JP4139894B2 - Crystal production method and pattern formation method - Google Patents
Crystal production method and pattern formation method Download PDFInfo
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- JP4139894B2 JP4139894B2 JP2003328437A JP2003328437A JP4139894B2 JP 4139894 B2 JP4139894 B2 JP 4139894B2 JP 2003328437 A JP2003328437 A JP 2003328437A JP 2003328437 A JP2003328437 A JP 2003328437A JP 4139894 B2 JP4139894 B2 JP 4139894B2
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- 239000013078 crystal Substances 0.000 title claims description 42
- 238000000034 method Methods 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 230000007261 regionalization Effects 0.000 title description 4
- 230000007547 defect Effects 0.000 claims description 44
- 239000000758 substrate Substances 0.000 claims description 24
- 238000005468 ion implantation Methods 0.000 claims description 15
- 230000031700 light absorption Effects 0.000 claims description 10
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 description 11
- 238000011084 recovery Methods 0.000 description 7
- 238000004040 coloring Methods 0.000 description 6
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 230000002950 deficient Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005094 computer simulation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- -1 gold ions Chemical class 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
この発明は、非金属の結晶体の欠陥を回復する方法、欠陥部分と欠陥が回復された部分とを有する結晶体の作製方法、パターン形成方法、およびＸ線量の検出体に関する。 The present invention relates to a method for recovering a defect in a non-metallic crystal, a method for manufacturing a crystal having a defective portion and a portion in which a defect has been recovered, a pattern forming method, and an X-ray dose detector.
結晶の欠陥が無機材料の物性（光学特性や電気特性等）に与える影響については、古くから議論されており、結晶欠陥の制御は無機材料の物性を制御するために重要である。特に、人工格子材料やナノ構造材料は、幾何学的構造の僅かな変化によって物性が大きく変化する。例えば、最近、電界放出管等への応用が注目されているカーボンナノチューブ（ＣＮＴ）の場合も、物性の制御のために結晶欠陥を制御することが求められている。 The influence of crystal defects on the physical properties (optical properties, electrical properties, etc.) of inorganic materials has been discussed for a long time, and control of crystal defects is important for controlling the physical properties of inorganic materials. In particular, the properties of artificial lattice materials and nanostructured materials change greatly due to slight changes in geometric structure. For example, recently, in the case of carbon nanotubes (CNT) that are attracting attention for application to field emission tubes and the like, it is required to control crystal defects in order to control physical properties.
結晶欠陥の制御方法の従来例としては、加熱処理が挙げられる。例えば、下記の特許文献１には、シリコン基板にイオン注入法で不純物をドーピングしたことにより生じた格子欠陥を、熱処理により回復することが記載されている。
また、下記の非特許文献１には、ドーピングされたＧａＡｓのキャリア移動度がレーザー照射により回復された例について記載されている。
さらに、ＮＥＣのMiyamotoらのグループは、光や電子励起による結晶欠陥の回復をコンピュータシミュレーションによって実証する研究を進めており（非特許文献２参照）、この研究は世界的に注目を集めている。
Non-Patent Document 1 below describes an example in which the carrier mobility of doped GaAs is recovered by laser irradiation.
Furthermore, the group of Miyamoto et al. Of NEC is proceeding with research to prove the recovery of crystal defects by light and electronic excitation by computer simulation (see Non-Patent Document 2), and this research has attracted worldwide attention.
しかしながら、人工格子材料やナノ構造材料の結晶欠陥を回復するために熱処理法を採用すると、温度上昇に伴って幾何学的構造が大幅に変化して分解する恐れがある。また、光や電子励起による結晶欠陥の回復方法については、未だ研究段階であって、具体的な手法が確立されていない。
本発明の課題は、温度上昇を伴わずに結晶欠陥を回復できる方法と非金属の結晶欠陥を容易に制御できる方法を提供することにある。
However, if a heat treatment method is employed to recover crystal defects in artificial lattice materials and nanostructured materials, the geometric structure may change significantly as the temperature rises, causing decomposition. In addition, the crystal defect recovery method by light or electronic excitation is still in the research stage, and no specific method has been established.
An object of the present invention is to provide a method capable of recovering crystal defects without increasing the temperature and a method capable of easily controlling non-metallic crystal defects.
上記課題を解決するために、本発明の結晶欠陥の回復方法は、格子欠陥を有する非金属の結晶体に対してＸ線照射を行うことにより、前記欠陥を回復させることを特徴とする。
従来から知られているように、格子欠陥の無い、ほぼ完全な結晶体にＸ線照射を行うと、この結晶体に欠陥が導入される。本発明者は、このように欠陥を導入する作用が有るＸ線照射を、過剰な欠陥を有する非金属の結晶体に対して行うと、欠陥が回復することを見出した。
In order to solve the above problems, the crystal defect recovery method of the present invention is characterized in that the defect is recovered by performing X-ray irradiation on a nonmetallic crystal body having a lattice defect.
As conventionally known, when an almost complete crystal body having no lattice defects is irradiated with X-rays, defects are introduced into the crystal body. The present inventor has found that defects are recovered when X-ray irradiation having an effect of introducing defects is performed on a non-metallic crystal body having excessive defects.
本発明はまた、欠陥部分と欠陥が回復された部分とを有する結晶体を作製する方法であって、非金属の結晶体にイオン注入を行うことで欠陥を導入する工程と、前記工程で導入された欠陥をＸ線照射により回復する工程と、を備えたことを特徴とする結晶体の作製方
法を提供する。
本発明はまた、非金属の結晶体からなる基材の表面の所定領域にイオン注入を行った後に、前記所定領域に部分的にＸ線を照射して光吸収波長を変化させることにより、前記表面に光吸収波長の違いで識別されるパターンを形成する方法を提供する。
本発明はまた、非金属の結晶体からなる基材の表面にイオン注入による格子欠陥が導入されていることを特徴とするＸ線量の検出体を提供する。
The present invention is also a method of manufacturing a crystal body having a defective portion and a portion in which the defect has been recovered, the step of introducing a defect by ion implantation into a non-metallic crystal body, And a step of recovering the formed defect by X-ray irradiation.
In the present invention, after ion implantation is performed on a predetermined region of the surface of the base material made of a nonmetallic crystal, the predetermined region is partially irradiated with X-rays to change the light absorption wavelength. A method for forming a pattern identified by a difference in light absorption wavelength on a surface is provided.
The present invention also provides an X-ray dose detector characterized in that lattice defects due to ion implantation are introduced into the surface of a substrate made of a non-metallic crystal.
本発明の「結晶欠陥の回復方法」によれば、格子欠陥を有する非金属の結晶欠陥の回復を温度上昇を伴わずに行うことができる。
本発明の「結晶体の作製方法」によれば、イオン注入工程とＸ線照射工程とにより、欠陥部分と欠陥が回復された部分とを有する結晶体を容易に作製することができる。すなわち、非金属の結晶欠陥を容易に制御することができる。
本発明の「結晶体の作製方法」によれば、非金属の結晶体からなる基材の表面の所定領域にイオン注入を行った後に、前記所定領域に部分的にＸ線を照射して光吸収波長を変化させることにより、前記表面に光吸収波長の違いで識別されるパターンを形成することができる。
熱処理法では、微細な部分のみを温度上昇させることが困難であるが、イオン注入およびＸ線照射は微細な部分のみに行うことができるため、本発明の「パターン形成方法」によれば、微細なパターンを形成することができる。
According to the “crystal defect recovery method” of the present invention, it is possible to recover a nonmetallic crystal defect having a lattice defect without increasing the temperature.
According to the “crystal production method” of the present invention, a crystal having a defective portion and a portion in which a defect has been recovered can be easily produced by an ion implantation step and an X-ray irradiation step. That is, non-metallic crystal defects can be easily controlled.
According to the “crystal production method” of the present invention, after ion implantation is performed on a predetermined region on the surface of a substrate made of a non-metallic crystal, the predetermined region is partially irradiated with X-rays to generate light. By changing the absorption wavelength, a pattern identified by the difference in the light absorption wavelength can be formed on the surface.
In the heat treatment method, it is difficult to raise the temperature of only a fine part, but since ion implantation and X-ray irradiation can be performed only on a fine part, according to the “pattern formation method” of the present invention, Various patterns can be formed.
以下、本発明の実施形態について説明する。
図１を用いて、本発明の「パターン形成方法」の一実施形態を説明する。
先ず、図１（ａ）に示すように、酸化マグネシウム単結晶（非金属の結晶体）からなる基板（基材）１を用意する。この基板１は透明である。この基板１の表面の中央部分（所定領域）１２に、イオンビーム走査法によりイオン注入を行った。これにより、この部分が着色領域２となった。図１（ｂ）はこの状態を示す。イオン注入は、金（Ａｕ）イオンを用い、加速電圧：３．１ＭｅＶ、注入量：２×１０16ion／ｃｍ2の条件で行った。
Hereinafter, embodiments of the present invention will be described.
An embodiment of the “pattern formation method” of the present invention will be described with reference to FIG.
First, as shown in FIG. 1A, a substrate (base material) 1 made of a magnesium oxide single crystal (non-metallic crystal) is prepared. This substrate 1 is transparent. Ions were implanted into the central portion (predetermined region) 12 of the surface of the substrate 1 by an ion beam scanning method. Thereby, this portion became the colored region 2. FIG. 1B shows this state. Ion implantation was performed using gold (Au) ions under the conditions of acceleration voltage: 3.1 MeV and implantation amount: 2 × 10 16 ions / cm 2 .
次に、この基板１の着色領域２が形成された面に、中央に円形の孔を開けたマスクを載せた状態で、Ｘ線を照射した。Ｘ線照射は、３０ｋＶで加速した電子ビーム１２０ｍＡをロジウムターゲットに衝突させることよって発生させたＸ線を用い、ターゲットから２５ｍｍ離れた位置に基板１を配置して、１５分間行った。その結果、図１（ｃ）に示すように、着色領域２のＸ線が照射された円形部分の色が薄くなって、円形のパターン３が形成された。 Next, X-rays were irradiated on the surface of the substrate 1 on which the colored region 2 was formed with a mask having a circular hole in the center. X-ray irradiation was performed for 15 minutes using the X-ray generated by colliding an electron beam 120 mA accelerated at 30 kV with a rhodium target, placing the substrate 1 at a position 25 mm away from the target. As a result, as shown in FIG. 1C, the color of the circular portion irradiated with the X-rays of the colored region 2 was lightened, and a circular pattern 3 was formed.
すなわち、この実施形態のパターン形成方法では、基板が透明であり、イオン注入により基板の表面の所定領域が着色領域となっており、この着色領域に部分的にＸ線を照射することで、その部分の色が着色領域より薄くなっている。
ここで、パターン３の部分と、着色領域２の部分（パターン３から外れる部分）と、基板１の部分（着色領域２から外れる部分）について、光吸収スペクトルを測定した。その結果を図２に示す。図２のチャートから分かるように、波長５７５ｎｍ付近に中心を有するピークがＸ線照射により小さくなっている。
That is, in the pattern forming method of this embodiment, the substrate is transparent, and a predetermined region on the surface of the substrate is a colored region by ion implantation, and by partially irradiating the colored region with X-rays, The color of the part is lighter than the colored area.
Here, light absorption spectra were measured for the pattern 3 portion, the colored region 2 portion (the portion deviating from the pattern 3), and the substrate 1 portion (the portion deviating from the colored region 2). The result is shown in FIG. As can be seen from the chart of FIG. 2, a peak having a center near the wavelength of 575 nm is reduced by X-ray irradiation.
また、Ｘ線照射前の着色領域２の中央部分（Ｘ線照射によりパターン３となる部分）と、Ｘ線照射後のパターン３の部分について、断面をＴＥＭ（透過型電子顕微鏡）で観察した写真を図３および図４に示す。図３がＸ線照射前の写真であり、図４がＸ線照射後の写真である。これらの写真は、基板１の表面（パターン３の形成面）から深さ方向の所定位置（２．５ｍｍ程度）までの部分の断面写真であり、上側が基板１の表面側である。 Moreover, the photograph which observed the cross section about the center part (part which becomes the pattern 3 by X-ray irradiation) of the coloring area | region 2 before X-ray irradiation, and the part of the pattern 3 after X-ray irradiation by TEM (transmission electron microscope). Is shown in FIG. 3 and FIG. FIG. 3 is a photograph before X-ray irradiation, and FIG. 4 is a photograph after X-ray irradiation. These photographs are cross-sectional photographs of a portion from the surface of the substrate 1 (formation surface of the pattern 3) to a predetermined position in the depth direction (about 2.5 mm), and the upper side is the surface side of the substrate 1.
図３の写真と図４の写真を比較すると、図３の方は、基板の厚さ方向で複数層に分かれていて、表面側ほど粗い粒子状に写っているのに対して、図４の方は均一であることが分かる。すなわち、Ｘ線照射前の着色領域２を示す図３の写真では、格子欠陥が認められ、Ｘ線照射後のパターン部３を示す図４の写真では、格子欠陥の回復が認められる。
また、エネルギー分散型蛍光Ｘ線分析装置（ＥＤＸ）により、各断面を深さ方向に元素分析した。その結果を図５および図６に示す。図５が、Ｘ線照射前の着色領域２に相当する図３の点Ａ１〜Ａ１２での分析結果を示す。図６が、Ｘ線照射後のパターン部３に相当する図４の点Ｂ１〜Ｂ１２での分析結果を示す。
Comparing the photograph of FIG. 3 and the photograph of FIG. 4, FIG. 3 is divided into a plurality of layers in the thickness direction of the substrate and appears to be coarser particles on the surface side, whereas FIG. It can be seen that the direction is uniform. That is, in the photograph of FIG. 3 showing the colored region 2 before X-ray irradiation, lattice defects are recognized, and in the photograph of FIG. 4 showing the pattern portion 3 after X-ray irradiation, recovery of the lattice defects is recognized.
Each cross section was subjected to elemental analysis in the depth direction by an energy dispersive X-ray fluorescence analyzer (EDX). The results are shown in FIG. 5 and FIG. FIG. 5 shows the analysis results at points A1 to A12 in FIG. 3 corresponding to the colored region 2 before X-ray irradiation. FIG. 6 shows the analysis results at points B1 to B12 in FIG. 4 corresponding to the pattern portion 3 after X-ray irradiation.
この結果から、ＭｇＯ単結晶からなる基板１に金をイオン注入することにより、表面側に金の微粒子が集中的に形成され、この金の微粒子がＸ線照射により基板１全体に拡散されたと考えられる。
以上のことから、ＭｇＯ単結晶からなる透明な基板に金をイオン注入することにより、格子欠陥が形成されて、その部分が吸収波長５７５ｎｍ付近の色に着色され、その部分にＸ線を照射することにより、格子欠陥の回復と、これに伴う色の変化、イオン注入された原子の拡散が生じることが分かった。
From this result, it is considered that gold fine particles are formed intensively on the surface side by ion implantation of gold into the substrate 1 made of MgO single crystal, and the gold fine particles are diffused throughout the substrate 1 by X-ray irradiation. It is done.
From the above, by implanting gold ions into a transparent substrate made of MgO single crystal, lattice defects are formed, and the portion is colored in a color near the absorption wavelength of 575 nm, and the portion is irradiated with X-rays. As a result, it was found that recovery of lattice defects, color change accompanying this, and diffusion of ion-implanted atoms occur.
したがって、前述のように、イオン注入された単結晶に対して、形成するパターンに応じた部分にだけＸ線を照射することにより、光吸収波長の違いで識別される微細なパターンを形成することができる。また、形成されたパターン以外の部分に再度Ｘ線を照射すれば、この部分の光吸収波長（色）が形成されたパターンと同じになるため、形成されたパターンを消すことができる。
さらに、非金属の結晶体からなる基材の表面にイオン注入による格子欠陥が導入されていると、この格子欠陥の光吸収波長（基材表面の色）がＸ線照射によって変化するため、この基材はＸ線量の検出体として使用することができる。例えば、前記基材の表面にイオン注入を行って着色されたものは色の変化により、前記基材の表面にイオン注入を行っても人間の目で透明に見えるものは色が着くことにより、Ｘ線量が検出できる。
Therefore, as described above, a fine pattern identified by the difference in light absorption wavelength can be formed by irradiating the ion-implanted single crystal only with a portion corresponding to the pattern to be formed. Can do. Further, if the portion other than the formed pattern is irradiated again with X-rays, the light absorption wavelength (color) of this portion becomes the same as the formed pattern, so that the formed pattern can be erased.
Furthermore, if lattice defects due to ion implantation are introduced into the surface of a base material made of a non-metallic crystal, the light absorption wavelength (color of the base material surface) of the lattice defects changes due to X-ray irradiation. The substrate can be used as an X-ray dose detector. For example, those colored by ion implantation on the surface of the base material change in color, and those that appear transparent to the human eye even when ion implantation is performed on the surface of the base material are colored. X-ray dose can be detected.
なお、この実施形態では、図１（ｃ）に示す状態の基板１が、「欠陥部分と欠陥が回復された部分とを有する結晶体」に相当する。パターン３が「欠陥が回復された部分」に相当し、着色領域２のパターン３以外の部分が「欠陥部分」に相当する。
また、この実施形態ではＭｇＯ単結晶からなる基板を「基材」として用いているが、他の非金属の結晶体（多結晶を含む）からなるものであってもよいし、形状も板状に限定されない。
In this embodiment, the substrate 1 in the state shown in FIG. 1C corresponds to “a crystal body having a defective portion and a portion in which the defect has been recovered”. The pattern 3 corresponds to the “part where the defect has been recovered”, and the part other than the pattern 3 in the colored region 2 corresponds to the “defect part”.
In this embodiment, the substrate made of MgO single crystal is used as the “base material”, but it may be made of other non-metallic crystal (including polycrystal), and the shape is also plate-like. It is not limited to.
結晶材料の格子欠陥は、電気的特性および光学的特性に大きな影響を及ぼすので、本発明の結晶欠陥の回復方法は、カーボンナノチューブなどを利用したディスプレー装置、高速スイッチィング素子等の電子デバイスの性能向上に役立つ。また、本発明のパターン形成方法は、高密度光メモリー、光ディスク、光学素子への応用等、情報、通信産業での利用が考えられる。 Since lattice defects of crystal materials have a great influence on electrical and optical characteristics, the crystal defect recovery method of the present invention is based on the performance of electronic devices such as display devices using carbon nanotubes, high-speed switching elements, etc. Helps improve. The pattern forming method of the present invention can be used in the information and communication industries, such as application to high-density optical memories, optical disks, and optical elements.
１ 基板（基材）
１２ 基板の表面の中央部分（所定領域）
２ 着色領域
３ パターン
1 Substrate (base material)
12 Central part of substrate surface (predetermined area)
2 Coloring area 3 Pattern
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003328437A JP4139894B2 (en) | 2003-09-19 | 2003-09-19 | Crystal production method and pattern formation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP2003328437A JP4139894B2 (en) | 2003-09-19 | 2003-09-19 | Crystal production method and pattern formation method |
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