JP2002220213A - Method for syntheszing iiib family nitrogen compound - Google Patents
Method for syntheszing iiib family nitrogen compoundInfo
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- JP2002220213A JP2002220213A JP2001010168A JP2001010168A JP2002220213A JP 2002220213 A JP2002220213 A JP 2002220213A JP 2001010168 A JP2001010168 A JP 2001010168A JP 2001010168 A JP2001010168 A JP 2001010168A JP 2002220213 A JP2002220213 A JP 2002220213A
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- Japan
- Prior art keywords
- nitrogen compound
- group iiib
- synthesizing
- nitrogen
- gallium
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、IIIＢ族窒素化合
物の合成方法に関するものである。[0001] The present invention relates to a method for synthesizing a Group IIIB nitrogen compound.
【０００２】[0002]
【従来の技術】半導体結晶を励起子ボーア半径程度に小
さくすると、量子サイズ効果を示すことがわかってい
る。励起子ボーア半径は、電子とホールが結合した状態
である励起子の空間的広がりを示す（数式１）。結晶の
サイズをこの倍の大きさ、つまり励起子ボーア半径の４
倍以下の直径にすると、量子サイズ効果により次のよう
な現象が観測されている。 バンドギャップエネルギーの増大 遷移確率の増大 非線型光学係数の増大 ホールバーニング また、量子サイズ効果ではないが、このような小さな結
晶では、体積当りの結晶欠陥によるエネルギーの増加が
大きいため、結晶中に欠陥が存在しにくく、結晶欠陥の
少ない結晶が得られることがわかっている。以上のよう
な現象は工業的に、 発光・吸収波長制御 発光輝度飽和レベルの向上 波長多重光記録 のような技術として利用できるため、発光デバイス、光
学デバイス、ディスプレイデバイス、光記録材料などへ
の応用が期待されている。2. Description of the Related Art It has been known that when a semiconductor crystal is reduced to about the exciton Bohr radius, a quantum size effect is exhibited. The exciton Bohr radius indicates the spatial spread of excitons in a state where electrons and holes are combined (Equation 1). The size of the crystal is twice as large, ie, the exciton Bohr radius of 4
When the diameter is twice or less, the following phenomenon is observed due to the quantum size effect. Increase in band gap energy Increase in transition probability Increase in non-linear optical coefficient Hole burning Also, although not a quantum size effect, in such a small crystal, the energy increase due to crystal defects per volume is large. It is known that crystals with few crystal defects can be obtained. The above phenomena can be used industrially as technologies such as emission / absorption wavelength control, enhancement of emission luminance saturation level, and wavelength division multiplexing optical recording, and application to light emitting devices, optical devices, display devices, optical recording materials, etc. Is expected.
【０００３】[0003]
【数１】 (Equation 1)
【０００４】しかしながら、これまでにこのような効果
が確認されているのは、II−VI族半導体の超微粒子によ
るものがほとんどであるため、信頼性および耐久性に問
題があった。またカドミウムやセレンといった環境汚染
物質を使用しているため、これに代わる材料が必要とさ
れてきた。II−VI族半導体に代わる材料として、窒化物
系半導体の微結晶合成の試みがなされている。とくに窒
化ガリウムは、熱分解により励起子ボーア半径である
２．５ｎｍすなわち直径では５ｎｍ程度の微結晶が形成
されることが知られている。例えば、トリオクチルアミ
ン中でガリウムイミドポリマー［Ｇａ（ＮＨ）3/2］nを
分解することで、フォトルミネッセンスを示すＧａＮ微
粒子が得られている（Appl. Phys. Lett. Vol. 785, N
o. 4, p. 478, 1999）。しかし、この熱分解物質は低温
で分解するため、取り扱いが非常に難しい。また結晶表
面をヘキサデシルアミンで処理するプロセスを設けなけ
ればならない。このような理由から量産時の歩留まりの
低下や製造コストの上昇をもたらす。本発明はこのよう
な問題点を解決する。However, most of such effects have been confirmed so far due to the use of ultrafine particles of II-VI group semiconductors, and thus have problems in reliability and durability. In addition, the use of environmental pollutants such as cadmium and selenium requires alternative materials. Attempts have been made to synthesize microcrystals of nitride-based semiconductors as materials that can replace II-VI group semiconductors. In particular, it is known that gallium nitride forms microcrystals having a exciton Bohr radius of 2.5 nm, that is, a diameter of about 5 nm by thermal decomposition. For example, gallium imide polymer [Ga (NH) 3/2 ] n is decomposed in trioctylamine to obtain GaN fine particles exhibiting photoluminescence (Appl. Phys. Lett. Vol. 785, N
o. 4, p. 478, 1999). However, since this pyrolysis material is decomposed at a low temperature, it is very difficult to handle. In addition, a process for treating the crystal surface with hexadecylamine must be provided. For these reasons, the yield during mass production is reduced and the manufacturing cost is increased. The present invention solves such a problem.
【０００５】すなわち本発明の目的は、製造コストを低
く抑えることができるとともに、容易にIIIＢ族窒素化
合物を合成することのできる方法を提供することにあ
る。That is, an object of the present invention is to provide a method capable of suppressing the production cost and easily synthesizing a group IIIB nitrogen compound.
【０００６】[0006]
【課題を解決するための手段】本発明は、少なくともII
IＢ族元素、窒素および炭素を含む化合物を、溶媒中で
加熱して分解することを特徴とするIIIＢ族窒素化合物
の合成方法を提供するものである。また本発明は、III
Ｂ族元素がガリウムであり、且つ生成されるIIIＢ族窒
素化合物が、窒化ガリウムである前記のIIIＢ族窒素化
合物の合成方法を提供するものである。また本発明は、
少なくともIIIＢ族元素、窒素および炭素を含む化合物
が、トリス（ジメチルアミノ）ガリウムである前記のII
IＢ族窒素化合物の合成方法を提供するものである。ま
た本発明は、溶媒が、トリオクチルアミンである前記の
IIIＢ族窒素化合物の合成方法を提供するものである。
また本発明は、励起子ボーア半径の４倍よりも小さい微
粒子であるIIIＢ族窒素化合物の合成方法を提供するも
のである。SUMMARY OF THE INVENTION The present invention provides at least II
An object of the present invention is to provide a method for synthesizing a group IIIB nitrogen compound, which comprises decomposing a compound containing a group IB element, nitrogen and carbon by heating in a solvent. The present invention also relates to III
An object of the present invention is to provide a method for synthesizing the above-mentioned group IIIB nitrogen compound in which the group B element is gallium and the generated group IIIB nitrogen compound is gallium nitride. The present invention also provides
The aforementioned II, wherein the compound containing at least a Group IIIB element, nitrogen and carbon is tris (dimethylamino) gallium.
It is intended to provide a method for synthesizing a Group IB nitrogen compound. Further, the present invention provides the above-mentioned, wherein the solvent is trioctylamine.
It is intended to provide a method for synthesizing a Group IIIB nitrogen compound.
The present invention also provides a method for synthesizing a group IIIB nitrogen compound which is fine particles smaller than four times the exciton Bohr radius.
【０００７】[0007]
【発明の実施の形態】本発明のIIIＢ族窒素化合物の合
成方法は、前記のように、少なくともIIIＢ族元素、窒
素および炭素を含む化合物を、溶媒中で加熱して分解す
ることを特徴としている。とくに、IIIＢ族元素がガリ
ウムであり、少なくともIIIＢ族元素、窒素および炭素
を含む化合物が、トリス（ジメチルアミノ）ガリウムで
あり、生成されるIIIＢ族窒素化合物が、窒化ガリウム
であるのが好ましい。また、本発明の合成方法に使用さ
れる溶媒としては、トリオクチルアミン、トリ−ｎ−オ
クチルホスフィンオキサイド等が挙げられる。BEST MODE FOR CARRYING OUT THE INVENTION The method for synthesizing a group IIIB nitrogen compound of the present invention is characterized in that, as described above, a compound containing at least a group IIIB element, nitrogen and carbon is decomposed by heating in a solvent. . In particular, the group IIIB element is preferably gallium, the compound containing at least the group IIIB element, nitrogen and carbon is tris (dimethylamino) gallium, and the group IIIB nitrogen compound produced is preferably gallium nitride. Examples of the solvent used in the synthesis method of the present invention include trioctylamine and tri-n-octylphosphine oxide.
【０００８】以下、少なくともIIIＢ族元素、窒素およ
び炭素を含む化合物としてトリス（ジメチルアミノ）ガ
リウム（以下ＴＤＭＡＧという）、IIIＢ族窒素化合物
として窒化ガリウム、溶媒としてトリオクチルアミン
（以下、ＴＯＡという）を用いて本発明の合成方法を説
明する。なお、本発明の合成方法は、これらに限定され
るものではない。Hereinafter, tris (dimethylamino) gallium (hereinafter referred to as TDMAG) is used as a compound containing at least a group IIIB element, nitrogen and carbon, gallium nitride is used as a group IIIB nitrogen compound, and trioctylamine (hereinafter referred to as TOA) is used as a solvent. The synthesis method of the present invention will be described. The synthesis method of the present invention is not limited to these.
【０００９】まず、ＴＤＭＡＧの合成について説明す
る。ＴＤＭＡＧは、従来用いられてきたガリウムイミド
ポリマーに比べ安定であるので好ましい。下記化学反応
式（１）により、ＴＤＭＡＧを合成することができる。First, the synthesis of TDMAG will be described. TDMAG is preferred because it is more stable than conventionally used gallium imide polymers. TDMAG can be synthesized by the following chemical reaction formula (1).
【００１０】[0010]
【化１】 Embedded image
【００１１】ジメチルアミノリチウム（以下、ＤＭＡＬ
という）と生成物のＴＤＭＡＧは反応性が高いので一連
の操作は全て不活性ガス雰囲気中で行うのがよい。グロ
ーブボックス内でＤＭＡＬと三塩化ガリウムを３：１の
モル比で秤量し、ｎ−ヘキサン中で攪拌しながら７２〜
１２０時間、具体的には９６時間以上反応させる。反応
温度は１０〜２５℃が好ましい。反応終了後ろ過を行
い、反応副生成物である塩化リチウムを取り除き、ＴＤ
ＭＡＧを取り出す。次に、下記化学反応式（２）によ
り、ＴＤＭＡＧをＴＯＡ中で熱分解する。Dimethylaminolithium (hereinafter referred to as DML)
) And the product TDMAG are highly reactive, so that all of the series of operations should be performed in an inert gas atmosphere. In a glove box, DMAL and gallium trichloride are weighed at a molar ratio of 3: 1, and stirred in n-hexane for 72-
The reaction is performed for 120 hours, specifically 96 hours or more. The reaction temperature is preferably from 10 to 25C. After completion of the reaction, filtration was performed to remove lithium chloride as a reaction by-product, and TD
Take out the MAG. Next, TDMAG is thermally decomposed in TOA according to the following chemical reaction formula (2).
【００１２】[0012]
【化２】 Embedded image
【００１３】この熱分解は、不活性ガス雰囲気中でＴＤ
ＭＡＧにＴＯＡを適量加え、６〜４８時間で３００〜３
５０℃の反応させることにより行う。具体的には２４時
間で３３０℃の熱分解反応が挙げられる。次に固体の分
解物質を分離し有機不純物を取り除くためｎ−ヘキサン
と無水メタノールで洗浄を数回行う。これにより、窒化
ガリウムを得ることができる。This thermal decomposition is carried out by TD in an inert gas atmosphere.
Add appropriate amount of TOA to MAG, 300 ~ 3 in 6 ~ 48 hours
The reaction is carried out at 50 ° C. Specifically, a thermal decomposition reaction at 330 ° C. for 24 hours can be mentioned. Next, washing is performed several times with n-hexane and anhydrous methanol to separate solid decomposed substances and remove organic impurities. Thereby, gallium nitride can be obtained.
【００１４】図１は、得られたサンプルのＸ線回折測定
の結果を示す図である。３５°付近のピークはzinc ble
nd構造の＜１１１＞面、あるいはWurtzite構造の＜１０
１＞によるものである。この結果だけでは結晶構造は確
定できないが、スペクトル半値幅は約５ｄｅｇであるこ
とから、これより平均粒径（直径）はScherrerの式を用
いると２〜３ｎｍと見積もられる。すなわち、ＧａＮの
励起子ボーア半径２．５ｎｍの４倍よりも小さな結晶が
合成されたことがわかる。なお、Scherrerの式は、下記
で示される。FIG. 1 is a diagram showing the results of X-ray diffraction measurement of the obtained sample. The peak around 35 ° is zinc ble
<111> plane of nd structure or <10> of Wurtzite structure
1>. Although the crystal structure cannot be determined from this result alone, the half-width of the spectrum is about 5 deg. Therefore, the average particle diameter (diameter) is estimated to be 2 to 3 nm using the Scherrer equation. That is, it is understood that a crystal smaller than four times the exciton Bohr radius of GaN of 2.5 nm was synthesized. The Scherrer equation is shown below.
【００１５】[0015]
【数２】 (Equation 2)
【００１６】次にこのサンプルの室温におけるフォトル
ミネッサンス（ＰＬ）および励起（ＰＬＥ）スペクトル
の測定結果を示す。図２は、ＰＬスペクトルの測定結果
を示す図である（励起波長：３２５ｎｍ）。波長４１０
ｎｍ（約３．０ｅＶ）、および４７０ｎｍ（約２．６ｅ
Ｖ）付近をピークとする二つの発光が観測されている。
波長４１０ｎｍのブロードなピークは過去の文献(J．Ph
ys．Chem. Solids 1970, Vol. 31, p. 707)よりβ−Ｇ
ａ2Ｏ 3によるものであることが分かっている。波長４７
０ｎｍ付近のブロードなピークは、後に示すＰＬＥスペ
クトルの結果から、ＧａＮによるものであることが分か
る。このＧａＮの発光は直接バンド間遷移による発光
（波長３６２ｎｍ）ではない。その起源は現時点では不
明であるが、窒素の欠陥や、合成時に混入してしまった
不純物、熱分解時の溶媒の分解によってできた有機物な
どが関与しているものと推測される。Next, a photole of this sample at room temperature was prepared.
Minesence (PL) and excitation (PLE) spectra
2 shows the measurement results. Fig. 2 shows the measurement results of the PL spectrum.
(Excitation wavelength: 325 nm). Wavelength 410
nm (about 3.0 eV), and 470 nm (about 2.6 eV).
Two light emission peaks near V) are observed.
The broad peak at a wavelength of 410 nm is described in the past literature (J. Ph.
ys. Chem. Solids 1970, Vol. 31, p. 707)
aTwoO ThreeIt is known to be due to Wavelength 47
The broad peak near 0 nm is the PLE spectrum shown later.
From the results of the vector, you can see that it is due to GaN
You. This GaN emission is due to direct interband transition.
(Wavelength 362 nm). Its origin is currently unclear
It is clear, but it was mixed in during the synthesis and the defect of nitrogen
Impurities, organic substances formed by the decomposition of solvents during thermal decomposition
It is presumed that they are involved.
【００１７】図３は、ＰＬＥスペクトルの測定結果を示
す図である。エミッション波長は４７９ｎｍで励起波長
をスキャンした。波長３６０ｎｍ（約３．４ｅＶ）付近
に吸収端がある。この吸収帯は、ＧａＮバンド端吸収に
よるものである。Wurtzite構造の場合、ＧａＮのバンド
端吸収波長は３６２ｎｍ（３．４１ｅＶ）、Zinc blend
構造の場合は約３８０ｎｍ（３．２〜３．３ｅＶ）と報
告されている。本実施の形態で測定された吸収端は、Wu
rtziteであれば測定誤差範囲内でバルクＧａＮの値と一
致している。Zinc blend構造であれば、量子サイズ効果
によりバンド端が２００〜３００ｍｅＶブルーシフトし
たと考えられる。FIG. 3 is a diagram showing the measurement results of the PLE spectrum. The emission wavelength was 479 nm and the excitation wavelength was scanned. There is an absorption edge near a wavelength of 360 nm (about 3.4 eV). This absorption band is due to GaN band edge absorption. In the case of the Wurtzite structure, the band edge absorption wavelength of GaN is 362 nm (3.41 eV), and Zinc blend
In the case of the structure, it is reported to be about 380 nm (3.2 to 3.3 eV). The absorption edge measured in the present embodiment is Wu
If it is rtzite, it matches the value of bulk GaN within the measurement error range. In the case of the Zinc blend structure, it is considered that the band edge has shifted blue by 200 to 300 meV due to the quantum size effect.
【００１８】このように、結晶構造は確定できないが、
ＰＬＥ測定による吸収端波長の値からＧａＮが合成され
ていることを示すことができる。また、Ｘ線回折ピーク
の半値幅から、結晶の平均粒径は２〜３ｎｍであること
も、すなわち励起子ボーア半径の４倍よりも小さいこと
も示すことができる。すなわち本発明の方法は、製造コ
ストを低く抑えることができるとともに、容易にIIIＢ
族窒素化合物を合成することができる。そして本発明の
方法で得られたIIIＢ族窒素化合物は、励起子ボーア半
径の４倍よりも小さい微粒子状のものである。なお、本
実施の形態ではIIIＢ族窒素化合物として窒化ガリウム
の場合について説明したが、この方法はＩｎ、Ａｌ、Ｂ
など多くのIIIＢ族金属元素の窒化物に応用できる。ま
た、ＴＤＭＡＧ結晶中にＸ｛Ｎ（ＣＨ3）2｝n（式中、
Ｘはドーピング元素を示し、ｎはドーピング元素の価数
を示す）を取り込むことで、発光センターやドナー、ア
クセプターイオンのドーピングをすることもできる。Thus, although the crystal structure cannot be determined,
The value of the absorption edge wavelength obtained by the PLE measurement can indicate that GaN is synthesized. Also, the half-width of the X-ray diffraction peak can indicate that the average grain size of the crystal is 2 to 3 nm, that is, smaller than four times the exciton Bohr radius. In other words, the method of the present invention can reduce the production cost and can easily prepare IIIB
A group nitrogen compound can be synthesized. The group IIIB nitrogen compound obtained by the method of the present invention is in the form of fine particles smaller than four times the exciton Bohr radius. In this embodiment, the case where gallium nitride is used as the group IIIB nitrogen compound has been described.
And many other group IIIB metal element nitrides. Further, in the TDMAG crystal, X {N (CH 3 ) 2 } n (where,
X represents a doping element, and n represents a valence of the doping element), whereby doping with a light-emitting center, a donor, or an acceptor ion can be performed.
【００１９】[0019]
【発明の効果】このように本発明によれば、製造コスト
を低く抑えることができるとともに、容易にIIIＢ族窒
素化合物を合成することのできる方法を提供することが
できる。また本発明の合成方法により合成された窒化物
微粒子は、II−IV族微粒子に比べ、環境に対する影響が
非常に少ない。さらに、本発明により得られた窒化物微
粒子を蛍光体に応用した場合、遷移確率の増大により、
通常の蛍光体に比べ輝度飽和レベルが大幅に向上し、粒
径変化による発光波長制御も可能である。さらにまた、
本発明により得られた窒化物微粒子を記録材料に応用し
た場合、ホールバーニングによる多値記録が可能となる
ため、干渉ピットや磁化状態、相変化等による記録方式
と比較して、大幅に記録密度を向上することができる。
また、本発明により得られた窒化物微粒子は、３次の非
線形光学係数の大きな材料を得ることができる。As described above, according to the present invention, it is possible to provide a method that can reduce the production cost and can easily synthesize a group IIIB nitrogen compound. Further, the nitride fine particles synthesized by the synthesis method of the present invention have very little influence on the environment as compared with the II-IV group fine particles. Furthermore, when the nitride fine particles obtained according to the present invention are applied to a phosphor, the transition probability increases,
The luminance saturation level is greatly improved as compared with ordinary phosphors, and the emission wavelength can be controlled by changing the particle size. Furthermore,
When the nitride fine particles obtained according to the present invention are applied to a recording material, multi-value recording by hole burning becomes possible, so that the recording density is significantly higher than the recording method using interference pits, magnetization state, phase change, etc. Can be improved.
Further, the nitride fine particles obtained by the present invention can obtain a material having a large third-order nonlinear optical coefficient.
【図１】実施の形態で得られたサンプルのＸ線回折測定
の結果を示す図である。FIG. 1 is a diagram showing a result of X-ray diffraction measurement of a sample obtained in an embodiment.
【図２】実施の形態で得られたサンプルのフォトルミネ
ッサンス（ＰＬ）スペクトルの測定結果を示す図であるFIG. 2 is a diagram showing a measurement result of a photoluminescence (PL) spectrum of a sample obtained in an embodiment.
【図３】実施の形態で得られたサンプルの励起（ＰＬ
Ｅ）スペクトルの測定結果を示す図である。FIG. 3 shows the excitation (PL) of the sample obtained in the embodiment.
E) It is a figure which shows the measurement result of a spectrum.
Claims (5)
素を含む化合物を、溶媒中で加熱して分解することを特
徴とするIIIＢ族窒素化合物の合成方法。1. A method for synthesizing a group IIIB nitrogen compound, comprising decomposing a compound containing at least a group IIIB element, nitrogen and carbon by heating in a solvent.
成されるIIIＢ族窒素化合物が、窒化ガリウムである請
求項１に記載のIIIＢ族窒素化合物の合成方法。2. The method for synthesizing a group IIIB nitrogen compound according to claim 1, wherein the group IIIB element is gallium, and the generated group IIIB nitrogen compound is gallium nitride.
素を含む化合物が、トリス（ジメチルアミノ）ガリウム
である請求項２に記載のIIIＢ族窒素化合物の合成方
法。3. The method for synthesizing a group IIIB nitrogen compound according to claim 2, wherein the compound containing at least a group IIIB element, nitrogen and carbon is tris (dimethylamino) gallium.
項３に記載のIIIＢ族窒素化合物の合成方法。4. The method for synthesizing a Group IIIB nitrogen compound according to claim 3, wherein the solvent is trioctylamine.
半径の４倍よりも小さい微粒子である請求項１〜４に何
れか１項記載のIIIＢ族窒素化合物の合成方法。5. The method for synthesizing a group IIIB nitrogen compound according to claim 1, wherein the group IIIB nitrogen compound is fine particles having a diameter smaller than four times the exciton Bohr radius.
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| JP2007077245A (en) * | 2005-09-13 | 2007-03-29 | Sharp Corp | Semiconductor phosphor particle and method for producing the same |
| JP4896126B2 (en) * | 2006-03-28 | 2012-03-14 | シャープ株式会社 | Group 13 nitride semiconductor phosphor and method for producing the same |
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