本発明は、昇華精製装置に関するものである。 The present invention relates to a sublimation purification apparatus.
常温で固体状態の材料を加熱気化せしめて予め所定の昇華温度に設定した材料回収部にて昇華精製することにより高純度の精製物を得る昇華精製装置としては、例えば特許文献１に開示されるものがある。 For example, Patent Document 1 discloses a sublimation purification apparatus that obtains a high-purity purified product by heating and vaporizing a solid-state material at room temperature and sublimating and purifying it in a material recovery unit that has been set to a predetermined sublimation temperature in advance. There is something.
この特許文献１に開示される昇華精製装置は、気化した材料が流通する筒状体の内部に多段昇華プレートを設けたもので、この多段昇華プレートにより材料が昇華を繰り返すことで、高純度の精製物が得られるとされている。 The sublimation purification apparatus disclosed in Patent Document 1 is provided with a multi-stage sublimation plate inside a cylindrical body through which the vaporized material circulates. It is said that a purified product is obtained.
しかしながら、特許文献１に開示される昇華精製装置は、筒状体と多段昇華プレートとの間に間隙があり、この間隙は上下（筒状体の長手方向）に一直線に繋がっているため、不純物が上下に自由に移動でき、従って、この不純物により精製物が汚染されるおそれがある。 However, the sublimation purification apparatus disclosed in Patent Document 1 has a gap between the cylindrical body and the multistage sublimation plate, and this gap is connected in a straight line vertically (in the longitudinal direction of the cylindrical body). Can move freely up and down, and thus the impurities may contaminate the purified product.
また、精製した材料は筒状体の内周面と各プレートに付着するため、収率を上げるためには精製物を回収する際、プレートを取り出すだけでなく、筒状体の内周面からも回収する必要があるが、この場合、筒状体を切断する必要があり、筒状体を切断する際に筒状体の一部が精製物に混入するおそれがある。また、一回の精製作業毎に新たな筒状体に交換する必要がありコスト高となる。 In addition, since the purified material adheres to the inner peripheral surface of the cylindrical body and each plate, in order to increase the yield, not only the plate is removed when collecting the purified product, but also from the inner peripheral surface of the cylindrical body. However, in this case, it is necessary to cut the tubular body, and when the tubular body is cut, a part of the tubular body may be mixed into the purified product. Moreover, it is necessary to replace with a new cylindrical body for each refining operation, resulting in high costs.
本発明は、上記問題点を解決したものであり、不純物の混入を可及的に防止でき、高純度の精製物を筒状体を切断する必要なく容易に且つコスト安に収率良く得ることが可能な極めて実用性に秀れた昇華精製装置を提供するものである。 The present invention solves the above-mentioned problems, can prevent contamination of impurities as much as possible, and can easily obtain a high-purity purified product at a low cost without the need to cut a cylindrical body. It is intended to provide a sublimation purification apparatus with excellent practicality that can be used.
添付図面を参照して本発明の要旨を説明する。 The gist of the present invention will be described with reference to the accompanying drawings.
加熱部１が周囲に配設された外筒体２内に加熱気化せしめた有機材料を流通させることで所望の化合物を精製する昇華精製装置であって、前記外筒体２内に複数の内筒体３を軸方向に連設状態に設けて、この内筒体３内を前記有機材料が流通する材料流通部４に設定し、この材料流通部４に、この材料流通部４を開口部６を残して閉塞することで前記有機材料の流通を調整する整流板５を前記軸方向に複数設けて、前記内筒体３と前記整流板５とで前記有機材料の流通路を形成したことを特徴とする昇華精製装置に係るものである。 A sublimation purification apparatus for purifying a desired compound by circulating an organic material heated and vaporized in an outer cylindrical body 2 in which a heating unit 1 is disposed, and includes a plurality of inner cylinders in the outer cylindrical body 2. The cylindrical body 3 is provided in a continuous state in the axial direction, and the inside of the inner cylindrical body 3 is set as a material flow portion 4 through which the organic material flows, and the material flow portion 4 is opened to the material flow portion 4. A plurality of rectifying plates 5 for adjusting the flow of the organic material by closing the channel 6 in the axial direction, and the inner cylindrical body 3 and the rectifying plate 5 form a flow path for the organic material. The present invention relates to a sublimation purification apparatus characterized by
また、加熱部１が周囲に配設された外筒体２内に加熱気化せしめた有機材料を流通させることで所望の化合物を精製する昇華精製装置であって、前記外筒体２内に複数の内筒体３を軸方向に連設状態に設けて、この内筒体３内を前記有機材料が流通する材料流通部４に設定し、この材料流通部４に、この材料流通部４を開口部６を残して閉塞することで前記有機材料の流通を調整する整流板５を前記軸方向に複数設け、この各整流板５の前記開口部６は、一直線に連通せずに前記材料流通部４の一端開口側から他端開口側が見通せない形状及び配置で夫々設けて、前記内筒体３と前記整流板５とで前記有機材料の流通路を蛇行形成したことを特徴とする昇華精製装置に係るものである。 The heating unit 1 is a sublimation purification apparatus for purifying a desired compound by circulating an organic material heated and vaporized in an outer cylindrical body 2 disposed around the heating unit 1. The inner cylinder 3 is provided in a continuous state in the axial direction, the inside of the inner cylinder 3 is set as a material circulation part 4 through which the organic material circulates, and the material circulation part 4 is connected to the material circulation part 4. A plurality of rectifying plates 5 for adjusting the flow of the organic material by closing the openings 6 are provided in the axial direction, and the openings 6 of the respective rectifying plates 5 do not communicate with each other in a straight line. Sublimation purification characterized in that the organic material flow path is meanderingly formed by the inner cylindrical body 3 and the rectifying plate 5 provided in a shape and arrangement in which the other end opening side cannot be seen from one end opening side of the portion 4. It concerns the device.
また、加熱部１が周囲に配設された外筒体２内に加熱気化せしめた有機材料を流通させることで所望の化合物を精製する昇華精製装置であって、前記外筒体２内に複数の内筒体３を軸方向に連設状態に設けて、この内筒体３内を前記有機材料が流通する材料流通部４に設定し、この材料流通部４に、この材料流通部４を開口部６を残して閉塞することで前記有機材料の流通を調整する整流板５を前記軸方向に複数設け、隣り合う前記整流板５の前記開口部６同士が互いに前記軸方向で重ならないようにその形状及び配置を設定して、前記内筒体３と前記整流板５とで前記有機材料の流通路を蛇行形成したことを特徴とする昇華精製装置に係るものである。 The heating unit 1 is a sublimation purification apparatus for purifying a desired compound by circulating an organic material heated and vaporized in an outer cylindrical body 2 disposed around the heating unit 1. The inner cylinder 3 is provided in a continuous state in the axial direction, the inside of the inner cylinder 3 is set as a material circulation part 4 through which the organic material circulates, and the material circulation part 4 is connected to the material circulation part 4. A plurality of rectifying plates 5 that adjust the flow of the organic material by closing the openings 6 are provided in the axial direction so that the openings 6 of the adjacent rectifying plates 5 do not overlap each other in the axial direction. The sublimation purification apparatus is characterized in that the flow path of the organic material is meandered by the inner cylindrical body 3 and the rectifying plate 5 by setting the shape and arrangement thereof.
また、前記材料流通部４にのみ前記有機材料が流通するように構成したことを特徴とする請求項１〜３のいずれか１項に記載の昇華精製装置に係るものである。 Moreover, it comprised so that the said organic material might distribute | circulate only to the said material distribution part 4, It concerns on the sublimation refinement | purification apparatus of any one of Claims 1-3 characterized by the above-mentioned.
また、前記内筒体３を前記整流板５を挟んで連設したことを特徴とする請求項１〜４のいずれか１項に記載の昇華精製装置に係るものである。 5. The sublimation purification apparatus according to claim 1, wherein the inner cylindrical body 3 is continuously provided with the rectifying plate 5 interposed therebetween.
また、前記内筒体３に前記整流板５を一体に設けたことを特徴とする請求項１〜５のいずれか１項に記載の昇華精製装置に係るものである。 Moreover, the said baffle plate 5 was integrally provided in the said inner cylinder 3, It concerns on the sublimation refinement | purification apparatus of any one of Claims 1-5 characterized by the above-mentioned.
また、前記整流板５は、前記有機材料の流通上流側ほど密に配置し、流通下流側ほど疎に配置したことを特徴とする請求項１〜６のいずれか１項に記載の昇華精製装置に係るものである。 The sublimation purification apparatus according to any one of claims 1 to 6, wherein the rectifying plates 5 are arranged densely toward the upstream side of the organic material and sparsely arranged toward the downstream side of the organic material. It is related to.
また、前記整流板５は、耐熱性ガラス、耐熱性金属、セラミックス若しくはフッ素樹脂の少なくともいずれか１種を含むものであることを特徴とする請求項１〜７のいずれか１項に記載の昇華精製装置に係るものである。 Moreover, the said baffle plate 5 contains at least any 1 type of heat resistant glass, a heat resistant metal, ceramics, or a fluororesin, The sublimation refinement | purification apparatus of any one of Claims 1-7 characterized by the above-mentioned. It is related to.
また、前記整流板５にして前記有機材料が接触する面が、耐熱性ガラス、耐熱性金属、セラミックス若しくはフッ素樹脂の少なくともいずれか１種を含む材料で形成されていることを特徴とする請求項８記載の昇華精製装置に係るものである。 The surface of the rectifying plate 5 that is in contact with the organic material is formed of a material containing at least one of heat-resistant glass, heat-resistant metal, ceramics, or fluororesin. This relates to the sublimation purification apparatus according to 8.
また、前記内筒体３は、耐熱性ガラス、耐熱性金属、セラミックス若しくはフッ素樹脂の少なくともいずれか１種を含むものであることを特徴とする請求項１〜９のいずれか１項に記載の昇華精製装置に係るものである。 The sublimation purification according to any one of claims 1 to 9, wherein the inner cylinder 3 contains at least one of heat-resistant glass, heat-resistant metal, ceramics, or fluororesin. It concerns the device.
また、前記内筒体３にして前記有機材料が接触する面が、耐熱性ガラス、耐熱性金属、セラミックス若しくはフッ素樹脂の少なくともいずれか１種を含む材料で形成されていることを特徴とする請求項１０記載の昇華精製装置に係るものである。 In addition, the surface of the inner cylinder 3 that contacts the organic material is formed of a material containing at least one of heat-resistant glass, heat-resistant metal, ceramics, or fluororesin. Item 11. The sublimation purification apparatus according to Item 10.
また、前記加熱部１は、抵抗加熱装置、ランプヒーター若しくは誘導加熱装置の少なくともいずれか１種を含んで成ることを特徴とする請求項１〜１１のいずれか１項に記載の昇華精製装置に係るものである。 The sublimation purification apparatus according to any one of claims 1 to 11, wherein the heating unit 1 includes at least one of a resistance heating device, a lamp heater, and an induction heating device. It is concerned.
また、前記外筒体２内に一端側から他端側に向かって温度勾配を形成するように前記加熱部１を構成したことを特徴とする請求項１〜１２のいずれか１項に記載の昇華精製装置に係るものである。 Moreover, the said heating part 1 was comprised so that the temperature gradient might be formed in the said outer cylinder 2 toward the other end side from the one end side, The any one of Claims 1-12 characterized by the above-mentioned. This relates to a sublimation purification apparatus.
また、前記外筒体２内に設けられる前記有機材料の容器８に、この有機材料を加熱気化せしめる加熱機構を設けたことを特徴とする請求項１〜１３のいずれか１項に記載の昇華精製装置に係るものである。 14. The sublimation according to claim 1, wherein the organic material container 8 provided in the outer cylindrical body 2 is provided with a heating mechanism for heating and vaporizing the organic material. It relates to a purification device.
また、前記外筒体２と前記加熱部１との間に熱伝導性の外套管９を設けたことを特徴とする請求項１〜１４のいずれか１項に記載の昇華精製装置に係るものである。 The sublimation purification apparatus according to any one of claims 1 to 14, wherein a thermally conductive outer tube 9 is provided between the outer cylindrical body 2 and the heating unit 1. It is.
また、前記外筒体２は外気を侵入させない真空容器であり、一端側に不活性ガスを導入する不活性ガス導入口を設け、他端側に不活性ガスを排出する不活性ガス排出口を設けたものであることを特徴とする請求項１〜１５のいずれか１項に記載の昇華精製装置に係るものである。 The outer cylinder 2 is a vacuum container that does not allow outside air to enter, and is provided with an inert gas inlet for introducing an inert gas on one end side, and an inert gas outlet for discharging the inert gas on the other end side. It is provided, It concerns on the sublimation purification apparatus of any one of Claims 1-15 characterized by the above-mentioned.
また、前記外筒体２に、この外筒体２内を中真空状態若しくは高真空状態とする真空排気機構を設けたことを特徴とする請求項１６記載の昇華精製装置に係るものである。 17. The sublimation purification apparatus according to claim 16, wherein the outer cylinder 2 is provided with an evacuation mechanism for making the inside of the outer cylinder 2 in a medium vacuum state or a high vacuum state.
また、前記外筒体２の設置角度を任意に可変できるように構成したことを特徴とする請求項１〜１７のいずれか１項に記載の昇華精製装置に係るものである。 Moreover, it comprised so that the installation angle of the said outer cylinder 2 could be changed arbitrarily, It concerns on the sublimation refinement | purification apparatus of any one of Claims 1-17 characterized by the above-mentioned.
本発明は上述のように構成したから、不純物の混入を可及的に防止でき、高純度の精製物を筒状体を切断する必要なく容易に且つコスト安に収率良く得ることが可能な極めて実用性に秀れた昇華精製装置となる。 Since the present invention is configured as described above, it is possible to prevent contamination of impurities as much as possible, and it is possible to easily obtain a high-purity purified product at a low cost without the need to cut the cylindrical body. It will be a sublimation purification device with excellent practicality.
好適と考える本発明の実施形態（発明をどのように実施するか）を、本発明の作用を示して簡単に説明する。 The preferred embodiment of the present invention (how to carry out the invention) will be briefly described, showing the operation of the present invention.
外筒体２内を加熱部１により加熱し、材料流通部４の一部を目的の化合物を得るための所定の捕集温度に設定して材料回収部とし、他の部位を不純物が捕集される温度に設定した状態で、材料流通部４に加熱気化した有機材料を流通させることで、材料回収部において目的の化合物を昇華精製する。 The inside of the outer cylindrical body 2 is heated by the heating unit 1, and a part of the material circulation unit 4 is set to a predetermined collection temperature for obtaining a target compound to be a material recovery unit, and impurities are collected in other parts. The target compound is sublimated and purified in the material recovery unit by circulating the heated and vaporized organic material in the material distribution unit 4 in a state where the temperature is set.
即ち、例えば加熱部１により外筒体２に流通上流側を高温とする温度勾配を形成し、材料回収部の流通上流側に高温昇華点不純物捕集部を、流通下流側に低温昇華点不純物捕集部を夫々設け、昇華温度が異なる物質（有機化合物）を各部で昇華精製する。 That is, for example, the heating unit 1 forms a temperature gradient in the outer cylinder 2 at a high temperature on the upstream side of the distribution, a high temperature sublimation point impurity collecting unit on the upstream side of the material recovery unit, and a low temperature sublimation point impurity on the downstream side of the distribution. Each of the collection parts is provided, and substances (organic compounds) having different sublimation temperatures are purified by sublimation.
この際、材料流通部４に設けた複数の整流板５により、有機材料は材料流通部４を真っ直ぐに通過せず曲がりながら流通するため、流通経路が延伸される。従って、有機材料が流通路を形成する各部材の壁面（内筒体３の内周面及び整流板５の表裏面）に衝突し易くなり、それだけ昇華を起こし易い構造となり理論段数が増加し、各部で確実に目的の化合物及び不純物が夫々昇華精製せしめられ、よって、目的の化合物及び不純物が明確に分離した状態で精製されることになり、不純物の昇華温度が目的の化合物の昇華温度と近接しているような有機材料からも高純度の精製物を得ることが可能となる。 At this time, the plurality of rectifying plates 5 provided in the material distribution unit 4 allows the organic material to flow while being bent without passing straight through the material distribution unit 4, so that the distribution route is extended. Accordingly, the organic material is likely to collide with the wall surfaces (the inner peripheral surface of the inner cylinder 3 and the front and back surfaces of the rectifying plate 5) of each member forming the flow path, and the number of theoretical stages increases because the structure easily causes sublimation. The target compound and impurities are surely purified by sublimation in each part, so that the target compound and impurities are purified in a clearly separated state, and the sublimation temperature of the impurity is close to the sublimation temperature of the target compound. It is possible to obtain a purified product with high purity from such organic materials.
特に、例えば、各整流板５の開口部６を、一直線に連通せずに材料流通部４の一端開口側から他端開口側が見通せない形状及び配置で夫々設けたり、隣り合う整流板５の開口部６同士が互いに軸方向で重ならないようにその形状及び配置を設定したりした場合には、有機材料の流通路を蛇行形成でき、確実に有機材料が曲がりながら流通し一層昇華を起こし易い構造を実現できる。 In particular, for example, the openings 6 of the respective rectifying plates 5 are provided in shapes and arrangements that do not communicate with one straight line and the other end opening side cannot be seen from the one end opening side of the material flow portion 4, or the openings of the adjacent rectifying plates 5. When the shape and arrangement are set so that the parts 6 do not overlap each other in the axial direction, the flow path of the organic material can be formed in a meandering manner, and the organic material can be surely circulated while being bent and more easily sublimated. Can be realized.
更に、精製物は流通路を形成する内筒体３の内周面及び整流板５の表裏面に付着し、外筒体２には殆ど付着しないため、精製物の回収は、外筒体２内から内筒体３及び整流板５を取り出して回収すれば良く、収率は極めて高くなる。また、従来のように筒状体（外筒体２）を切断する必要がないため、それだけ精製作業が簡易となりコストを抑えることができ、また、切断時の不純物の混入も防止できることになる。 Furthermore, since the purified product adheres to the inner peripheral surface of the inner cylinder 3 and the front and back surfaces of the rectifying plate 5 forming the flow path, and hardly adheres to the outer cylinder 2, the purified product can be recovered by the outer cylinder 2. What is necessary is just to take out and collect | recover the inner cylinder 3 and the baffle plate 5 from the inside, and a yield will become very high. Further, since it is not necessary to cut the cylindrical body (outer cylindrical body 2) as in the prior art, the refining operation can be simplified and the cost can be reduced, and contamination of impurities at the time of cutting can be prevented.
また、整流板５は例えば流通下流側の低温昇華点不純物が逆流することを防ぐ仕切りにもなるため、それだけ不純物が混入し難く高純度の精製物を得ることが可能となる。 Moreover, since the rectifying plate 5 also serves as a partition that prevents the low-temperature sublimation point impurities on the downstream side of the flow from flowing back, for example, it is possible to obtain a high-purity purified product that is less likely to contain impurities.
従って、本発明は、不純物の混入を可及的に防止でき、高純度の精製物を筒状体を切断する必要なく容易に且つコスト安に収率良く得ることが可能なものとなる。 Therefore, according to the present invention, contamination of impurities can be prevented as much as possible, and a highly purified product can be obtained easily and at a low cost and in a high yield without the need to cut the cylindrical body.
本発明の具体的な実施例について図面に基づいて説明する。 Specific embodiments of the present invention will be described with reference to the drawings.
本実施例は、加熱部１が周囲に配設された外筒体２内に加熱気化せしめた有機材料を流通させることで所望の化合物を精製する昇華精製装置であって、前記外筒体２内に複数の内筒体３を軸方向に連設状態に設けて、この内筒体３内を前記有機材料が流通する材料流通部４に設定し、この材料流通部４に、この材料流通部４を開口部６を残して閉塞することで前記有機材料の流通を調整する整流板５を前記軸方向に複数設けて、前記内筒体３と前記整流板５とで前記有機材料の流通路を形成したものである。 The present embodiment is a sublimation purification apparatus for purifying a desired compound by circulating an organic material heated and vaporized in an outer cylindrical body 2 around which a heating unit 1 is disposed. A plurality of inner cylinders 3 are provided in a continuous state in the axial direction, and the inside of the inner cylinder 3 is set as a material distribution part 4 through which the organic material circulates. A plurality of rectifying plates 5 for adjusting the circulation of the organic material by closing the portion 4 with the opening 6 being closed are provided in the axial direction, and the circulation of the organic material is performed between the inner cylinder 3 and the rectifying plate 5. A road is formed.
具体的には、外筒体２は、外気を侵入させない一端部及び他端部が閉塞された筒状の真空容器であり、一端側に気化した有機材料を搬送するアルゴン、ヘリウム若しくは窒素等の不活性ガスを導入する不活性ガス導入口を設け、他端側に不活性ガスを排出する不活性ガス排出口を設けたものである。尚、外筒体２は石英ガラス製である。 Specifically, the outer cylindrical body 2 is a cylindrical vacuum container whose one end and the other end that do not allow the outside air to enter, are closed, such as argon, helium, or nitrogen that conveys the vaporized organic material to one end. An inert gas inlet for introducing an inert gas is provided, and an inert gas outlet for discharging the inert gas is provided on the other end side. The outer cylinder 2 is made of quartz glass.
本実施例においては、図１中の外筒体２の下端部側から内筒体３内（材料流通部４）を流通するように不活性ガスを所定の流量で導入し（矢印Ａ）、上端部側から排出する（矢印Ｂ）ように構成している。 In the present embodiment, an inert gas is introduced at a predetermined flow rate (arrow A) so as to circulate in the inner cylinder 3 (material circulation part 4) from the lower end side of the outer cylinder 2 in FIG. It discharges from the upper end side (arrow B).
この外筒体２には、真空排気機構が設けられ、外筒体２内（及び内筒体３内）を中真空状態、好ましくは高真空状態とすることができるように構成している。 The outer cylinder 2 is provided with a vacuum exhaust mechanism so that the inside of the outer cylinder 2 (and the inside of the inner cylinder 3) can be in a medium vacuum state, preferably a high vacuum state.
外筒体２の周囲には、外筒体２の外周面を囲繞するように環状の加熱部１を複数設けている。この加熱部１は、抵抗加熱装置、ランプヒーター若しくは誘導加熱装置の少なくともいずれか１種を含んで成るもので、本実施例においては抵抗加熱装置が採用されており、外筒体２内に一端側から他端側に向かって温度勾配を形成するように構成している。尚、加熱部１としては少なくとも室温から９５０℃程度まで加熱できるものを用いる。 A plurality of annular heating portions 1 are provided around the outer cylindrical body 2 so as to surround the outer peripheral surface of the outer cylindrical body 2. The heating unit 1 includes at least one of a resistance heating device, a lamp heater, and an induction heating device. In this embodiment, a resistance heating device is employed, and one end is provided in the outer cylinder 2. A temperature gradient is formed from the side toward the other end side. In addition, as the heating part 1, what can be heated at least from room temperature to about 950 ° C. is used.
本実施例においては、流通上流側となる図１中下端側を高温とする温度勾配を形成するように各抵抗加熱装置を制御する。具体的には、外筒体２の軸方向に沿って複数の環状の抵抗加熱装置を配設し、各抵抗加熱装置を流通上流側ほど高温で、流通下流側ほど低温で外筒体２（材料流通部４）を加熱するように構成している。 In the present embodiment, each resistance heating device is controlled so as to form a temperature gradient in which the lower end side in FIG. Specifically, a plurality of annular resistance heating devices are arranged along the axial direction of the outer cylinder 2, and each resistance heating device is heated at a higher temperature on the upstream side of the flow and at a lower temperature on the downstream side of the flow. The material distribution part 4) is configured to be heated.
尚、例えば図２に図示したように、外筒体２と加熱部１との間に熱伝導性の外套管９を設けても良い。この場合、材料流通部４の温度勾配をより滑らかにすることができ、昇華温度が近接する化合物を夫々明確に分離した形で精製できることになる。 For example, as shown in FIG. 2, a thermally conductive outer tube 9 may be provided between the outer cylinder 2 and the heating unit 1. In this case, the temperature gradient of the material distribution part 4 can be made smoother, and the compounds having close sublimation temperatures can be purified in a clearly separated form.
外筒体２内には、材料流通部４を形成する複数の内筒体３を軸方向に連設状態に設けている。また、最下端に位置する内筒体３内（外筒体２の下端面上）には、有機半導体材料としてのトリス−（８−ヒドロキシノリナト）アルミニウム（Ａｌｑ３）やバソキュプロイン（ＢＣＰ）などの有機材料が充填される容器８（坩堝状の有機材料蒸発源）を設けている。即ち、容器８を内筒体３内に設け、この容器８からの有機材料が外筒体２の内周面と内筒体３の外周面との間の空間部に流出せず、材料流通部４にのみ流通するように構成している。また、容器８には、有機材料を加熱気化せしめる加熱機構を設けている。In the outer cylinder 2, a plurality of inner cylinders 3 that form the material flow part 4 are provided in an axially connected state. Further, in the inner cylinder 3 positioned on the lowermost end (on the lower end surface of the outer cylinder 2), tris- (8-hydroxynorinato) aluminum (Alq3 ) or bathocuproine (BCP) as an organic semiconductor material, etc. A container 8 (crucible organic material evaporation source) is provided. That is, the container 8 is provided in the inner cylinder 3, and the organic material from the container 8 does not flow out to the space between the inner peripheral surface of the outer cylinder 2 and the outer peripheral surface of the inner cylinder 3. It is configured to circulate only in the section 4. The container 8 is provided with a heating mechanism that heats and vaporizes the organic material.
尚、材料流通部４の途中部において殆どの材料は昇華せしめられ最下流部（上端部）からは流出しないため、この材料流通部４の最下流部から外筒体２の内周面と内筒体３の外周面との間の空間部に有機材料が侵入することはほとんどない。 Since most of the material is sublimated in the middle part of the material circulation part 4 and does not flow out from the most downstream part (upper end part), the inner peripheral surface and the inner surface of the outer cylindrical body 2 from the most downstream part of the material circulation part 4. The organic material hardly enters the space between the outer peripheral surface of the cylindrical body 3.
内筒体３は、図１に図示したように、整流板５を挟んで連設している。即ち、本実施例においては、内筒体３と整流板５とを交互に連設して材料流通部４を構成している。 As illustrated in FIG. 1, the inner cylindrical body 3 is continuously provided with a rectifying plate 5 interposed therebetween. That is, in the present embodiment, the material circulation part 4 is configured by alternately connecting the inner cylinders 3 and the current plate 5.
この内筒体３と整流板５との連設部分の構造としては、可及的に内筒体３内から有機材料が外部に漏出し難い構造を採用するのが望ましい。例えば内筒体３の端部開口部と係合する係合部を設けて互いにずれにくい構成（ずれ幅を抑える構成）とすると良い。即ち、図３〜５に図示したように、整流板５の表裏面の外周部に夫々前記係合部としての、段部10を設けたり（図３）、外側に下り傾斜するテーパー部11を設けたり（図４）、内側に下り傾斜するテーパー部12を設ける（図５）と良い。本実施例においては、各整流板５に前記段部10を設けて有機材料の漏出を防止している。 As a structure of the continuous portion of the inner cylinder 3 and the current plate 5, it is desirable to adopt a structure in which the organic material is hardly leaked from the inner cylinder 3 to the outside as much as possible. For example, an engagement portion that engages with the end opening of the inner cylindrical body 3 may be provided so that they are not easily displaced from each other (configuration that suppresses the displacement width). That is, as shown in FIGS. 3 to 5, step portions 10 as the engaging portions are provided on the outer peripheral portions of the front and back surfaces of the rectifying plate 5 (FIG. 3), or a tapered portion 11 that is inclined downward is formed on the outer side. It is good to provide (FIG. 4), or to provide the taper part 12 which inclines and falls inside (FIG. 5). In this embodiment, each step plate 5 is provided with the step portion 10 to prevent leakage of the organic material.
また、図３〜５の例に限らず、例えば図６に図示したように、内筒体３と整流板５との連設部に略隙間なく被嵌される環状のずれ防止体25を用いて互いにずれない構成としても良い。図中符号26は、ずれ防止体25を支持する支持部である。 Further, not limited to the examples of FIGS. 3 to 5, for example, as illustrated in FIG. 6, an annular shift prevention body 25 that is fitted to the connecting portion of the inner cylinder 3 and the rectifying plate 5 without a substantial gap is used. It is also possible to adopt a configuration that does not shift from each other. Reference numeral 26 in the figure is a support portion that supports the slip prevention body 25.
また、図７に図示したように、外筒体２の内周面と内筒体３の外周面との間の空間部７（外筒体２の内径と内筒体３の外径のクリアランス）を狭くすることで、具体的には、内筒体３の肉厚の１／２未満とすることで、ずれ幅を抑制して有機材料が外部に漏出しない構成としても良い。 Further, as illustrated in FIG. 7, a clearance 7 between the inner peripheral surface of the outer cylindrical body 2 and the outer peripheral surface of the inner cylindrical body 3 (clearance between the inner diameter of the outer cylindrical body 2 and the outer diameter of the inner cylindrical body 3. ) Is narrowed, specifically, it may be configured to be less than ½ of the wall thickness of the inner cylindrical body 3 so as to suppress the shift width and prevent the organic material from leaking to the outside.
尚、整流板５を内筒体３により挟む構成でなく、整流板５を内筒体３内に一体に設ける構成としても良い。具体的には、図８，９に図示したように、内筒体３の内周面に整流板５を載置可能な載置段部13（図８）若しくは段部の内側をテーパー状とした載置テーパー段部14（図９）を周設し、この載置段部13若しくは載置テーパー段部14に整流板５を着脱自在に載置固定しても良い。また、この載置段部13若しくは載置テーパー段部14を内筒体３内に複数設けて内筒体３に複数の整流板５を設けられるようにすると内筒体３の本数を抑えることができる。 In addition, it is good also as a structure which provides the rectification | straightening board 5 integrally in the inner cylinder 3 instead of the structure which pinches | interposes the rectification | straightening board 5 with the inner cylinder 3. FIG. Specifically, as shown in FIGS. 8 and 9, the mounting step portion 13 (FIG. 8) on which the rectifying plate 5 can be placed on the inner peripheral surface of the inner cylinder 3 or the inside of the step portion is tapered. The mounting taper step portion 14 (FIG. 9) may be provided around the mounting step portion 13 or the mounting taper step portion 14 so that the rectifying plate 5 is detachably mounted. Further, if a plurality of mounting step portions 13 or mounting tapered step portions 14 are provided in the inner cylindrical body 3 so that a plurality of rectifying plates 5 can be provided in the inner cylindrical body 3, the number of the inner cylindrical bodies 3 can be suppressed. Can do.
各整流板５の開口部６は、一直線に連通せずに材料流通部４の一端開口側から他端開口側が見通せない形状及び配置で夫々設けている。言い換えると、隣り合う整流板５の開口部６同士が互いに軸方向で重ならないようにその形状及び配置を設定している。従って、内筒体３と整流板５とで形成される有機材料の流通路は蛇行状態となる。 The opening 6 of each rectifying plate 5 is provided in such a shape and arrangement that the other end opening side cannot be seen from the one end opening side of the material flow part 4 without communicating with one straight line. In other words, the shape and arrangement are set so that the openings 6 of the adjacent rectifying plates 5 do not overlap each other in the axial direction. Therefore, the flow path of the organic material formed by the inner cylinder 3 and the rectifying plate 5 is in a meandering state.
具体的には、図１０（ａ）に図示したように半月状の開口部６を整流板５の左右端部に交互に設けたり、更に特に高温部において流通経路を延伸するために図１１（ａ）に図示したように板体15を整流板５に複数突設したり、図１２に図示したように整流板５の外周寄り位置に等間隔で４つ設けた円状の開口部６を各整流板５で交互に９０度ずつ位相をずらして設けることで流通路を蛇行形成する。尚、図１０（ｂ）及び図１１（ｂ）は、図１０（ａ）及び図１１（ａ）の概略断面図である。本実施例においては図１２に図示したように円状の開口部６を各整流板５で交互に９０度ずつ位相をずらして設けることで流通路を蛇行形成している。 Specifically, as shown in FIG. 10 (a), half-moon shaped openings 6 are alternately provided at the left and right ends of the rectifying plate 5, or more particularly in order to extend the flow path in the high temperature portion, as shown in FIG. As shown in FIG. 12A, a plurality of plate bodies 15 project from the rectifying plate 5, or four circular openings 6 provided at equal intervals near the outer periphery of the rectifying plate 5 as shown in FIG. The flow paths are meandered by providing the current plates 5 alternately 90 degrees out of phase. 10B and 11B are schematic cross-sectional views of FIGS. 10A and 11A. In this embodiment, as shown in FIG. 12, the circular openings 6 are alternately provided by the rectifying plates 5 so as to be shifted in phase by 90 degrees to form a meandering flow path.
また、整流板５は、有機材料の高温側である流通上流側ほど密に配置し、低温側である流通下流側ほど疎に配置している。具体的には、図１３に図示したように、材料流通部４の上流側を高温昇華点不純物を捕集する高温昇華点不純物捕集部16に設定し、下流側を低温昇華点不純物を捕集する低温昇華点不純物捕集部17に設定し、その間を目的物たる精製物を捕集する材料回収部18に設定しており、この高温昇華点不純物捕集部16において、整流板５を低温昇華点不純物捕集部17における配置間隔より狭い配置間隔で配置し、この高温昇華点不純物捕集部16における昇華の機会を可及的に多くして材料回収部18において高温昇華点不純物が昇華することを可及的に防止している。 Further, the rectifying plates 5 are densely arranged on the upstream side of the organic material, which is the high temperature side, and are sparsely arranged on the downstream side, which is the low temperature side. Specifically, as shown in FIG. 13, the upstream side of the material flow part 4 is set to a high temperature sublimation point impurity collecting part 16 for collecting high temperature sublimation point impurities, and the downstream side is used to collect low temperature sublimation point impurities. The low temperature sublimation point impurity collecting unit 17 is set, and the material recovery unit 18 for collecting the purified product as a target object is set between them. In this high temperature sublimation point impurity collecting unit 16, the rectifying plate 5 is It is arranged at an arrangement interval narrower than the arrangement interval in the low temperature sublimation point impurity collecting unit 17, and the sublimation point impurity in the high temperature sublimation point impurity collecting unit 16 is increased as much as possible, so that the high temperature sublimation point impurity is present in the material recovery unit 18. Sublimation is prevented as much as possible.
整流板５の配置間隔は、内筒体３の内径などにもよるが、３０〜５０ｍｍ程度とするのが好ましい。更に高温昇華点不純物捕集部16では１０〜２０ｍｍ程度の間隔で密に配置すると特に好ましい。 Although the arrangement | positioning space | interval of the baffle plate 5 is based also on the internal diameter etc. of the inner cylinder 3, it is preferable to set it as about 30-50 mm. Further, it is particularly preferable that the high temperature sublimation point impurity collecting section 16 is densely arranged at intervals of about 10 to 20 mm.
また、整流板５で仕切られて上記各部が形成されるように加熱部１による加熱温度を制御すると共に整流板５の配置間隔及び内筒体３の長さを設定している。よって、各部が整流板５によって仕切られてそれだけ精製物への不純物の混入を防止できることになる。また、図１４に図示したように内筒体３と整流板５とを分解して精製物を回収する作業も容易となる。 Further, the heating temperature by the heating unit 1 is controlled so as to be partitioned by the rectifying plate 5 to form the above-described parts, and the arrangement interval of the rectifying plates 5 and the length of the inner cylindrical body 3 are set. Therefore, each part is partitioned by the rectifying plate 5, and the contamination of impurities into the purified product can be prevented accordingly. Further, as shown in FIG. 14, the work of recovering the purified product by disassembling the inner cylinder 3 and the current plate 5 is also facilitated.
内筒体３及び整流板５としては、パイレックス（登録商標）や石英ガラスのような耐熱性ガラス、ステンレス、タンタル、タングステン、モリブデン、チタンなどの耐熱性金属、アルミナ、ジルコニア、窒化ボロン、窒化ケイ素などのセラミックス若しくはフッ素樹脂のいずれか１種を含むものが採用される。本実施例においてはいずれも石英ガラス製のものが採用されている。 Examples of the inner cylinder 3 and the current plate 5 include heat-resistant glass such as Pyrex (registered trademark) and quartz glass, heat-resistant metals such as stainless steel, tantalum, tungsten, molybdenum, and titanium, alumina, zirconia, boron nitride, and silicon nitride. Those containing any one of ceramics or fluororesin such as are used. In this embodiment, quartz glass is used.
尚、全体を石英ガラス製とせずに、少なくとも有機材料が接触する面が上記材料で形成されるように（覆われるように）しても良い。 Note that, instead of being made entirely of quartz glass, at least the surface with which the organic material contacts may be formed (covered) with the above material.
また、本実施例においては、図１に図示したように外筒体２及び内筒体３（材料流通部４）を、水平面に対して垂直縦置状態で設けて、下端側から上端側に有機材料を流通させる構成としているが、これらを垂直縦置状態に限らず傾斜状態に設けても良い。また、所定の傾斜状態で固定する構成としても良いし、任意に傾斜角度を可変できる構成としても良い。 Further, in the present embodiment, as shown in FIG. 1, the outer cylinder 2 and the inner cylinder 3 (material circulation portion 4) are provided in a vertically vertical state with respect to the horizontal plane, and the lower end side to the upper end side. Although it is set as the structure which distribute | circulates an organic material, you may provide these in not only the vertical vertical state but an inclined state. Moreover, it is good also as a structure fixed in a predetermined inclination state, and it is good also as a structure which can change an inclination angle arbitrarily.
例えば、図１５に図示したように傾斜させた場合も、図１と同様に内筒体３同士は重力により密着するため有機材料の漏出は抑制される。 For example, even when tilted as shown in FIG. 15, the inner cylinders 3 are brought into close contact with each other by gravity as in FIG.
また、例えば低温昇華点不純物が材料回収部に落下する問題が生じる場合には、図１６に図示したように図１と上下を反転した構成とし、上端側から下端側へと有機材料を流通させることで落下の問題を防ぐことが可能となる。尚、この場合、容器８は、図１７に図示したように底面に突設した挿通管19から気化した有機材料が下方側へと移動するように構成し、最上端の内筒体３内に固定する。また、容器８を図１７のような構成とせずに、連設される複数の内筒体３と平行に通常の坩堝状の容器８を内装した筒状体を設け、この筒状体の上部と内筒体３の側周面とを連通せしめて気化した有機材料が材料流通部４に導入されるように構成しても良い。 Further, for example, when the problem that the low-temperature sublimation point impurities fall into the material recovery unit occurs, the configuration is reversed upside down from FIG. 1 as shown in FIG. 16, and the organic material is circulated from the upper end side to the lower end side. This makes it possible to prevent the problem of falling. In this case, the container 8 is configured such that the organic material evaporated from the insertion tube 19 projecting from the bottom surface as shown in FIG. 17 moves downward, and is placed in the innermost cylinder 3 at the uppermost end. Fix it. Further, the container 8 is not configured as shown in FIG. 17, but a cylindrical body in which a normal crucible-shaped container 8 is installed in parallel with the plurality of continuous inner cylinders 3 is provided, and an upper portion of the cylindrical body is provided. Further, the vaporized organic material may be introduced into the material circulation part 4 by communicating with the side peripheral surface of the inner cylinder 3.
また、内筒体３と整流板５の表面粗さを粗くすることでも不純物の落下を防ぐことができるが、ＪＩＳ Ｂ−０６０１；２００１における算術平均粗さＲａが１．６μｍ以上であることが好ましい。 Moreover, although the fall of an impurity can also be prevented by roughening the surface roughness of the inner cylinder 3 and the current plate 5, the arithmetic average roughness Ra in JIS B-0601; 2001 is 1.6 μm or more. preferable.
また、外筒体２及び内筒体３（材料流通部４）を、水平面に対して平行横置状態で設けた場合には、内筒体３と整流板５との間に隙間ができ、材料の漏出が起こる可能性があるため、複数の内筒体３（及び内筒体３に挟まれる整流板５）を外筒体２の一端面（流通上流側端面）に押し付ける押付機構を設けると良い。具体的には、例えば、図１８〜図２１に図示したように、スプリング20の付勢力を利用したり（図１８）、重り21の倒れ力を利用したり（図１９）、テーパー面24上の重り22の落ち込み力を利用したり（図２０）、マグネット23の反発力を利用した（図２１）押付機構を設けると良い。 Moreover, when the outer cylinder 2 and the inner cylinder 3 (material circulation part 4) are provided in a state of being placed parallel to the horizontal plane, a gap is formed between the inner cylinder 3 and the current plate 5; Since there is a possibility of material leakage, a pressing mechanism is provided that presses the plurality of inner cylinders 3 (and the current plate 5 sandwiched between the inner cylinders 3) against one end surface (the upstream end surface of the distribution) of the outer cylinder 2. And good. Specifically, for example, as shown in FIGS. 18 to 21, the biasing force of the spring 20 (FIG. 18), the falling force of the weight 21 (FIG. 19), It is preferable to provide a pressing mechanism using the falling force of the weight 22 (FIG. 20) or using the repulsive force of the magnet 23 (FIG. 21).
尚、上記任意に傾斜角度を可変できる構成とした場合には、外筒体２の長手方向端部にして管軸と直交する軸を中心に回転させて遠心力により隙間を無くしたりする構成としても良い。また、静電気を利用して隙間を無くす構成としても良い。 In addition, when it is set as the structure which can change the said inclination angle arbitrarily, as a structure which makes it rotate centering on the axis | shaft orthogonal to a pipe axis at the longitudinal direction edge part of the outer cylinder 2, and eliminates a clearance gap by centrifugal force Also good. Moreover, it is good also as a structure which eliminates a clearance gap using static electricity.
上述のように構成した本実施例に係る昇華精製装置を用いての昇華精製について説明する。昇華精製を行う際には、有機材料を加熱気化する前に、外筒体２内（内筒体３内を含む）を真空ベーキングし、その後、外筒体２内を大気に置換することなく有機材料を加熱気化せしめるのが好ましい。 Sublimation purification using the sublimation purification apparatus according to the present embodiment configured as described above will be described. When performing sublimation purification, the inside of the outer cylinder 2 (including the inside of the inner cylinder 3) is vacuum-baked before the organic material is vaporized by heating, and then the inside of the outer cylinder 2 is replaced with the atmosphere. The organic material is preferably vaporized by heating.
具体的には、加熱部１により外筒体２（材料流通部４）に流通上流側を高温とする温度勾配を形成し、材料流通部４の流通上流側から順に、高温昇華点不純物捕集部16、材料回収部18、低温昇華点不純物捕集部17を形成し、昇華温度が異なる物質（有機化合物）を各部で昇華精製する。 Specifically, the heating section 1 forms a temperature gradient in the outer cylinder 2 (material circulation section 4) at a high temperature on the upstream side of the distribution, and sequentially collects high temperature sublimation point impurities from the upstream side of the distribution of the material circulation section 4. A part 16, a material recovery part 18, and a low-temperature sublimation point impurity collecting part 17 are formed, and substances (organic compounds) having different sublimation temperatures are purified by sublimation.
この際、材料流通部４に設けた複数の整流板５により流通路が蛇行形成され、有機材料は材料流通部４を真っ直ぐに通過せず曲がりながら流通するため、流通経路が延伸される。従って、有機材料が流通路を形成する各部材の壁面（内筒体３の内周面及び整流板５の表裏面）に衝突し易くなり、それだけ昇華を起こし易い構造となり理論段数が増加し、各部で確実に目的の化合物及び不純物が夫々昇華精製せしめられ、よって、目的の化合物及び不純物が明確に分離した状態で精製されることになり、不純物の昇華温度が目的の化合物の昇華温度と近接しているような有機材料からも高純度の精製物を得ることが可能となる。 At this time, the flow path is meanderingly formed by the plurality of rectifying plates 5 provided in the material flow part 4, and the organic material flows without turning straight through the material flow part 4, so that the flow path is extended. Therefore, the organic material is likely to collide with the wall surfaces (the inner peripheral surface of the inner cylindrical body 3 and the front and back surfaces of the rectifying plate 5) of each member forming the flow path, and the number of theoretical stages increases because the structure easily causes sublimation. The target compound and impurities are surely purified by sublimation in each part, so that the target compound and impurities are purified in a clearly separated state, and the sublimation temperature of the impurity is close to the sublimation temperature of the target compound. It is possible to obtain a purified product with high purity from such organic materials.
更に、精製物は流通路を形成する内筒体３の内周面及び整流板５の表裏面に付着し、外筒体２には殆ど付着しないため、精製物の回収は、外筒体２内から内筒体３及び整流板５を取り出して分離させて回収すれば良く、収率は極めて高くなる。また、従来のように筒状体（外筒体２）を切断する必要がないため、それだけ精製作業が簡易となりコストを抑えることができ、また、切断時の不純物の混入も防止できることになる。 Furthermore, since the purified product adheres to the inner peripheral surface of the inner cylinder 3 and the front and back surfaces of the rectifying plate 5 forming the flow path, and hardly adheres to the outer cylinder 2, the purified product can be recovered by the outer cylinder 2. What is necessary is just to take out the inner cylinder 3 and the current plate 5 from the inside, separate them, and collect them, and the yield will be extremely high. Further, since it is not necessary to cut the cylindrical body (outer cylindrical body 2) as in the prior art, the refining operation can be simplified and the cost can be reduced, and contamination of impurities at the time of cutting can be prevented.
また、整流板５は例えば流通下流側の低温昇華点不純物が逆流することを防ぐ仕切りにもなるため、それだけ不純物が混入し難く高純度の精製物を得ることが可能となる。 Moreover, since the rectifying plate 5 also serves as a partition that prevents the low-temperature sublimation point impurities on the downstream side of the flow from flowing back, for example, it is possible to obtain a high-purity purified product that is less likely to contain impurities.
また、整流板５の間隔を適宜設定し、石英製の内筒体３及び整流板５を用いることで、一層良好な精製物を得ることが可能となる。 In addition, it is possible to obtain a better purified product by appropriately setting the interval between the rectifying plates 5 and using the quartz inner cylinder 3 and the rectifying plate 5.
従って、本実施例は、不純物の混入を可及的に防止でき、高純度の精製物を筒状体を切断する必要なく容易に且つコスト安に収率良く得ることが可能なものとなる。 Therefore, in this embodiment, it is possible to prevent the contamination of impurities as much as possible, and it is possible to easily obtain a high-purity purified product at a low cost and without a need to cut the cylindrical body.
本実施例の効果を裏付ける実験例について説明する。 An experimental example supporting the effect of the present embodiment will be described.
図２２の上側の写真は実際の実験装置（外筒体内に内筒体及び整流板を設けたもの）であり、下側のグラフはこの実験装置を用いてＡｌｑ３及びＢＣＰを昇華精製する際の加熱温度の詳細を示すものである。The upper photograph in FIG. 22 is an actual experimental apparatus (with an inner cylinder and a current plate provided in the outer cylinder), and the lower graph is when subliming and purifying Alq3 and BCP using this experimental apparatus. This shows the details of the heating temperature.
図２３は、整流板（バッフル）の配置間隔を（各整流板間は等間隔で）種々変えて得られた精製物の品質の比較結果を示すものである。低電圧であるほど高品質の精製物が得られたことを示す。尚、精製前とは精製前のＡｌｑ３であり、バッフル無とは整流板無しで精製したものであり、市販精製品とは、市販されている精製品のＡｌｑ３（純度＞９９．９％、ＥＬ用）である。これより、整流板の間隔は３０〜４０ｍｍに設定するのが好ましいことが確認できた。FIG. 23 shows the comparison results of the quality of purified products obtained by variously changing the arrangement interval of the baffle plates (equal intervals between the baffle plates). The lower the voltage, the higher the quality purified product was obtained. Note that “before purification” means Alq3 before purification, “without baffle” means purification without a baffle plate, and “purified product” refers to Alq3 (purity> 99.9%) of a commercially available purified product. , For EL). From this, it has confirmed that it was preferable to set the space | interval of a baffle plate to 30-40 mm.
図２４（材料はＡｌｑ３），２５（材料はＢＣＰ）は、前記精製前と、前記バッフル無と、整流板を４０ｍｍで等間隔に配置した装置を用いて精製したバッフル有と、整流板の間隔を４０ｍｍで等間隔に配置し更に高温昇華点不純物捕集部に相当する部分（図２２の写真のｆと材料との間）に整流板を２枚追加した装置を用いて精製した高温バッフル有と、前記市販精製品（図２４のみ）とで品質を比較した比較結果を示すものである。これより、高温昇華点不純物捕集部に密に整流板を配置することで、品質が向上することが確認できた。FIG. 24 (material is Alq3 ), 25 (material is BCP), before the purification, without the baffle, with baffle refined using a device in which current plates are arranged at equal intervals of 40 mm, High-temperature baffle refined using a device in which two rectifying plates are added to the portion corresponding to the high-temperature sublimation point impurity trapping part (between f and the material in the photograph in FIG. 22), which are arranged at regular intervals of 40 mm. The comparison result which compared quality with existence and the said commercial refined product (only FIG. 24) is shown. From this, it was confirmed that the quality was improved by densely arranging the rectifying plate in the high temperature sublimation point impurity collecting part.
図２６（材料はＡｌｑ３），２７（材料はＢＣＰ）は、ＳＵＳ製の整流板を４０ｍｍで等間隔に配置し更に高温昇華点不純物捕集部に相当する部分にＳＵＳ製の整流板を２枚追加した装置を用いて精製した高温バッフル有（ＳＵＳ製）と、石英（ガラス）製の整流板を４０ｍｍで等間隔に配置し更に高温昇華点不純物捕集部に相当する部分に石英（ガラス）製の整流板を、材料がＡｌｑ３の場合は３枚、ＢＣＰの場合は２枚追加した装置を用いて精製した高温バッフル有（石英製）とで品質を比較した比較結果を示すものである。これより、石英（ガラス）製の整流板を用いることで、品質が向上することが確認できた。26 (material is Alq3 ) and 27 (material is BCP), SUS rectifier plates are arranged at equal intervals of 40 mm, and SUS rectifier plates are arranged in a portion corresponding to the high temperature sublimation point impurity collecting part. High-temperature baffle (purchased by SUS) refined using the added device and quartz (glass) rectifying plates are arranged at equal intervals of 40 mm, and quartz (glass) is added to the portion corresponding to the high-temperature sublimation point impurity collecting part. 3) shows a comparison result of quality comparison with a high-temperature baffle (made of quartz) refined using a device in which three rectifier plates made of Alq3 and two in the case of BCP are added. . From this, it was confirmed that the quality was improved by using a rectifying plate made of quartz (glass).
図２８は、整流板のない従来法で精製したもの（バッフル無）の品質及び収率と、図２５の高温バッフル有の品質及び収率とを比較した比較結果を示すものである。従来法においては、複数回精製することで品質を向上させる（素子性能を向上させる）必要があり、それだけ収率が低下するが、本実施例に係る高温バッフル有では少ない精製回数で高品質のものが得られ、それだけ収率が良くなることが確認できた。 FIG. 28 shows a comparison result comparing the quality and yield of a product refined by a conventional method without a baffle (no baffle) and the quality and yield of the high temperature baffle shown in FIG. In the conventional method, it is necessary to improve the quality by refining multiple times (improve the device performance), and the yield decreases accordingly. However, with the high temperature baffle according to this example, high quality can be achieved with a small number of purifications. It was confirmed that the yield was improved.
以上から、本実施例に係る昇華精製装置によれば高品質の精製物を収率良く得ることが可能となることが確認できた。 From the above, it has been confirmed that the sublimation purification apparatus according to the present example makes it possible to obtain a high-quality purified product with good yield.
１ 加熱部
２ 外筒体
３ 内筒体
４ 材料流通部
５ 整流板
６ 開口部
８ 容器
９ 外套管DESCRIPTION OF SYMBOLS 1 Heating part 2 Outer cylinder 3 Inner cylinder 4 Material distribution part 5 Current plate 6 Opening part 8 Container 9 Outer tube
| Application Number | Priority Date | Filing Date | Title |
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| JP2009201958AJP5585977B2 (en) | 2009-09-01 | 2009-09-01 | Sublimation purification equipment |
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| JP2009201958AJP5585977B2 (en) | 2009-09-01 | 2009-09-01 | Sublimation purification equipment |
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| JP2011050853Atrue JP2011050853A (en) | 2011-03-17 |
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