21 inner surface, is by connexion attack in strong alkaline solution, resulting a Akumaito comprising iron compound, Fe + ions are the biggest problems of contamination to products, various countermeasures have been taken.

一例として種子Aの表面を隔離する方法があるが、十分ではなく、又保護した面は成長が阻害されて生産効率が低下する。 There is a method to isolate the surface of the seeds A as an example, but not sufficient, also protected surface decreases the production efficiency growth is inhibited.

又、容器本体21の内面を銀、金、白金等で被覆するか、 Further, either to cover the inner surface of the container body 21 silver, gold, platinum, or the like,
或は上記貴金属で製作した内筒容器を容器本体21に内蔵させて、Fe +イオンの発生自体を阻止することもなされている。 Or a cylindrical container inner fabricated with the noble metal be built in the container body 21, it has also been made to prevent the occurrence itself of Fe + ions.

(発明が解決しようとする課題) 容器本体21の内面を、銀、金、白金筒で被覆する場合は、容器本体21の内壁との密着性を確保する上から、水圧拡管又は爆着等の手段を要し、製作が非常に困難である許りでなく、容器本体21の構造によつては、密封個所のシート面の保守に問題を生じ、又銀、金、白金等で製作した内筒容器を容器本体21に内蔵させる場合には、内筒容器に、一方的な外圧が作用しないように、内筒容器の内外の圧力を均等化させる必要があり、このためには、内筒容器の内外の液量割合を同一に保持することが肝要である。 The inner surface of the (0006) the container body 21, silver, gold, when coating with platinum barrel, from the top to secure the adhesion between the inner wall of the container body 21, such as hydraulic pipe expansion or explosive bonding requires means, production is not Motori is very difficult, I go-between in the structure of the container body 21, it causes problems in the maintenance of the sheet surface of the sealing point, Matagin, gold, among which were fabricated in platinum, etc. in case of incorporating a cylindrical container to the container body 21, the inner cylinder container, as unilateral external pressure is not applied, it is necessary to equalize the pressure inside and outside of the inner cylinder chamber, for this purpose, the inner cylinder it is important to hold the inner and outer liquid volume ratio of the container in the same. しかして、上記両者の適用範囲は、共に実験用の小型容器に限定されていた。 Thus, the scope of application of the two has been both limited to a small container for the experiment.

(課題を解決するための手段) 本発明は、上記の事情に鑑みてなされ、大型にして工業用に適した水熱合成用容器を提供するものであり、その構成は次の通りである。 (Means for Solving the Problems) The present invention has been made in consideration of the above circumstances, there is provided a hydrothermal synthesis vessel suitable for industrial and large, its structure is as follows. すなわち、第1発明は、外部から加熱される容器本体内に筒状間隙を設けて内蔵され、 That is, the first invention is built by providing a cylindrical gap in the container body to be heated from the outside,
少なくとも内面が、銀、金、白金等の貴金属で形成された内筒容器の蓋に微小孔を設け、該微小孔を被う壁を蓋の上面側又は下面側に設けて蓋と壁とで形成される緩衝室となし、該壁面にも微小孔を有せしむる水熱合成用容器である。 At least the inner surface, silver, gold, a small hole is provided in the lid of the cylindrical container inner formed by a noble metal such as platinum, a lid and a wall provided with a wall covering the fine small hole on the top side or the underside of the lid It formed the buffer chamber and without a container Shimuru hydrothermal Yuse micropores in the wall surface.

又、第2発明は、外部から加熱される容器本体内に筒状間隙を設けて内蔵され、少なくとも内面が銀、金、白金等の貴金属で形成された内筒容器の蓋に微小孔を設け、 The second invention is incorporated in a cylindrical gap provided in the container body is heated from the outside, provided at least the inner surface is silver, gold, capped micropores of the cylindrical container inner formed by a noble metal such as platinum ,
該微小孔を被う壁を蓋の上面側又は下面側に設けて蓋と壁とで形成される緩衝室となし、該壁面にも微小孔を有せしむる水熱合成用容器に於て、緩衝室の空間容積、前記筒状間隙の実空間容積及び内筒容器の実空間容積に、 The wall covering the fine stoma At a top side or a buffer chamber and without that provided on the lower surface side is formed by the lid and the wall, container Shimuru hydrothermal Yuse micropores in the wall surface of the lid , the space volume of the buffer chamber, the real space volume in the real space volume and the inner cylinder chamber of the cylindrical gap,
それぞれ一定の液量割合としてアルカリ溶液を充填し、 Each alkaline solution charged with a constant amount of liquid fraction,
かつ緩衝室と筒状間隙とに充填したアルカリ溶液の濃度を内筒容器内のアルカリ濃度よりも薄く設定した水熱合成用容器である。 And a buffer chamber and the tubular gap and container set hydrothermal synthesis thinner than the alkali concentration of the inner tube in the container the density of the filled alkaline solution.

そして、上記両発明に於て、熱伝導性良好な通気性物質を容器本体と内筒容器との間の筒状間隙に充填させることもある。 Then, At a the both invention, also it is filled with thermally conductive good breathability material in the cylindrical gap between the container body and the inner cylinder chamber.

(作 用) 次に作用について説明する。 (For work) and then the operation will be explained.

水熱合成用容器の内筒容器の中に種子と原料とを入れて、容器本体を外部から加熱して水熱合成が行われる。 Some of the inner cylinder chamber of the container for hydrothermal synthesis to put the seeds and the raw material, the hydrothermal synthesis is performed by heating the container body from the outside.

その際、内筒容器は、少なくとも内面が貴金属で形成してあるので、容器本体内でFe +イオンが発生して、種子に影響を与えることがない。 At that time, the inner cylinder vessel, since at least the inner surface is formed with a precious metal, and Fe + ions are generated in the container body, there is no influence on seeds.

又容器本体の筒状間隙と内筒容器内とは、内筒容器の蓋及び緩衝室の壁面に設けた微小孔で連通しているので、 Also within the tubular gap and the inner tube container of the container body, because it communicates with the micro hole formed in the wall of the lid and the buffer chamber of the inner cylinder chamber,
内筒容器内外の圧力が均衡し、内筒容器は一方的な外圧を受けない。 And the pressure in the inner cylinder chamber and out the balance, the inner cylinder chamber is not subject to unilateral external pressure. 従つて、内筒容器が歪んだり、破損することがない。 Follow go-between, distorted inner cylinder container, is not damaged.

又前記の水熱合成用容器の緩衝室の空間容積、筒状間隙の実空間容積及び内筒容器の実空間容積に、それぞれ一定の液量割合とするアルカリ溶液を充填し、かつ緩衝室及び筒状間隙に充填したアルカリ溶液の濃度を、内筒容器内のアルカリ溶液濃度よりも薄くして使用することによつて、筒状間隙内と内筒容器内との圧力は、実質的に均衡する。 The space volume of the buffer chamber of the container for the hydrothermal synthesis, the real space volume in the real space volume and the inner cylinder chamber of the tubular gap was filled with in each alkaline solution to a predetermined liquid volume ratio, and the buffer chamber and the concentration of the alkaline solution was filled into the cylindrical gap, the pressure of the inner cylinder Yotsute to be used in thinner than the alkali concentration of the solution in the container, the tubular gap inside the inner tube in the container, substantially balanced to. しかも、圧力変化が生じると、両微小孔を通して筒状間隙内と内筒容器内の圧力が均衡する。 Moreover, when the pressure change occurs, the pressure in the inner cylinder in the container and the cylindrical gap in through both micropores are balanced.

筒状間隙内の圧力が上昇した場合には、Fe +イオンを含んだ微量のアルカル溶液が微小孔から緩衝室内へ侵入するが、緩衝室内のアルカリ溶液と混合し、Fe +イオンが稀釈されて内筒容器内へ侵入するので、種子に与える影響が微小であり、加えて、筒状間隙に充填したアルカリ溶液の濃度が薄いので容器本体の内面が侵蝕され難く、 When the pressure in the cylindrical gap is increased, although Arukaru solution of trace containing Fe + ions entering from micropores to buffer chamber, is mixed with a buffer chamber of the alkaline solution, Fe + ions are diluted since entering into the inner cylinder container, influence seed is small, in addition, difficult since the low concentration of the alkali solution was filled into the cylindrical gap inside surface of the container body is eroded,
Fe +イオンの発生量が減少するのと相俟つて種子への影響が更に軽減される。 Impact on cooperation with connexion seed and the generation amount of Fe + ions are reduced is further reduced.

更に、熱伝導性良好な通気性物質を筒状間隙に充填しておくと、容器本体から内筒容器への熱伝達が良好になされ、かつ筒状間隙内の圧力を均等に保つ。 Further, when the heat conductivity good breathability material be filled in the cylindrical gap, heat transfer to the inner cylinder container from the container body is made good, and keep the pressure in the cylindrical gap evenly.

(実施例) 本発明に係る水熱合成用容器の実施例を図面に基づいて説明する。 It will be described based on examples (Example) container hydrothermal synthesis according to the present invention with reference to the drawings.

第1図に於て、1は外部から加熱される容器本体であり、高強度、高靭性かつ耐蝕性に優れた金属材料からなる。 At a first figure, 1 is a container body is heated from the outside, made of a high strength, a metal material having excellent high toughness and corrosion resistance. 2は容器本体の蓋であり、パツキング2aを介装して、複数個のクランプ3にて容器本体1に着脱可能に装着されている。 2 is a lid of the container body, and interposed Patsukingu 2a, and is detachably mounted on the container main body 1 at a plurality of clamps 3.

4は、有底筒状の内筒容器であり、銀、金、白金等の貴金属製又はTi(チタン)材等の内面に貴金属を合せ材とした材料からなつている。 4 is a inner tube container bottomed cylindrical, silver, gold, and summer from precious metal or Ti materials with material fit a noble metal on the inner surface of the (titanium) material or the like such as platinum. 着脱可能な内筒容器の蓋4a及び底板4bも同様の材料からなり、該蓋4aのほぼ中央部には、第2図に詳示するように微小孔4a′を設けてある。 The lid 4a and the bottom plate 4b of the removable inner tube container also made of a material similar to that of, in a substantially central portion of the lid 4a, is provided with micropores 4a 'as shown in detail in Figure 2.
この微小孔4a′は、圧力が作用しない状態では、表面張力によつて自重では液体が流下しない大きさであり、具体的には0.4mmφ程度である。 The micropores 4a 'is in the state in which the pressure does not act, in'll connexion own weight to the surface tension is a size that liquid does not flow down, particularly of the order of 0.4 mm. そして、該容器の蓋4aの上面に、微小孔4a′を被つて箱形部材5aを固着して緩衝室5を形成し、この箱型部材5aの天板にも0.4mmφ程度の微小孔5bを設けてある。 Then, the upper surface of the container lid 4a, micropores 4a 'to form a buffer chamber 5 by fixing the object connexion box-shaped member 5a, microporous 5b of about 0.4mmφ to the top plate of the box-shaped member 5a a is provided. なお、この微小孔5bの位置は、緩衝室5に充填される液体の液面よりも高い位置とする。 The position of the micropores 5b is positioned higher than the liquid level of the liquid to be filled into the buffer chamber 5.

又、緩衝室5の少なくとも内面は貴金属で形成されている。 At least the inner surface of the buffer chamber 5 is formed by a noble metal.

上記の構成からなる内筒容器4が容器本体1との間に筒状間隙1aを設けて該本体1に内蔵されている。 Inner cylinder container 4 having the above structure is provided with a cylindrical gap 1a is incorporated in the body 1 between the container body 1.

6aは内筒容器4内に設けられた対流制御板であり、6bは内筒容器4と本体1との間の筒状間隙1aに設けられた対流制御板である。 6a is a convection control plate provided on the inner cylinder container 4, 6b are convection control plate provided in the cylindrical gap 1a between the inner cylinder container 4 and the body 1. そして、内筒容器4内の対流制御板6a The convection control plate 6a of the inner cylindrical vessel 4
の上方に種子を、下方に原料をそれぞれ収容し、緩衝室5の空間容積及び容器本体1と内筒容器4との筒状間隙 Cylindrical gap seeds upwards, raw materials were respectively housed downward, the space volume and the container body 1 and the inner cylinder chamber 4 of the buffer chamber 5
1aの実空間容積及び内筒容器4の実空間容積に、それぞれ一定の液量割合とするアルカリ溶液を充填し、かつ緩衝室5及び筒状間隙1aに充填したアルカリ溶液の濃度を、内筒容器4内のアルカリ濃度よりも薄く設定する。 In the real space real space volume of the volume and the inner cylinder container 4 1a, respectively filling the alkaline solution to be constant liquid volume ratio, and the concentration of the alkaline solution was filled into the buffer chamber 5 and the cylindrical gap 1a, the inner cylinder thin set than the alkali concentration in the container 4.

この状態にて、容器本体1を外部から加熱して、水熱合成を行う。 In this state, by heating the container body 1 from the outside, it performs a hydrothermal synthesis.

次に作用を説明する。 Next, a description will be given of the operation.

緩衝室5は、微小孔5bを介して筒状間隙1aと又微小孔4 Buffer chamber 5, or microporous 4 a cylindrical gap 1a through micropores 5b
a′を介して内筒容器4の内部と連通しているので、筒状間隙1a内の液量と内筒容器4内の液量とが一定割合から若干相違し、或は加熱によつて筒状間隙1a内の液温と内筒容器4内の液温との相違に基づいて、内筒容器4の内外に圧力差を生ずると、緩衝室5内のアルカリ溶液が、内筒容器4内又は筒状間隙1a内へと移動して、内筒容器4の内外圧力の均衡が保たれる。 Since the communication with the interior of the inner cylinder container 4 via a ', a cylindrical liquid amount of gap in 1a and liquid volume of the inner cylinder container 4 and is slightly different from the constant rate, or Yotsute the heating based on the difference in liquid temperature Metropolitan inner cylinder container 4 within the liquid temperature Prefecture in the cylindrical gap 1a, the resulting pressure difference inside and outside of the inner cylinder container 4, an alkaline solution of the buffer chamber 5, the inner cylinder container 4 navigate to the inner or tubular gap inside 1a, balancing internal and external pressure of the inner cylinder container 4 is maintained.

又筒状間隙1a内のFe +イオンを含んだアルカリ溶液は、 The alkaline solution containing Fe + ions in cylindrical gap 1a is
緩衝室5内のアルカリ溶液と混合して内筒容器4内へ入るので、Fe +イオンは稀釈されており、その製品に対する影響が減少する。 Since entering into the inner cylinder chamber 4 and mixed with an alkaline solution of the buffer chamber 5, Fe + ions are diluted, reducing the impact on the product.

又、筒状間隙1a内のアルカリ溶液は、内筒容器4内のアルカリ溶液によりも濃度を薄くしてあるので、容器本体1の侵蝕度合が低下し、Fe +イオンの発生が減少する。 Further, the alkaline solution in the cylindrical gap 1a, since also the alkaline solution of the inner cylinder chamber 4 are thin density, corrosion degree of the container main body 1 is lowered, the generation of Fe + ions is decreased.

第3図に、緩衝室の他の構造例として緩衝室5′を示す。 In Figure 3, it shows the buffer chamber 5 'as another example of the configuration of the buffer chamber. 内筒容器の蓋4aの下面に、微小孔4a′を被つて箱形部材5′aを固着して緩衝室5′を形成し、液面よりも上方となる側板にも0.4mmφ程度の微小孔5′bを設けてある。 The lower surface of the lid 4a of the inner cylinder chamber, micropores 4a to form a 'to be connexion box-shaped member 5'a damping chamber by fixing the 5', the order of 0.4mmφ also upward to become the side plates the liquid level fine a hole 5'b is provided.

なお、この緩衝室5′は、内外面共に貴金属であることが好ましい。 Incidentally, the buffer chamber 5 'is preferably both inner and outer surfaces, the noble metals.

このような緩衝室5′を設ければ、微小孔4a′から流入したFe +イオンを含むアルカリ溶液は、緩衝室5′内のアルカリ溶液と混合して、Fe +イオンが希釈されて内筒容器4内へ入るので実施例とほぼ同様な作用効果を有す。 'By providing the microporous 4a' such damping chamber 5 alkaline solution containing Fe + ions flowing from is mixed with the alkaline solution in the buffer chamber 5 ', the inner and Fe + ions are diluted cylinder since entering into the container 4 have a substantially same effect as example.

又、容器本体1と内筒容器4との間の熱伝達は、良好であることが望まれるので、筒状間隙1aの巾が大きく、熱伝達が疎外されるような場合には、熱伝導性良好にして通気性を有し、かつ熱膨張率の大きい材料、例えばNi金属発泡体を筒状間隙1a内に充填する。 Further, heat transfer between the inner cylinder container 4 and the container body 1, since it is desired to be good, large width of the cylindrical gap 1a, if such heat transfer is alienation, thermal conductivity sex good as to have breathable and filling material having a large thermal expansion coefficient, for example, a Ni metal foam into the tubular gap inside 1a.

ここで、通気性を要求するのは、筒状間隙1a内の均圧を保持するためであり、又大きな熱膨張率を要求するのは、温度上昇と共に容器本体1の内壁及び内筒容器4の外壁への密着が良好となるためである。 Here, to request breathability is for the purpose of holding the pressure equalization in the cylindrical gap 1a, also to request a larger coefficient of thermal expansion, the inner wall and the inner cylinder container 4 container body 1 as the temperature increases adhesion to the outer wall of the is to become good.

(発明の効果) 以上の説明によつて理解されるように、本発明によれば、下記の効果を有する。 As by connexion it understood the above description (Effect of the Invention) According to the present invention has the following effects.

本装置によれば、種子を内部に配置した内筒容器自体からのFe +イオンの発生がない。 According to this device, there is no occurrence of Fe + ions seeds from cylindrical container itself among placed therein.

内筒容器は、比較的薄肉で製作されるが、内外圧力を均衡できるので、内筒容器の歪や破損を生じることなく、安定した操業がなされる。 Inner tube container is being manufactured at a relatively thin, it is possible to balance the internal and external pressures, without causing distortion or damage of the inner cylinder container, stable operation is made.

容器本体がアルカリ溶液に侵蝕されて発生したFe +イオンは、内筒容器に対する外圧が高くなつた場合には、 Fe + ions container body occurs is corroded in alkaline solution, when the external pressure was high summer against the inner cylindrical vessel,
緩衝室内のアルカリ溶液で稀釈されて内筒容器内へ入るので、種子に対するFe +イオンの影響が軽微となる。 Since the diluted with an alkaline solution of a buffer chamber enters into the inner cylinder chamber, the impact of Fe + ions to the seed becomes insignificant.

容器本体が接触するアルカリ溶液は、濃度が薄いので容器本体が侵蝕されて発生するFe +イオンの量を減少できる。 Container alkaline solution body contact can reduce the amount of Fe + ions generated are corroded the container body the density is thin.

以上の効果、良質な人工水晶のような水熱合成による製品を供給できるようになつた。 Above effects, it has fallen so that it can supply the product by hydrothermal synthesis, such as high-quality artificial quartz.

【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS

第1図は、本発明に係る水熱合成用容器の実施例の半部を示す断面図、第2図は、本実施例の内筒容器の蓋と緩衝室とを示す要部断面図、第3図は、同じく内筒容器の蓋と緩衝室との他の構造例を示す要部断面図、第4図は、従来の水熱合成用容器の断面図である。 Figure 1 is a sectional view showing a half portion of the embodiment of the container for hydrothermal synthesis according to the present invention, Figure 2 is a fragmentary sectional view showing the lid of the inner cylinder container of the present embodiment and the buffer chamber, Figure 3 is a cross sectional view showing another example of the configuration of the lid and the buffer chamber of the inner tube container also, FIG. 4 is a cross-sectional view of a conventional container for hydrothermal synthesis. 1:容器本体、1a:筒状間隙、4:内筒容器、4a:内筒容器の蓋、4a′:微小孔、4b:底板、5,5′:緩衝室、5a,5′a: 1: container body, 1a: cylindrical gap 4: inner tube container, 4a: inner tube container lid, 4a ': micropores, 4b: bottom plate, 5,5': buffer chamber, 5a, 5'a:
箱形部材(壁)、5b,5′b:微小孔、6a,6b:対流制御板。 The box-shaped member (wall), 5b, 5'b: micropores, 6a, 6b: convection control plate.

Claims (3)

    【特許請求の範囲】 [The claims]
  1. 【請求項1】外部から加熱される容器本体内に筒状間隙を設けて内蔵され、少なくとも内面が、銀、金、白金等の貴金属で形成された内筒容器の蓋に微小孔を設け、該微小孔を被う壁を蓋の上面側又は下面側に設けて蓋と壁とで形成される緩衝室となし、該壁面にも微小孔を有せしむることを特徴とする水熱合成用容器。 1. A built in in the container body is heated from the outside is provided a cylindrical gap, provided at least the inner surface, silver, gold, capped micropores of the cylindrical container inner formed by a noble metal such as platinum, fine stoma walls covering the lid upper side or on the lower surface side is formed by the lid and the walls buffer chamber and without, hydrothermal synthesis, wherein Shimuru also Yuse micropores in the wall surface use container.
  2. 【請求項2】外部から加熱される容器本体内に筒状間隙を設けて内蔵され、少なくとも内面が銀、金、白金等の貴金属で形成された内筒容器の蓋に微小孔を設け、該微小孔を被う壁を蓋の上面側又は下面側に設けて蓋と壁とで形成される緩衝室となし、該壁面にも微小孔を有せしむる水熱合成用容器に於て、緩衝室の空間容積、前記筒状間隙の実空間容積及び内筒容器の実空間容積に、それぞれ一定の液量割合としてアルカリ溶液を充填し、かつ緩衝室と筒状間隙とに充填したアルカリ溶液の濃度を内筒容器内のアルカリ濃度よりも薄く設定したことを特徴とする水熱合成用容器。 2. A built in in the container body is heated from the outside is provided a cylindrical gap, at least the inner surface is silver, gold, capped micropores of the cylindrical container inner formed by a noble metal such as platinum is provided, the the wall covering the micropores at a top side or a buffer chamber and without that provided on the lower surface side is formed by the lid and the wall, container Shimuru hydrothermal Yuse micropores in the wall surface of the lid, space volume of the buffer chamber, the alkaline solution in the real space volume of the real space volume and the inner cylinder chamber of the cylindrical gap, which is filled with the alkali solution, respectively as a constant liquid volume ratio, and were filled into a buffer chamber and a cylindrical gap hydrothermal synthesis vessel, characterized in that the set thinner than the alkali concentration of the inner tube in the container the density of.
  3. 【請求項3】熱伝導性良好な通気性物質を容器本体と内筒容器との間の筒状間隙に充填させた特許請求の範囲第1項又は第2項記載の水熱合成用容器。 3. A thermally conductive good breathability cylindrical first term range of the gap in the patent claims which has filled or hydrothermal synthesis container of the second claim of between substance container body and the inner tube container.
JP19433888A 1988-08-05 1988-08-05 Container for hydrothermal synthesis Expired - Lifetime JPH0722692B2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP19433888A JPH0722692B2 (en) 1988-08-05 1988-08-05 Container for hydrothermal synthesis
CN 90101411 CN1022335C (en) 1988-08-05 1990-02-03 Container for use in hydrothermal synthesis

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Application Number Priority Date Filing Date Title
JP19433888A JPH0722692B2 (en) 1988-08-05 1988-08-05 Container for hydrothermal synthesis
CN 90101411 CN1022335C (en) 1988-08-05 1990-02-03 Container for use in hydrothermal synthesis
DE19904003377 DE4003377C1 (en) 1988-08-05 1990-02-05

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JPH0243939A JPH0243939A (en) 1990-02-14
JPH0722692B2 true JPH0722692B2 (en) 1995-03-15

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US7081162B2 (en) 2001-06-06 2006-07-25 Nichia Corporation Method of manufacturing bulk single crystal of gallium nitride
US7132730B2 (en) 2001-10-26 2006-11-07 Ammono Sp. Z.O.O. Bulk nitride mono-crystal including substrate for epitaxy
US7160388B2 (en) 2001-06-06 2007-01-09 Nichia Corporation Process and apparatus for obtaining bulk monocrystalline gallium-containing nitride
US7335262B2 (en) 2002-05-17 2008-02-26 Ammono Sp. Z O.O. Apparatus for obtaining a bulk single crystal using supercritical ammonia
US7589358B2 (en) 2002-05-17 2009-09-15 Ammono Sp. Z O.O. Phosphor single crystal substrate and method for preparing the same, and nitride semiconductor component using the same
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US5552039A (en) * 1994-07-13 1996-09-03 Rpc Waste Management Services, Inc. Turbulent flow cold-wall reactor
JP3366820B2 (en) * 1997-02-19 2003-01-14 株式会社日立製作所 Oxidation processing method and apparatus and a reaction vessel
US6398867B1 (en) * 1999-10-06 2002-06-04 General Electric Company Crystalline gallium nitride and method for forming crystalline gallium nitride
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US7374615B2 (en) 2001-06-06 2008-05-20 Ammono.Sp.Zo.O Method and equipment for manufacturing aluminum nitride bulk single crystal
US7081162B2 (en) 2001-06-06 2006-07-25 Nichia Corporation Method of manufacturing bulk single crystal of gallium nitride
US7422633B2 (en) 2001-06-06 2008-09-09 Ammono Sp. Zo. O. Method of forming gallium-containing nitride bulk single crystal on heterogeneous substrate
US7160388B2 (en) 2001-06-06 2007-01-09 Nichia Corporation Process and apparatus for obtaining bulk monocrystalline gallium-containing nitride
US7252712B2 (en) 2001-06-06 2007-08-07 Ammono Sp. Z O.O. Process and apparatus for obtaining bulk monocrystalline gallium-containing nitride
US7057211B2 (en) 2001-10-26 2006-06-06 Ammono Sp. Zo.O Nitride semiconductor laser device and manufacturing method thereof
US7420261B2 (en) 2001-10-26 2008-09-02 Ammono Sp. Z O.O. Bulk nitride mono-crystal including substrate for epitaxy
US7132730B2 (en) 2001-10-26 2006-11-07 Ammono Sp. Z.O.O. Bulk nitride mono-crystal including substrate for epitaxy
US7335262B2 (en) 2002-05-17 2008-02-26 Ammono Sp. Z O.O. Apparatus for obtaining a bulk single crystal using supercritical ammonia
US7589358B2 (en) 2002-05-17 2009-09-15 Ammono Sp. Z O.O. Phosphor single crystal substrate and method for preparing the same, and nitride semiconductor component using the same
US9127372B2 (en) 2005-01-12 2015-09-08 The Japan Steel Works, Ltd. Pressure vessel for growing single crystals
US9926642B2 (en) 2005-01-12 2018-03-27 Furuya Metal Co., Ltd. Method of manufacturing a pressure vessel for growing single crystals

Also Published As

Publication number Publication date
CN1053819A (en) 1991-08-14
CN1022335C (en) 1993-10-06
JPH0243939A (en) 1990-02-14
DE4003377C1 (en) 1991-08-08

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