JPH0722692B2 - Hydrothermal synthesis container - Google Patents
Hydrothermal synthesis containerInfo
- Publication number
- JPH0722692B2 JPH0722692B2 JP63194338A JP19433888A JPH0722692B2 JP H0722692 B2 JPH0722692 B2 JP H0722692B2 JP 63194338 A JP63194338 A JP 63194338A JP 19433888 A JP19433888 A JP 19433888A JP H0722692 B2 JPH0722692 B2 JP H0722692B2
- Authority
- JP
- Japan
- Prior art keywords
- container
- lid
- buffer chamber
- hydrothermal synthesis
- cylindrical
- 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.)
- Expired - Lifetime
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/046—Pressure-balanced vessels
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/0204—Apparatus characterised by their chemically-resistant properties comprising coatings on the surfaces in direct contact with the reactive components
- B01J2219/0236—Metal based
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
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。TECHNICAL FIELD The present invention relates to a hydrothermal synthesis container used for manufacturing artificial quartz and the like.
（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。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。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。人工水晶の場合を例
にとると、温度350〜400℃、圧力1000〜1500kg/cm2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。(Prior Art) An example of a conventional container for hydrothermal synthesis is shown in FIG. Reference numeral 21 is a container body, 22 is a lid, 23 is a clamp, 24 is a convection control plate, 25 is a heater, and 26 are thermocouples. The seed A and the raw material B are contained in the container body 21 and immersed in the strong alkaline solution heated by the heater 25. Taking artificial quartz as an example, since the container body 21 is used at a temperature of 350 to 400 ° C and a pressure of 1000 to 1500 kg / cm 2 , the container body 21 is made of a metal material having high strength, high toughness, and excellent corrosion resistance. To be done.
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。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。Products manufactured by hydrothermal synthesis have many applications in fields such as electronics and optics, and there is a tendency for them to become smaller and thinner in the future. is there. In particular, the inner surface of the container body 21 is corroded by the strong alkaline solution to generate an iron compound, which is an acumite, and Fe + ions are mixed into the product, which is the biggest problem, and various measures are 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。As an example, there is a method of isolating the surface of the seed A, but it is not sufficient, and the growth of the protected surface is inhibited and the production efficiency is reduced.
又、容器本体21の内面を銀、金、白金等で被覆するか、
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。Also, whether the inner surface of the container body 21 is coated with silver, gold, platinum, or the like,
Alternatively, the inner cylindrical container made of the above-mentioned noble metal may be incorporated in the container body 21 to prevent generation 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。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。(Problems to be Solved by the Invention) When the inner surface of the container body 21 is coated with a silver, gold, or platinum cylinder, in order to ensure adhesion with the inner wall of the container body 21, a water pipe or explosion It requires a means and is very difficult to manufacture, and the structure of the container body 21 causes a problem in maintenance of the seat surface of the sealing portion, and is made of silver, gold, platinum or the like. When the cylindrical container is built in the container body 21, it is necessary to equalize the pressure inside and outside the inner cylindrical container so that the one-sided external pressure does not act on the inner cylindrical container. It is important to maintain the same liquid volume ratio inside and outside the container. However, both of the above-mentioned application ranges are limited to small containers for experiments.
（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。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、
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。(Means for Solving the Problems) The present invention has been made in view of the above circumstances, and provides a hydrothermal synthesis container that is large in size and suitable for industrial use, and has the following configuration. That is, according to the first aspect of the present invention, the container body, which is heated from the outside, is provided with a cylindrical gap provided therein.
At least the inner surface is made of a noble metal such as silver, gold, platinum, etc., and a fine hole is provided in the lid of the inner cylindrical container, and a wall covering the fine hole is provided on the upper surface side or the lower surface side of the lid to form a lid and a wall. This is a container for hydrothermal synthesis, which does not serve as a buffer chamber to be formed and has micropores on its 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、
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水熱合
成用容器である。A second aspect of the present invention is to provide a minute hole in a lid of an inner cylindrical container which is built in a container body heated from the outside with a cylindrical gap and at least the inner surface of which is made of a noble metal such as silver, gold or platinum. ,
A container for hydrothermal synthesis in which a wall covering the minute holes is provided on the upper surface side or the lower surface side of the lid to form a buffer chamber formed by the lid and the wall, and the wall surface also has the minute holes. , The space volume of the buffer chamber, the actual space volume of the cylindrical gap and the actual space volume of the inner cylindrical container,
Each is filled with an alkaline solution with a constant liquid volume ratio,
Further, it is a container for hydrothermal synthesis in which the concentration of the alkaline solution filled in the buffer chamber and the tubular gap is set to be lower than the alkaline concentration in the inner tubular container.
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。Further, in both of the above inventions, a breathable substance having good thermal conductivity may be filled in the tubular gap between the container body and the inner tubular container.
（作 用） 次に作用について説明する。(Operation) Next, the operation will be described.
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。The seed and the raw material are put in the inner cylindrical container of the container for hydrothermal synthesis, and the container body is externally heated to perform hydrothermal synthesis.
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 this time, since at least the inner surface of the inner cylindrical container is formed of a noble metal, Fe + ions are not generated in the container body and the seed is not affected.
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、
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。従つて、内筒容器が歪んだり、破損するこ
とがない。Further, since the cylindrical gap of the container body and the inside of the inner container are communicated with each other by the fine holes provided in the lid of the inner container and the wall surface of the buffer chamber,
The pressure inside and outside the inner cylinder container is balanced, and the inner cylinder container does not receive unilateral external pressure. Therefore, the inner cylindrical container is not distorted or 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。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。Further, the buffer chamber of the hydrothermal synthesis container, the actual space volume of the cylindrical gap, and the actual space volume of the inner cylinder container are respectively filled with an alkaline solution having a constant liquid volume ratio, and the buffer chamber and By making the concentration of the alkaline solution filled in the cylindrical gap thinner than the concentration of the alkaline solution in the inner cylindrical container, the pressure in the cylindrical gap and that in the inner cylindrical container are substantially balanced. To do. Moreover, when a pressure change occurs, the pressure in the cylindrical gap and the pressure in the inner cylindrical container are balanced through both micro holes.
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、
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。When the pressure in the cylindrical gap rises, a small amount of alcal solution containing Fe + ions enters the buffer chamber through the micropores, but it mixes with the alkaline solution in the buffer chamber and the Fe + ions are diluted. Since it penetrates into the inner cylindrical container, the effect on seeds is minimal, and in addition, since the concentration of the alkaline solution filling the cylindrical gap is low, the inner surface of the container body is unlikely to be eroded,
The effect on seeds is further reduced in combination with the decrease in the amount of Fe + ions generated.
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。Furthermore, when the air-permeable substance having good thermal conductivity is filled in the cylindrical gap, the heat transfer from the container body to the inner cylindrical container is made good, and the pressure in the cylindrical gap is kept uniform.
（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。(Example) The Example of the container for hydrothermal synthesis which concerns on this invention is described based on drawing.
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。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。In FIG. 1, reference numeral 1 denotes a container body heated from the outside, which is made of a metal material having high strength, high toughness and excellent corrosion resistance. Reference numeral 2 denotes a lid of the container body, which is detachably attached to the container body 1 with a plurality of clamps 3 via a packing 2a.
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。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。
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。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。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。Reference numeral 4 denotes a bottomed cylindrical inner cylinder container made of a noble metal such as silver, gold, platinum or the like, or a material such as a Ti (titanium) material having an inner surface made of a noble metal. The lid 4a and the bottom plate 4b of the detachable inner cylindrical container are also made of the same material, and a minute hole 4a 'is provided in substantially the central portion of the lid 4a as shown in detail in FIG.
The minute holes 4a 'are of a size such that the liquid does not flow down under its own weight due to surface tension when pressure is not applied, and is specifically about 0.4 mmφ. Then, the box-shaped member 5a is fixed to the upper surface of the lid 4a of the container to fix the box-shaped member 5a to form the buffer chamber 5, and the top plate of the box-shaped member 5a has a micro-hole 5b of about 0.4 mmφ. Is provided. The position of the minute holes 5b is higher than the liquid level of the liquid filled in 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 made of 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。The inner cylindrical container 4 having the above-described structure is built in the main body 1 with a cylindrical gap 1a provided between the inner cylindrical container 4 and the main 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。そして、内筒容器４内の対流制御板6a
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
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。6a is a convection control plate provided in the inner cylindrical container 4, and 6b is a convection control plate provided in the cylindrical gap 1a between the inner cylindrical container 4 and the main body 1. And the convection control plate 6a in the inner cylindrical container 4
The seeds above and the raw materials below, respectively, and the space volume of the buffer chamber 5 and the cylindrical gap between the container body 1 and the inner container 4.
The actual space volume of 1a and the actual space volume of the inner cylinder container 4 are filled with an alkali solution having a constant liquid volume ratio, and the concentration of the alkali solution filled in the buffer chamber 5 and the cylindrical gap 1a is changed to the inner cylinder. It is set to be thinner 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, the container body 1 is externally heated to perform hydrothermal synthesis.
次に作用を説明する。Next, the operation will be described.
緩衝室５は、微小孔5bを介して筒状間隙1aと又微小孔4
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。The buffer chamber 5 has a cylindrical gap 1a and a minute hole 4b through a minute hole 5b.
Since it communicates with the inside of the inner cylindrical container 4 via a ', the liquid amount in the cylindrical gap 1a and the liquid amount in the inner cylindrical container 4 may be slightly different from a certain ratio, or due to heating. When a pressure difference is generated between the inside and the outside of the inner cylindrical container 4 based on the difference between the liquid temperature in the cylindrical gap 1a and the liquid temperature in the inner cylindrical container 4, the alkaline solution in the buffer chamber 5 is By moving to the inside or the cylindrical gap 1a, the internal and external pressures of the inner cylindrical container 4 are balanced.
又筒状間隙1a内のFe+イオンを含んだアルカリ溶液は、
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。Also, the alkaline solution containing Fe + ions in the cylindrical gap 1a is
Since it mixes with the alkaline solution in the buffer chamber 5 and enters the inner cylindrical container 4, Fe + ions are diluted and the influence on the product is reduced.
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, since the alkaline solution in the cylindrical gap 1a has a lower concentration than that of the alkaline solution in the inner cylindrical container 4, the erosion degree of the container body 1 is reduced and the generation of Fe + ions is reduced.
第３図に、緩衝室の他の構造例として緩衝室５′を示
す。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。FIG. 3 shows a buffer chamber 5'as another structural example of the buffer chamber. A box-shaped member 5'a is fixed to the lower surface of the lid 4a of the inner cylindrical container to fix a box-shaped member 5'a to form a buffer chamber 5 ', and the side plate above the liquid surface has a minute diameter of about 0.4 mmφ. 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。The buffer chamber 5'is preferably made of noble metal on both the inner and outer surfaces.
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。If such a buffer chamber 5'is provided, the alkaline solution containing Fe + ions that has flowed in through the micropores 4a 'is mixed with the alkaline solution in the buffer chamber 5', and the Fe + ions are diluted to form an inner cylinder. Since it enters the container 4, it has substantially the same operational effect as the embodiment.
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。Moreover, since it is desired that the heat transfer between the container body 1 and the inner cylindrical container 4 is good, when the width of the cylindrical gap 1a is large and the heat transfer is alienated, the heat transfer is not performed. A material having good properties, breathability, and a large coefficient of thermal expansion, such as Ni metal foam, is filled in the cylindrical gap 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, the air permeability is required for maintaining the pressure equalization in the cylindrical gap 1a, and the large thermal expansion coefficient is required for the inner wall of the container body 1 and the inner cylindrical container 4 as the temperature rises. This is because the adhesion of the to the outer wall becomes 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。(Effects of the Invention) As can be understood from the above description, 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, Fe + ions are not generated from the inner cylindrical container itself in which the seed is arranged.
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。The inner cylindrical container is manufactured to have a relatively thin wall, but since the inner and outer pressures can be balanced, the inner cylindrical container can be stably operated without being distorted or damaged.
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、
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。Fe + ions generated when the container body is eroded by the alkaline solution, when the external pressure on the inner container becomes high,
Since it is diluted with the alkaline solution in the buffer chamber and enters the inner cylindrical container, the effect of Fe + ions on the seeds is slight.
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。Since the alkaline solution with which the container body comes into contact has a low concentration, the amount of Fe + ions generated by the corrosion of the container body can be reduced.
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。With the above effects, it has become possible to supply products manufactured by hydrothermal synthesis such as high-quality artificial quartz.
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。 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:
箱形部材（壁）、5b,5′b:微小孔、6a,6b:対流制御板。FIG. 1 is a cross-sectional view showing a half part of an embodiment of a hydrothermal synthesis container according to the present invention, and FIG. 2 is a main-part cross-sectional view showing a lid and a buffer chamber of an inner cylindrical container of the present embodiment, FIG. 3 is a sectional view of an essential part showing another example of the structure of the lid and the buffer chamber of the inner cylindrical container, and FIG. 4 is a sectional view of a conventional hydrothermal synthesis container. 1: Container body, 1a: Cylindrical gap, 4: Inner cylinder container, 4a: Inner cylinder container lid, 4a ': Micro holes, 4b: Bottom plate, 5,5': Buffer chamber, 5a, 5'a:
Box-shaped members (walls), 5b, 5'b: Micro holes, 6a, 6b: Convection control plate.
Claims (3)
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 micropore is provided in a lid of an inner cylindrical container which is built in a container body heated from the outside with a cylindrical gap and at least an inner surface of which is made of a noble metal such as silver, gold or platinum, A hydrothermal synthesis characterized in that a wall covering the minute holes is provided on the upper surface side or the lower surface side of the lid to form a buffer chamber formed by the lid and the wall, and the wall surface is also provided with the minute holes. Container.
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 micropore is provided in a lid of an inner cylindrical container which is built in a container body heated from the outside with a cylindrical gap and at least the inner surface of which is made of a noble metal such as silver, gold or platinum. In a container for hydrothermal synthesis in which a wall covering the micropores is provided on the upper surface side or the lower surface side of the lid to form a buffer chamber formed by the lid and the wall, and the wall surface also has the micropores. The space volume of the buffer chamber, the actual space volume of the cylindrical gap and the actual space volume of the inner cylindrical container are respectively filled with an alkaline solution at a constant liquid volume ratio, and the alkaline solution filled in the buffer chamber and the cylindrical gap. The hydrothermal synthesis container is characterized in that the concentration of is set lower than the alkali concentration in the inner cylindrical container.
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. The hydrothermal synthesis container according to claim 1 or 2, wherein a gas permeable substance having a good thermal conductivity is filled in a tubular space between the container body and the inner tubular container.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63194338A JPH0722692B2 (en) | 1988-08-05 | 1988-08-05 | Hydrothermal synthesis container |
| CN90101411.7A CN1022335C (en) | 1988-08-05 | 1990-02-03 | Container for hydrothermal synthesis |
| DE4003377A DE4003377C1 (en) | 1988-08-05 | 1990-02-05 |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63194338A JPH0722692B2 (en) | 1988-08-05 | 1988-08-05 | Hydrothermal synthesis container |
| CN90101411.7A CN1022335C (en) | 1988-08-05 | 1990-02-03 | Container for hydrothermal synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0243939A JPH0243939A (en) | 1990-02-14 |
| JPH0722692B2 true JPH0722692B2 (en) | 1995-03-15 |
Family
ID=36754727
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63194338A Expired - Lifetime JPH0722692B2 (en) | 1988-08-05 | 1988-08-05 | Hydrothermal synthesis container |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPH0722692B2 (en) |
| CN (1) | CN1022335C (en) |
| DE (1) | DE4003377C1 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7057211B2 (en) | 2001-10-26 | 2006-06-06 | Ammono Sp. Zo.O | Nitride semiconductor laser device and manufacturing method thereof |
| 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 |
| US9127372B2 (en) | 2005-01-12 | 2015-09-08 | The Japan Steel Works, Ltd. | Pressure vessel for growing single crystals |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4229468C2 (en) * | 1992-09-03 | 1995-06-14 | Streitenberg Hubert Dr Med | Containers for liquid or pasty ingredients threatened by bacterial attack |
| 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 treatment method and apparatus and reaction vessel |
| SE518803C2 (en) | 1999-09-03 | 2002-11-26 | Chematur Eng Ab | Method and reaction system with high pressure and high temperature suitable for supercritical water oxidation |
| US6398867B1 (en) * | 1999-10-06 | 2002-06-04 | General Electric Company | Crystalline gallium nitride and method for forming crystalline gallium nitride |
| JP2003063889A (en) * | 2001-08-24 | 2003-03-05 | Tokyo Denpa Co Ltd | Vessel for growing single crystal |
| CN1297695C (en) * | 2003-04-25 | 2007-01-31 | 郎丽红 | Autoclave for artificial quartz crystal |
| CN112442730A (en) * | 2019-08-29 | 2021-03-05 | 桂林百锐光电技术有限公司 | Device for growing large-size single crystal by temperature difference hydrothermal method |
-
1988
- 1988-08-05 JP JP63194338A patent/JPH0722692B2/en not_active Expired - Lifetime
-
1990
- 1990-02-03 CN CN90101411.7A patent/CN1022335C/en not_active Expired - Fee Related
- 1990-02-05 DE DE4003377A patent/DE4003377C1/de not_active Expired - Lifetime
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7081162B2 (en) | 2001-06-06 | 2006-07-25 | Nichia Corporation | Method of manufacturing bulk single crystal of gallium nitride |
| 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 |
| US7374615B2 (en) | 2001-06-06 | 2008-05-20 | Ammono.Sp.Zo.O | Method and equipment for manufacturing aluminum nitride bulk single crystal |
| US7422633B2 (en) | 2001-06-06 | 2008-09-09 | Ammono Sp. Zo. O. | Method of forming gallium-containing nitride bulk single crystal on heterogeneous substrate |
| US7057211B2 (en) | 2001-10-26 | 2006-06-06 | Ammono Sp. Zo.O | Nitride semiconductor laser device and manufacturing method thereof |
| US7132730B2 (en) | 2001-10-26 | 2006-11-07 | Ammono Sp. Z.O.O. | Bulk nitride mono-crystal including substrate for epitaxy |
| US7420261B2 (en) | 2001-10-26 | 2008-09-02 | 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 |
|---|---|
| CN1022335C (en) | 1993-10-06 |
| CN1053819A (en) | 1991-08-14 |
| DE4003377C1 (en) | 1991-08-08 |
| JPH0243939A (en) | 1990-02-14 |
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