JPH0243939A - Container for hydrothermal synthesis - Google Patents
Container for hydrothermal synthesisInfo
- Publication number
- JPH0243939A JPH0243939A JP63194338A JP19433888A JPH0243939A JP H0243939 A JPH0243939 A JP H0243939A JP 63194338 A JP63194338 A JP 63194338A JP 19433888 A JP19433888 A JP 19433888A JP H0243939 A JPH0243939 A JP H0243939A
- Authority
- JP
- Japan
- Prior art keywords
- container
- lid
- buffer chamber
- inner cylindrical
- 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.)
- Granted
Links
- 238000001027 hydrothermal synthesis Methods 0.000 title claims description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010931 gold Substances 0.000 claims abstract description 9
- 229910052737 gold Inorganic materials 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 239000012670 alkaline solution Substances 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 13
- 239000010970 precious metal Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 6
- 239000010453 quartz Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- GQWNECFJGBQMBO-UHFFFAOYSA-N Molindone hydrochloride Chemical compound Cl.O=C1C=2C(CC)=C(C)NC=2CCC1CN1CCOCC1 GQWNECFJGBQMBO-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 239000006262 metallic foam Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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)
Abstract
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。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a container for hydrothermal synthesis used in the production 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。(Conventional technology) An example of a conventional hydrothermal synthesis container is shown in FIG.
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内には種子人と原料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３５０〜４０
０℃、圧力１０００〜１５００ｋｙ／ｃ１！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。21 is a container body, 22 is a lid, 23 is a clamp, 24 is a convection control plate, 25 is a heater, and each 26 is a thermocouple. Seeds and raw material B are housed in the container body 21, and are immersed in a strong alkaline solution heated by a heater 25. Taking the case of artificial quartz as an example, the temperature is 350 to 40
0℃, pressure 1000-1500ky/c1! The container body 21 is made of a metal material with high strength, high toughness, and excellent corrosion resistance.
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って
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６Ｄ、種々の対策
がとられている。Products manufactured by hydrothermal synthesis are often used in fields such as electronics and optics, and there is a tendency for them to become smaller and thinner in the future, but the main factor that causes product quality to deteriorate is the contamination of foreign substances. be. In particular, the biggest problem is that the inner surface of the container body 21 is corroded by a strong alkaline solution, producing an iron compound called akumite, and Fe ions are mixed into the product.6D, various countermeasures have been taken.
一例として種子人の表面を隔離する方法があるが、十分
ではなく、又保鏝した面は成長が阻害されて生産効率が
低下する。One example is a method of isolating the surface of the seedlings, but this is not sufficient and the protected surface inhibits growth and reduces production efficiency.
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。Furthermore, the generation of Fe ions itself has been prevented by coating the inner surface of the container body 21 with silver, gold, platinum, etc., or by incorporating an inner cylindrical container made of the above-mentioned precious metals into the container body 21. There is.
（発明が解決しようとする課題）
容器本体２１の内面を、銀、金、白金等で被覆する場合
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
ある許シでなく、容器本体２１の構造によっては、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 silver, gold, platinum, etc., in order to ensure adhesion to the inner wall of the container body 21,
This type of container is very difficult to manufacture because it requires means such as hydraulic expansion or explosive bonding, and depending on the structure of the container body 21, it may cause problems in maintaining the sheet surface of the sealed area, and silver, gold, platinum, etc. When incorporating the inner cylinder container manufactured by the above method into the container body 21, it is necessary to equalize the pressure inside and outside the inner cylinder container so that unilateral external pressure does not act on the inner cylinder container. It is important to maintain the same ratio of liquid volume inside and outside the inner cylindrical container. However, the scope of application of both of the above is limited to small containers for experimental use.
（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
構成は次の通シである。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、該微小孔を被って蓋を
一面とし、他壁面にも微小孔を有する緩衝室を設けた水
熱合成用容器でおる。(Means for Solving the Problems) The present invention has been made in view of the above circumstances, and provides a large-sized hydrothermal synthesis container suitable for industrial use, the structure of which is as follows. . That is, the first invention provides a cylindrical gap inside a container body that is heated from the outside, and
A microhole is provided in the lid of the inner cylinder container, at least the inner surface of which is made of a precious metal such as silver, gold, platinum, etc., and a buffer chamber with micropores is provided on the other wall surface, covering the microhole and making the lid one side. Pour into a container for hydrothermal synthesis.
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、
該微小孔を被って蓋を一面とし、他壁面にも微小孔を有
する緩衝室を設けた水熱合成用容器に於て、緩貸室の空
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
溶液のめ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。Further, the second invention provides a lid of an inner cylindrical container which is housed with a cylindrical gap in a container body that is heated from the outside and whose at least the inner surface is made of a precious metal such as silver, gold, or platinum. ,
In a hydrothermal synthesis container that has a lid covering the micropores on one side and a buffer chamber having micropores on the other wall, the spatial volume of the loose chamber, the actual spatial volume of the cylindrical gap, and the interior The actual space volume of the cylindrical container was filled with an alkaline solution at a constant liquid volume ratio, and the concentration of the alkaline solution filled in the buffer chamber and the cylindrical gap was set to be thinner than the alkali concentration in the inner cylindrical container. This is a container for hydrothermal synthesis.
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。In both of the above inventions, the cylindrical gap between the container body and the inner cylindrical container may be filled with a breathable material having good thermal conductivity.
（作 用） 次に作用について説明する。(for production) Next, the effect 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。Seeds and raw materials are placed in the inner cylindrical container of a hydrothermal synthesis container, and 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
であるので、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, since at least the inner surface of the inner cylindrical container is made of precious metal, Fe ions are generated within the container body.
It does not affect the 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°Ｃ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。従って、内筒容器が歪んだり、破損する
ことがない。In addition, the cylindrical gap in the container body and the inside of the inner cylinder are communicated through micro holes provided in the lid of the inner cylinder and the wall of the buffer chamber, so the pressure inside and outside the inner cylinder is balanced, and the inner cylinder The container is not subjected to unilateral external pressure. Therefore, the inner cylinder container will not be 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
よって、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 space volume of the buffer chamber, the real space volume of the cylindrical gap, and the real space volume of the inner cylindrical container of the hydrothermal synthesis container are each filled with an alkaline solution at a constant liquid volume ratio, and the buffer chamber and By using the alkaline solution filled in the cylindrical gap at a lower concentration than the alkaline solution in the inner cylindrical container, the pressures in the cylindrical gap and in the inner cylindrical container are substantially balanced. Furthermore, when a pressure change occurs, the pressures within the cylindrical gap and within the inner cylindrical container are balanced through both micropores.
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シ、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っ
て種子への影響が更に軽減される。When the pressure inside the cylindrical gap increases, a small amount of alkaline solution containing Fe ions enters the buffer chamber through the micropores, but mixes with the alkaline solution in the buffer chamber and
Since the ions are diluted and enter the inner cylindrical container, the effect on the seeds is minimal.In addition, the concentration of the alkaline solution filled in the cylindrical gap is low, so the inner surface of the container body is less likely to be eroded. Combined with the reduction in the amount of ions generated, the impact on seeds 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。Furthermore, if the cylindrical gap is filled with an air-permeable substance having good thermal conductivity, heat transfer from the container body to the inner cylindrical container is improved, and the pressure in the cylindrical gap is maintained 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。(Example) An example of a container for hydrothermal synthesis according to the present invention will be described based on the drawings.
第１図に於て、１は外部から加熱される容器本体でちゃ
、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、バッキング２ａを介装して
、複数個のフランジ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 which is heated from the outside and is made of a metal material with 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 at a plurality of flanges 3 with a backing 2a interposed therebetween.
４は、有底筒状の内筒容器であシ、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っている。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４ ａｌ
を設けである。この微小孔４ ａｌは、圧力が作用しな
い状態では、表面張力によって自重では液体が流下しな
い大きさであシ、具体的には０．４ ［φ程度である。4 is a bottomed cylindrical inner cylindrical container made of a precious metal such as silver, gold, or platinum, or made of a material such as Ti (titanium) with a noble metal laminated on the inner surface. The removable lid 4a and bottom plate 4b of the inner cylindrical container are also made of the same material, and the lid 4a has a small hole 4 al approximately in the center as shown in detail in FIG.
This is provided. The micropores 4 al have a size that does not allow liquid to flow down under their own weight due to surface tension in a state where no pressure is applied, and specifically, the diameter is about 0.4 [φ.
そして、該容器の蓋４ａの上面に、微小孔４ ａｌを被
って箱形部材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０．４ ｍφ程度の微小孔５ｂを
設けである。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。Then, a box-shaped member 5a is fixed to the top surface of the lid 4a of the container, covering the micro-hole 4al to form a buffer chamber 5, and the top plate of the box-shaped member 5a also has a micro-hole of about 0.4 mφ. A hole 5b is provided. Note that the position of this microhole 5b is the same as that of the buffer chamber 5.
The position shall be higher than the level of the liquid being filled.
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。Further, at least the inner surface of the buffer chamber 5 is made of 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-mentioned structure is built into the container main body 1 with a cylindrical gap 1a provided therebetween.
６ａは内筒容器４内に設けられた対流制御板であり、６
ｂ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;
b is a convection control plate provided in the cylindrical gap 1a between the inner cylindrical container 4 and the main body 1. Seeds are stored above the convection control plate 6a in the inner cylindrical container 4, and raw materials are stored below. The volume and the actual space volume of the inner cylindrical container 4 are filled with alkaline solution at a constant liquid volume ratio, respectively, and the concentration of the alkaline solution filled in the buffer chamber 5 and the cylindrical gap 1a is determined by Set it lower than the alkaline concentration.
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 heated from the outside to perform hydrothermal synthesis.
次に作用を説明する。Next, the action will be explained.
緩衝室５は、微小孔５ｂを介して筒状間隙１ａと又微小
孔４ ａｌ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ｌａ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、或は加熱によって筒状間隙ｌａ
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ｌａ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 communicates with the cylindrical gap 1a via the microhole 5b and the inside of the inner cylindrical container 4 via the microhole 4al, so that the amount of liquid in the cylindrical gap la and the inner cylindrical container 4 are in communication with each other. If the amount of liquid in the cylindrical gap is slightly different from a constant ratio, or by heating, the amount of liquid in the cylindrical gap la
When a pressure difference is created between the inside and outside of the inner cylinder container 4 based on the difference between the liquid temperature inside the inner cylinder container 4 and the liquid temperature inside the inner cylinder container 4, the alkaline solution in the buffer chamber 5 will It moves into the gap la, and the balance between the internal and external pressures of the inner cylindrical container 4 is maintained.
又筒状間隙ｌａ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。In addition, the alkaline solution containing Fe ions in the cylindrical gap la is mixed with the alkaline solution in the buffer chamber 5, and then flows into the inner cylindrical container 4.
As it enters the interior, the Fe+ ions are diluted and their impact on the product is reduced.
又、筒状間隙ｌａ内のアルカリ溶液は、内筒容器４内の
アルカリ溶液よりも濃度を薄くしであるので、容器本体
１の侵餘度合が低下し、Ｆｅ イオンの発生が減少す
る。Furthermore, since the alkaline solution in the cylindrical gap la has a lower concentration than the alkaline solution in the inner cylindrical container 4, the degree of attack on the container body 1 is reduced, and the generation of Fe 2 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４ ａｌを被って
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０．４關φ程度の微小孔５′
ｂを設けである。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, covering the microhole 4al to form a buffer chamber 5', and the side plate above the liquid level also has a 0.4 mm diameter. Micropores of about 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, it is preferable that both the inner and outer surfaces of this buffer chamber 5' are made of noble metal.
このような緩衝室５′を設ければ、微小孔４ ａｌ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 イオンが稀
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 flowing through the microhole 4 al will mix with the alkaline solution in the buffer chamber 5', the Fe ions will be diluted, and the alkaline solution will flow into the inner cylinder container 4. Since it goes inside, it has almost the same 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Ｎ
ｉ金属発泡体を筒状間隙Ｉａ内に充填する。Further, since it is desired that the heat transfer between the container body 1 and the inner cylindrical container 4 be good, the width of the cylindrical gap 1a is large.
If heat transfer is poor, use a material that has good thermal conductivity, good air permeability, and a high coefficient of thermal expansion, such as N.
i Fill the cylindrical gap Ia with metal foam.
ここで、通気性を要求するのは、筒状間隙ｌａ内の均圧
を保持するためであシ、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, air permeability is required in order to maintain equal pressure within the cylindrical gap la, and a large coefficient of thermal expansion is required in order to maintain the inner wall of the container body 1 and the inner cylindrical container as the temperature rises. This is because the adhesion of No. 4 to the outer wall becomes better.
（発明の効果）
以上の説明によっ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 understood from the above explanation, 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, no Fe ions are generated from the inner cylindrical container itself in which the seeds are placed.
■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。■Although the inner cylindrical container is manufactured with a relatively thin wall, the internal and external pressures can be balanced, allowing stable operation without distortion or damage to the inner cylindrical container.
■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、円筒容器に対する外圧が高くなった場合に
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 generated when the container body is eroded by alkaline solution
When the external pressure on the cylindrical container becomes high, the ions are diluted with the alkaline solution in the buffer chamber and enter the inner cylindrical container, so that the influence of Fe 2 ions on the seeds becomes 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。■The alkaline solution that the container body comes into contact with has a low concentration, so it is possible to reduce the amount of Fe ions that are generated when the container body is eroded.
以上の結果、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った。As a result of the above, we are now able to supply products produced by hydrothermal synthesis, such as high-quality artificial quartz.
ｆｆ、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
器の善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、５ｂ、５’ｂ：微小孔、６ａ、６ｂ ：
対流制御板。
代理人弁理士 前 １）宏 之（ほか１名）第２図
第４図
第１図
２ａ
ａ
Ｃff, Figure 1 is a sectional view showing a half part of the embodiment of the container for hydrothermal synthesis according to the present invention, and Figure 2 is a sectional view of the main part showing the lid and buffer chamber of the inner cylindrical container of this embodiment. , FIG. 3 is a cross-sectional view of the main part showing another example of the structure of the inner cylinder container and the buffer chamber, and FIG.
The figure is a sectional view of a conventional hydrothermal synthesis container. 1: Container body, 1a: Cylindrical gap, 4: Inner cylindrical container, 4a:
Lid of inner cylinder container, 4a': microhole, 4b = bottom plate, 5, 5
': Buffer chamber, 5b, 5'b: Micropore, 6a, 6b:
Convection control board. Representative Patent Attorney 1) Hiroshi (and 1 other person) Figure 2 Figure 4 Figure 1 2a a C
Claims (3)
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
を被つて蓋を一面とし、他壁面にも微小孔を有する緩衝
室を設けたことを特徴とする水熱合成用容器。(1) A microhole is provided in the lid of an inner cylindrical container that is built into a container body that is heated from the outside with a cylindrical gap, and at least the inner surface is made of a precious metal such as silver, gold, or platinum. A container for hydrothermal synthesis characterized by having a lid covering one side with holes and a buffer chamber having micropores on the other wall.
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
被つて蓋を一面とし、他壁面にも微小孔を有する緩衝室
を設けた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 microhole is provided in the lid of the inner cylinder container, which is built into a container body that is heated from the outside with a cylindrical gap, and whose at least the inner surface is made of a precious metal such as silver, gold, or platinum. In a hydrothermal synthesis container that has a lid on one side and a buffer chamber with micropores on the other wall, the spatial volume of the buffer chamber, the actual spatial volume of the cylindrical gap, and the actual volume of the inner cylindrical container. In the spatial volume,
Fill each with alkaline solution at a constant liquid volume ratio,
A container for hydrothermal synthesis, characterized in that the concentration of the alkaline solution filled in the buffer chamber and the cylindrical gap is set to be lower than the alkali concentration in the inner cylindrical container.
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 container for hydrothermal synthesis according to claim 1 or 2, wherein the cylindrical gap between the container body and the inner cylindrical container is filled with an air-permeable substance having good thermal conductivity.
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 use in 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 use in hydrothermal synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0243939A true JPH0243939A (en) | 1990-02-14 |
| JPH0722692B2 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003063889A (en) * | 2001-08-24 | 2003-03-05 | Tokyo Denpa Co Ltd | Vessel for growing single crystal |
| JP2003511326A (en) * | 1999-10-06 | 2003-03-25 | ゼネラル・エレクトリック・カンパニイ | Crystalline gallium nitride and method of forming crystalline gallium nitride |
Families Citing this family (11)
| 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 |
| CN100453710C (en) | 2001-06-06 | 2009-01-21 | 波兰商艾蒙诺公司 | Process and apparatus for obtaining bulk monocrystalline gallium-containing nitride |
| PL207400B1 (en) | 2001-06-06 | 2010-12-31 | Ammono Społka Z Ograniczoną Odpowiedzialnością | Method of and apparatus for obtaining voluminous, gallium containing, monocrystalline nitride |
| WO2003035945A2 (en) | 2001-10-26 | 2003-05-01 | Ammono Sp. Zo.O. | Substrate for epitaxy |
| JP4097601B2 (en) | 2001-10-26 | 2008-06-11 | アンモノ・スプウカ・ジ・オグラニチョノン・オドポヴィエドニアウノシツィオン | Nitride semiconductor laser device and manufacturing method thereof |
| EP1514958B1 (en) | 2002-05-17 | 2014-05-14 | Ammono S.A. | Apparatus for obtaining a bulk single crystal using supercritical ammonia |
| PL225427B1 (en) | 2002-05-17 | 2017-04-28 | Ammono Spółka Z Ograniczoną Odpowiedzialnością | Light emitting element structure having nitride bulk single crystal layer |
| CN1297695C (en) * | 2003-04-25 | 2007-01-31 | 郎丽红 | High pressure still for artificial quartz crystal |
| JP4276627B2 (en) | 2005-01-12 | 2009-06-10 | ソルボサーマル結晶成長技術研究組合 | Pressure vessel for single crystal growth and method for producing the same |
-
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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003511326A (en) * | 1999-10-06 | 2003-03-25 | ゼネラル・エレクトリック・カンパニイ | Crystalline gallium nitride and method of forming crystalline gallium nitride |
| JP4942270B2 (en) * | 1999-10-06 | 2012-05-30 | モーメンティブ・パフォーマンス・マテリアルズ・インク | Crystalline gallium nitride and method of forming crystalline gallium nitride |
| JP2003063889A (en) * | 2001-08-24 | 2003-03-05 | Tokyo Denpa Co Ltd | Vessel for growing single crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0722692B2 (en) | 1995-03-15 |
| DE4003377C1 (en) | 1991-08-08 |
| CN1022335C (en) | 1993-10-06 |
| CN1053819A (en) | 1991-08-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH0243939A (en) | Container for hydrothermal synthesis | |
| ES2647215T3 (en) | Industrial steam generator for depositing an alloy coating on a metal strip | |
| JPH04120259A (en) | Method and device for producing equipment member by laser beam spraying | |
| CN101982563A (en) | Plasma treatment device | |
| DE29903296U1 (en) | Microreactor | |
| CN104891431A (en) | Production method of miniature alkali metal atom chamber unit | |
| WO2007030667A4 (en) | Batch processing chamber with removable heater | |
| US4727935A (en) | Heat exchanger and method for making same | |
| CN106086779A (en) | A kind of micro-or nano size circulation aperture cellular solid and preparation method thereof | |
| US5057286A (en) | Vessel for use in hydrothermal synthesis | |
| US11898748B2 (en) | Burners and additive manufacturing methods | |
| JP2003176197A (en) | Single crystal growing vessel | |
| KR920003914B1 (en) | Vessel for use in hydro thermal synthesis | |
| CN217173945U (en) | Silicon carbide crystal growth device | |
| JP2008243893A (en) | Substrate processing apparatus | |
| JPH06502448A (en) | Film forming device using evaporation in vacuum | |
| WO1995023769A1 (en) | Device for moulding articles from glass | |
| CN214810658U (en) | Synthetic cavity structure, assembly and tool | |
| US4596628A (en) | Method for manufacturing components of complex wall construction | |
| JPS62112781A (en) | Chemical vapor deposition apparatus | |
| JPH05335243A (en) | Liquid bubbling apparatus | |
| JP2003063889A (en) | Vessel for growing single crystal | |
| JPH0678171B2 (en) | How to observe soot | |
| JPH02245280A (en) | Production of fluid discharger and porous discharge part for immersed substrate treating device | |
| US20030127050A1 (en) | Chemical vapor deposition apparatus |