JPH01172297A - Production of organic single crystal - Google Patents
Production of organic single crystalInfo
- Publication number
- JPH01172297A JPH01172297A JP33168087A JP33168087A JPH01172297A JP H01172297 A JPH01172297 A JP H01172297A JP 33168087 A JP33168087 A JP 33168087A JP 33168087 A JP33168087 A JP 33168087A JP H01172297 A JPH01172297 A JP H01172297A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- organic
- organic single
- film thickness
- thickness
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 238000000034 method Methods 0.000 claims abstract description 53
- 230000003287 optical effect Effects 0.000 claims abstract description 7
- 239000012808 vapor phase Substances 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 claims abstract description 5
- 238000005092 sublimation method Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims description 9
- 150000002894 organic compounds Chemical class 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 16
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 239000011521 glass Substances 0.000 description 9
- YEKPNMQQSPHKBP-UHFFFAOYSA-N 2-methyl-6-nitrobenzoic anhydride Chemical compound CC1=CC=CC([N+]([O-])=O)=C1C(=O)OC(=O)C1=C(C)C=CC=C1[N+]([O-])=O YEKPNMQQSPHKBP-UHFFFAOYSA-N 0.000 description 7
- 239000000758 substrate Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000007738 vacuum evaporation Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 230000010365 information processing Effects 0.000 description 3
- 239000013081 microcrystal Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000004093 laser heating Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- IXYATCDSDHQBLY-UHFFFAOYSA-N n,n-diethyl-4-[2-(4-nitrophenyl)ethenyl]aniline Chemical compound C1=CC(N(CC)CC)=CC=C1C=CC1=CC=C([N+]([O-])=O)C=C1 IXYATCDSDHQBLY-UHFFFAOYSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/361—Organic materials
Landscapes
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (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］
本発明は良質の有機単結晶を必要とする産業分野、例え
ば光学、非線形光学、音響光学、情報処理、通信分野に
、十分使用可能な有機単結晶を提供することのできる有
機単結晶の製造法に関する。Detailed Description of the Invention [Industrial Field of Application] The present invention provides an organic single crystal that can be fully used in industrial fields that require high-quality organic single crystals, such as optics, nonlinear optics, acousto-optics, information processing, and communication fields. The present invention relates to a method for producing an organic single crystal that can provide a single crystal.
［従来の技術］
有機化合物の単結晶製造法には、大別して、（ア）気相
法（昇華法など）
（イ）溶融法〈ブリッジマン法など）
（つ）溶液法
がある。[Prior Art] Methods for producing single crystals of organic compounds can be roughly divided into (a) gas phase methods (sublimation method, etc.), (b) melting methods (Bridgeman method, etc.), and (1) solution methods.
（ア）気相法による直接の有機単結晶の作製は、一般に
有機化合物分子がランダムにガラスなどの基体に付着し
、無秩序な微結晶集合体しか得られず、このようにして
得られた微結晶集合体では光散乱が多く、光学用途とし
ては使用できない。(a) Direct production of organic single crystals by the gas phase method generally results in organic compound molecules randomly adhering to a substrate such as glass, resulting in only disordered microcrystal aggregates; Crystal aggregates cause a lot of light scattering and cannot be used for optical purposes.
それに比べて、（イ）溶融法は所望の場所に所望の大き
さと形、更に詳しくは、サブミクロンの膜厚制御をした
有機単結晶を作製するのに多用され、（つ）溶液法は、
より穏やかな条件下で結晶製造できること、広範な条件
設定が可能であること、及び比教的容易に大型単結晶が
得られるなどの特徴を有する。In comparison, (a) the melting method is often used to produce organic single crystals of a desired size and shape in a desired location, more specifically, with submicron film thickness control; (b) the solution method is
It has the characteristics of being able to produce crystals under milder conditions, being able to set a wide range of conditions, and being able to easily obtain large single crystals.
しかしながら、従来の溶融法あるいは溶液法は、精密な
膜厚制御が困難であり、溶融法あるいは溶液法の有機単
結晶製造では以下に述べるような問題点があった。However, with the conventional melting method or solution method, it is difficult to precisely control the film thickness, and the production of organic single crystals using the melting method or solution method has the following problems.
溶融法あるいは溶液法を単独で適用した場合、例えば光
学用途に利用するに都合の良い、平滑な面を有する所望
の精密な厚さの有機単結晶を製造することは非常に困難
であった。良質の有機単結晶を必要とする産業分野、例
えば光学、非線形光学、音響光学、情報処理、通信分野
では製造された有機単結晶を用いて各種機能素子を構成
するには、所望の精密な厚さの平滑面を有することが好
都合であり、そうでない場合には、切削、研磨といった
、精密な膜厚を得るには困難かつ生産性を低下させる工
程が必要であった。When a melt method or a solution method is applied alone, it is very difficult to produce an organic single crystal with a desired precise thickness and a smooth surface suitable for use in optical applications, for example. In industrial fields that require high-quality organic single crystals, such as optics, nonlinear optics, acousto-optics, information processing, and communication fields, it is necessary to obtain the desired precise thickness in order to construct various functional elements using manufactured organic single crystals. It is advantageous to have a smooth surface; otherwise, difficult and productivity-lowering processes such as cutting and polishing would be required to obtain a precise film thickness.
［発明が解決しようとする問題点］
本発明は、かかる従来技術における問題点を解決しよう
とするものであり、所望の精密な厚さの平滑な面を有し
、利用するに都合が良い良質の有機単結晶を製造するこ
とを目的とする。[Problems to be Solved by the Invention] The present invention aims to solve the problems in the prior art. The purpose is to produce organic single crystals.
［問題点を解決するための手段］
上記目的を達成するため本発明方法は下記の構成を有す
る。[Means for Solving the Problems] In order to achieve the above object, the method of the present invention has the following configuration.
「有機単結晶上に、該単結晶と同種の有機化合物を気相
法で堆積することにより、該有機単結晶上に成長単結晶
部分を付加することを特徴とする有機単結晶の製造法。``A method for producing an organic single crystal, which comprises adding a growing single crystal portion onto the organic single crystal by depositing an organic compound of the same type as the single crystal on the organic single crystal by a vapor phase method.
」
本発明の母体有機単結晶の結晶製造法は、公知の溶融法
と溶液法が適用可能である。即ち、溶融法はブリッジマ
ン法、ストックバーガー法などのるつぼ冷却法、チョク
ラルスキー法などの回転引上げ法、フローティング・ゾ
ーン法、ベルヌーイ法及びレーザ加熱結晶法などがある
。特に、ブリッジマン法及びその変法は有機物質の単結
晶を作製するのに多用される。また、加熱の方法として
、通常のヒーター加熱、高周波加熱の他、局所的加熱方
法としてレーザ加熱がある。” As the method for producing the host organic single crystal of the present invention, known melting methods and solution methods can be applied. That is, melting methods include a crucible cooling method such as the Bridgman method and the Stockberger method, a rotational pulling method such as the Czochralski method, a floating zone method, the Bernoulli method, and a laser heating crystallization method. In particular, the Bridgman method and its modifications are often used to produce single crystals of organic substances. In addition to heating methods such as normal heater heating and high frequency heating, laser heating is also available as a local heating method.
これら溶融結晶化法は、融液を冷却し、融点あるいは融
点以下で種子結晶の存在または非存在下に結晶を成長さ
せる方法であって、その制御は、温度をコントロールす
ることによって行われる。These melt crystallization methods are methods of cooling a melt and growing crystals at or below the melting point in the presence or absence of seed crystals, and are controlled by controlling the temperature.
その形状は、どのようなものであってもよく、例えば、
膜状、塊状などが挙げられ、また、どのような膜厚であ
ってもよい。The shape may be any shape, for example,
It may be in the form of a film or a lump, and may have any thickness.
また溶液法は（Ａ＞溶媒蒸発、（Ｂ）温度降下あるいは
（Ｃ）貧溶媒添加など有機化合物の溶解度の低下を利用
する。Further, the solution method utilizes a decrease in the solubility of an organic compound, such as (A>solvent evaporation, (B) temperature decrease, or (C) addition of a poor solvent).
上記の溶液法においても適当な種子結晶を用いても適用
可能である。The above solution method can also be applied using appropriate seed crystals.
溶融法と溶液法による単結晶の作製は、例えば無機結晶
、半導体、金属、セラミックス、ガラス、プラスチック
など結晶成長方位を制御する基体上、あるいは制御しな
い基体上で行ったものであっても良い。これら基体は必
要に応じて表面処理などの前処理を施したものであって
も良い。Single crystals may be produced by melting and solution methods on substrates that control crystal growth orientation, such as inorganic crystals, semiconductors, metals, ceramics, glass, and plastics, or on substrates that do not. These substrates may be subjected to pretreatment such as surface treatment, if necessary.
この様にして得られた母体有機単結晶は、へき開研磨な
ど平滑面を作製して用いる。あるいは、平滑性の良い表
面を有するものはそのまま用いてもよい。The base organic single crystal thus obtained is used after producing a smooth surface by cleavage polishing. Alternatively, those having a smooth surface may be used as is.
本発明の成長単結晶部分の製造法は、母体単結晶の結晶
性を、該母体単結晶上に形成される気相堆積薄膜に引継
ぐことにより単結晶を成長させんとする、いわゆるホモ
エピタキシャル成長技術によるものである。The method for manufacturing the grown single crystal portion of the present invention is a so-called homoepitaxial growth technique in which a single crystal is grown by inheriting the crystallinity of a host single crystal to a vapor-deposited thin film formed on the host single crystal. This is due to
気相法を用いれば、数μｍ以下、好ましくは５μｍ以下
、さらにはオングストロームオーダーの成長単結晶部分
の精密な膜厚制御が可能となる。If the vapor phase method is used, it is possible to precisely control the thickness of the grown single crystal portion on the order of several μm or less, preferably 5 μm or less, and even on the order of angstroms.
即ち、光学的モニターの併用によって有機単結晶の膜厚
を製造作業中に知ることができ、所望の膜厚に成長した
時点で気相法による堆積を停止すれば良い。That is, the film thickness of the organic single crystal can be known during the manufacturing process by using an optical monitor, and the vapor phase deposition can be stopped when the film has grown to the desired thickness.
有機系材料、とりわけ化合物分子の単結晶製造に関して
、この様な気相ホモエピタキシャル成長が可能であるこ
とを発見し、かつ、製造技術として利用可能なまでに発
展させたことは本発明の最も強調すべき点である。The most important feature of the present invention is the discovery that such vapor phase homoepitaxial growth is possible for the production of single crystals of organic materials, especially compound molecules, and the development of this method to the point where it can be used as a production technology. This is an important point.
用いる気相法としては、物理的方法の昇華法、真空蒸着
法、スパッター法、イオン・ビーム法及び分子ビーム法
などがある。そして化学的方法としてＣＶＤなどがある
。良質な有機単結晶を簡便に得る方法としては昇華法、
真空蒸着法が好ましい。The gas phase method used includes physical methods such as sublimation method, vacuum evaporation method, sputtering method, ion beam method, and molecular beam method. Chemical methods include CVD and the like. Sublimation method is a simple method to obtain high quality organic single crystals.
Vacuum deposition is preferred.
［実施例］
以下、実施例を用いて説明するが、本発明はこれらの例
によってなんらその効力を限定されることはない。[Examples] The present invention will be described below using Examples, but the effectiveness of the present invention is not limited by these Examples in any way.
実施例１
大きな２次非線形光学効果を有する有機材料の４′−二
トロペンジリデン−３−アセトアミノ−４−メトキシア
ニリン（ＭＮＢＡ）の微結晶５．０ｇを、２００ ｍｌ
のベンゼン／クロロホルム（体積比２：１）混合溶媒中
で、溶液結晶化法の１つであるスローエバポレーション
法により結晶化させた。Example 1 5.0 g of microcrystals of 4'-nitropenzylidene-3-acetamino-4-methoxyaniline (MNBA), an organic material having a large second-order nonlinear optical effect, was added to 200 ml.
Crystallization was performed in a mixed solvent of benzene/chloroform (volume ratio 2:1) by slow evaporation, which is one of the solution crystallization methods.
得られた結晶をエタノール／イソ・プロパツール（体積
比１：１）混合溶媒中で洗浄し、清浄なスライドグラス
上に乗せ、自然乾燥した。この結晶の大きさは最大のも
ので、約３ ｃｍ Ｘ Ｓ ｍｍ Ｘ数μｍ（タテ×ヨ
コ×厚さ）であった。偏光顕微鏡観察によってこの結晶
が単結晶であることがわかった。The obtained crystals were washed in a mixed solvent of ethanol/isopropanol (volume ratio 1:1), placed on a clean slide glass, and air-dried. The maximum size of this crystal was approximately 3 cm x S mm x several μm (vertical x horizontal x thickness). Observation using a polarized light microscope revealed that this crystal was a single crystal.
平滑な２面を有する２ｍｍＸ３ｍｍＸ５μｍの大きさの
単結晶をスライドグラス上に乗せたまま真空蒸着装置内
にセットし、１０’Ｔｏｒｒまで排気後、ＭＮＢＡを約
５００人の厚さに蒸着した。偏光顕微鏡観察により偏光
特性、透光性、均一性は蒸着前と変らないが、膜厚増大
による偏光色の変化が見られることから、ホモエピタキ
シャル成長していることがわかった。A single crystal with a size of 2 mm x 3 mm x 5 μm and having two smooth surfaces was placed on a slide glass in a vacuum evaporation apparatus, and after exhausting to 10' Torr, MNBA was evaporated to a thickness of about 500 mm. Observation using a polarized light microscope revealed that although the polarization properties, light transmittance, and uniformity remained the same as before vapor deposition, changes in the polarized light color due to the increase in film thickness were observed, indicating homoepitaxial growth.
実施例２
Ｍ Ｎ Ｂ Ａ ５ ｇを４００ ｍｌのアセトンから
スローエバポレーション法により結晶化させた。得られ
た１ ｃｍ Ｘ Ｓ ｍｍ Ｘ数百μｍの結晶は偏光顕
微鏡観察により単結晶であることがわかった。この単結
晶の広い面に平行にへき開が可能であった。Example 2 5 g of MNBA was crystallized from 400 ml of acetone by slow evaporation. The obtained crystal measuring 1 cm x S mm x several hundred μm was found to be a single crystal by observation with a polarizing microscope. Cleavage was possible parallel to the wide plane of this single crystal.
へき開によって、膜厚を約１２０μｍとした平滑な２面
を有する単結晶をスライドグラス上に乗せ昇華装置中に
セットし、この単結晶上に１０４Ｔｏｒｒ、１９０℃の
条件下で３０分かけて約２μｍの膜厚となるまで昇華法
によるＭＮＢＡの堆積を行った。偏光顕微鏡観察により
、堆積薄膜がホモエピタキシャル成長し、結晶全体が完
全な単結晶になっていることが確認された。By cleaving, a single crystal with two smooth sides with a film thickness of approximately 120 μm was placed on a slide glass and set in a sublimation device, and a film thickness of approximately 2 μm was deposited on this single crystal under conditions of 104 Torr and 190° C. for 30 minutes. MNBA was deposited by sublimation until the film thickness reached . Observation using a polarized light microscope confirmed that the deposited thin film had grown homoepitaxially, and the entire crystal had become a perfect single crystal.
比較例１
スライドグラスを真空蒸着装置内にセットし、１０ ’
Ｔ ｏ ｒ ｒまで排気後、ＭＮＢＡを５００人の厚
さに蒸着した。偏光顕微鏡観察で透光性の低い微結、品
の集合体であることがわかった。Comparative Example 1 A slide glass was set in a vacuum evaporation device and heated for 10'
After evacuation to Torr, MNBA was deposited to a thickness of 500 mm. Observation with a polarized light microscope revealed that it was a collection of fine particles with low translucency.
実施例３
ＭＮＢＡ （融点１８８℃）をスペーサーを介した間隔
５μｍの２枚のスライドグラス基体間に約１９０℃で溶
融して吸い上げる。次に空隙中のモザイク状微結晶を、
温度分布をもつ水平炉の中を５ｍｍ／ｈｒの速度で移動
させるという結晶化法を適用することによって、単結晶
化させた。Example 3 MNBA (melting point: 188°C) is melted at about 190°C and sucked up between two slide glass substrates separated by a spacer of 5 μm. Next, the mosaic microcrystals in the voids are
Single crystallization was performed by applying a crystallization method in which the material was moved at a speed of 5 mm/hr in a horizontal furnace with temperature distribution.
得られた単結晶上に、実施例１と同様にして真空蒸着に
よりＭＮＢＡの堆積を行った。その結果、″ホモエピタ
キシャル成長によって膜厚を増大し、単結晶をさらに成
長させることができた。MNBA was deposited on the obtained single crystal by vacuum evaporation in the same manner as in Example 1. As a result, we were able to increase the film thickness through homoepitaxial growth and further grow the single crystal.
実施例４
３次非線形光学材料として公知の４′−ジエチルアミノ
−４−ニトロスチルベン（ＤＥＡＮＳ。Example 4 4'-diethylamino-4-nitrostilbene (DEANS), which is known as a third-order nonlinear optical material.
融点１８２〜１８８℃）をスライドグラス間でスペーサ
ーを用いずに溶融結晶化法により結晶化させた。片面の
スライドグラスを剥離し、偏光顕微鏡観察により単結晶
であること、及びハイミクロン干渉膜厚計による膜厚測
定から、８ｍｍＸ３ｍｍＸ１．７μｍの薄膜単結晶であ
ることがわかった。次にこれを真空蒸着装置内にセット
し、ＤＥＡＮＳを約２００人魚着した。(melting point 182-188°C) was crystallized between glass slides by the melt crystallization method without using a spacer. The slide glass on one side was peeled off, and observation using a polarizing microscope revealed that it was a single crystal, and film thickness measurement using a high micron interference film thickness meter revealed that it was a thin single crystal film measuring 8 mm x 3 mm x 1.7 μm. Next, this was set in a vacuum evaporation apparatus, and about 200 mermaids of DEANS were applied.
偏光顕微鏡観察により、蒸着薄膜がホモエピタキシャル
成長し、膜厚が増大した単結晶を得たことを確認した。Observation using a polarized light microscope confirmed that the deposited thin film had grown homoepitaxially to obtain a single crystal with increased film thickness.
［発明の効果］
本発明によれば、所望の精密な厚さの平滑な面を有し、
利用するに都合が良い良質の有機単結晶を簡便に得るこ
とができる。従って、バルク結晶の切削、研磨といった
精密膜厚制御には不都合な、困難かつ生産性を低下させ
る工程を簡略化出来るので、たとえば光学、非線形光学
、音響光学、情報処理、通信などの産業分野で、これを
大いに活用出来る。[Effects of the Invention] According to the present invention, it has a smooth surface with a desired precise thickness,
High-quality organic single crystals that are convenient for use can be easily obtained. Therefore, it is possible to simplify the difficult and productivity-reducing processes that are inconvenient for precise film thickness control, such as cutting and polishing bulk crystals, so it can be used in industrial fields such as optics, nonlinear optics, acousto-optics, information processing, and communications. , you can make great use of this.
Claims (5)
気相法で堆積することにより、該有機単結晶上に成長単
結晶部分を付加することを特徴とする有機単結晶の製造
法。(1) Production of an organic single crystal, characterized in that a grown single crystal portion is added to the organic single crystal by depositing an organic compound of the same type as the single crystal on the organic single crystal by a vapor phase method. Law.
とを特徴とする特許請求の範囲第（１）項記載の有機単
結晶の製造法。(2) The method for producing an organic single crystal according to claim (1), wherein the grown single crystal portion has a thickness of 5 μm or less.
溶液結晶化法により得られるものであることを特徴とす
る特許請求の範囲第（１）項記載の有機単結晶の製造法
。(3) The method for producing an organic single crystal according to claim (1), wherein the organic single crystal is obtained by a melt crystallization method or a solution crystallization method of an organic compound.
とする特許請求の範囲第（１）項記載の有機単結晶の製
造法。(4) The method for producing an organic single crystal according to claim (1), wherein the organic compound is a nonlinear optical material.
特徴とする特許請求の範囲第（１）項記載の有機単結晶
の製造法。(5) The method for producing an organic single crystal according to claim (1), wherein the gas phase method is a vacuum evaporation method or a sublimation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33168087A JPH01172297A (en) | 1987-12-26 | 1987-12-26 | Production of organic single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33168087A JPH01172297A (en) | 1987-12-26 | 1987-12-26 | Production of organic single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01172297A true JPH01172297A (en) | 1989-07-07 |
| JPH058159B2 JPH058159B2 (en) | 1993-02-01 |
Family
ID=18246377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33168087A Granted JPH01172297A (en) | 1987-12-26 | 1987-12-26 | Production of organic single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01172297A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03294827A (en) * | 1990-04-13 | 1991-12-26 | Toray Ind Inc | Lamination type organic nonlinear optical crystal body and production thereof |
| US5554220A (en) * | 1995-05-19 | 1996-09-10 | The Trustees Of Princeton University | Method and apparatus using organic vapor phase deposition for the growth of organic thin films with large optical non-linearities |
| CN103757692A (en) * | 2014-01-13 | 2014-04-30 | 中南大学 | Preparation method of ordered organic semiconductor mono-crystal array film |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2564380Y2 (en) * | 1993-12-10 | 1998-03-09 | 大阪瓦斯株式会社 | Tightening torque confirmation fitting |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60166298A (en) * | 1984-02-10 | 1985-08-29 | Hitachi Ltd | Preparation of film |
| JPS6236095A (en) * | 1985-08-06 | 1987-02-17 | Nec Corp | Formation of organic thin film crystal |
-
1987
- 1987-12-26 JP JP33168087A patent/JPH01172297A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60166298A (en) * | 1984-02-10 | 1985-08-29 | Hitachi Ltd | Preparation of film |
| JPS6236095A (en) * | 1985-08-06 | 1987-02-17 | Nec Corp | Formation of organic thin film crystal |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03294827A (en) * | 1990-04-13 | 1991-12-26 | Toray Ind Inc | Lamination type organic nonlinear optical crystal body and production thereof |
| US5554220A (en) * | 1995-05-19 | 1996-09-10 | The Trustees Of Princeton University | Method and apparatus using organic vapor phase deposition for the growth of organic thin films with large optical non-linearities |
| WO1996037639A3 (en) * | 1995-05-19 | 1997-01-16 | Univ Princeton | Method and apparatus using organic vapor phase deposition for the growth of organic thin films with large optical non-linearities |
| CN103757692A (en) * | 2014-01-13 | 2014-04-30 | 中南大学 | Preparation method of ordered organic semiconductor mono-crystal array film |
| CN103757692B (en) * | 2014-01-13 | 2016-05-25 | 中南大学 | A kind of preparation method of ordered organic semiconductor monocrystalline array film |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH058159B2 (en) | 1993-02-01 |
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