JPH06180400A - Sample capsule for x-ray microscope - Google Patents
Sample capsule for x-ray microscopeInfo
- Publication number
- JPH06180400A JPH06180400A JP4332024A JP33202492A JPH06180400A JP H06180400 A JPH06180400 A JP H06180400A JP 4332024 A JP4332024 A JP 4332024A JP 33202492 A JP33202492 A JP 33202492A JP H06180400 A JPH06180400 A JP H06180400A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- ray
- capsule
- spacer
- soft
- 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.)
- Pending
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は観察試料を装填するＸ線
顕微鏡用試料カプセルに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample capsule for an X-ray microscope for loading an observation sample.
【０００２】[0002]
【従来の技術】試料を収納してＸ線顕微鏡で生体観察を
行うための試料カプセルが知られている（例えば、特開
昭６３−２６３５００号公報、特開昭６３−２９８２０
０号公報参照）。2. Description of the Related Art Sample capsules are known for accommodating a sample and observing a living body with an X-ray microscope (for example, JP-A-63-263500 and JP-A-63-29820).
No. 0 publication).
【０００３】図４は軟Ｘ線を用いるＸ線顕微鏡の概要を
示し、図５（ａ），（ｂ）は、種々の材料における軟Ｘ
線の波長と線吸収係数との関係を示す。軟Ｘ線は、Ｘ線
と呼ばれる波長１ｐｍ〜１０ｎｍの領域の電磁波の内の
通常は２００ｐｍ以上の波長を有するものとされ、波長
４００〜８００ｎｍの可視光線よりも２桁以上も短い波
長の電磁波である。また、この軟Ｘ線は通過する物質に
よく吸収される。種々の物質内における光路単位長さ当
りの軟Ｘ線の吸収率、すなわち線吸収係数は、物質の密
度に比例し、一般的には波長が長くなる程高くなる。ま
た軟Ｘ線は、図５（ａ），（ｂ）に示すように、各物質
の分子構造に応じて線吸収係数が低い波長領域をいくつ
か有している。FIG. 4 shows an outline of an X-ray microscope using soft X-rays, and FIGS. 5A and 5B show soft X-rays in various materials.
The relationship between the wavelength of a line and a linear absorption coefficient is shown. Soft X-rays are usually electromagnetic waves having a wavelength of 200 pm or more among electromagnetic waves in the wavelength range of 1 pm to 10 nm called X-rays, and are electromagnetic waves having a wavelength two or more digits shorter than visible light having a wavelength of 400 to 800 nm. is there. Further, this soft X-ray is well absorbed by the substance passing through. The absorption rate of soft X-rays per unit length of the optical path in various substances, that is, the linear absorption coefficient, is proportional to the density of the substance, and generally increases as the wavelength increases. Further, as shown in FIGS. 5 (a) and 5 (b), the soft X-ray has some wavelength regions with low linear absorption coefficient depending on the molecular structure of each substance.
【０００４】図４において、Ｘ線発生器１の出力光軸上
にコンデンサー光学系２、試料容器３、結合光学系４、
撮像装置５が直列に配置される。なお、Ｘ線発生器１か
ら撮像装置５までのＸ線光学系の光路長は約２ｍであ
る。また、この光学系全体は排気系６を有する真空槽７
に収納されている。In FIG. 4, a condenser optical system 2, a sample container 3, a coupling optical system 4, are arranged on the output optical axis of the X-ray generator 1.
The image pickup devices 5 are arranged in series. The optical path length of the X-ray optical system from the X-ray generator 1 to the image pickup device 5 is about 2 m. The entire optical system is a vacuum chamber 7 having an exhaust system 6.
It is stored in.
【０００５】観察試料を装填した試料カプセル８を試料
容器３内にセットした後、排気系６により真空槽７内を
真空排気し、真空度を４．８×１０-2Ｐａ以下に維持し
た状態で観察を行う。Ｘ線発生器１から射出された軟Ｘ
線ビームはコンデンサー光学系２により収束され、試料
容器３にセットされた試料カプセル８を通過する。観察
試料を通過した軟Ｘ線は結像光学系４により撮像装置５
へ導かれ、撮像装置５上に観察像を結像する。撮像装置
５はこの観察像をモニタ装置９に表示する。A state in which the sample capsule 8 loaded with the observation sample is set in the sample container 3 and then the vacuum chamber 7 is evacuated by the exhaust system 6 to maintain the degree of vacuum at 4.8 × 10 -2 Pa or less. Observe at. Soft X emitted from X-ray generator 1
The line beam is converged by the condenser optical system 2 and passes through the sample capsule 8 set in the sample container 3. The soft X-ray that has passed through the observation sample is imaged by the imaging optical system 4 to the imaging device 5
Is guided to form an observation image on the imaging device 5. The imaging device 5 displays this observation image on the monitor device 9.
【０００６】軟Ｘ線を用いたＸ線顕微鏡は、軟Ｘ線に対
し１気圧下で２×１０-3μｍ-1程度の吸収率を有する大
気による吸収を避けるために、光学系全体をその光路長
に応じた高い真空度に保つ必要があり、軟Ｘ線の収束に
係るレンズ素子に性能のよいものが得にくいなどの欠点
を有するが、可視光線より格段に短い波長のＸ線を用い
るので従来の光学顕微鏡よりも高い解像度を期待でき
る。また、透過材料越しに生体の直接観察を行うことが
でき、組織培養液と共に生体を液封した試料カプセルを
用いれば、生体試料を損傷することなく長時間の生体試
料の生理観察が可能となる。従って、電子顕微鏡の場合
のような、試料の乾燥や金属蒸着など、観察対象物に損
傷を与える前処理が不要となる。An X-ray microscope using soft X-rays uses an entire optical system in order to avoid absorption by the atmosphere having an absorptance of about 2 × 10 −3 μm −1 for soft X-rays at 1 atmosphere. It has a drawback that it is necessary to maintain a high degree of vacuum according to the optical path length, and it is difficult to obtain a lens element related to the convergence of soft X-rays with good performance, but X-rays with a wavelength significantly shorter than visible light are used. Therefore, higher resolution can be expected than that of the conventional optical microscope. In addition, it is possible to directly observe the living body through the permeable material, and by using the sample capsule in which the living body is liquid-sealed together with the tissue culture liquid, it becomes possible to observe the physiological sample for a long time without damaging the biological sample. . Therefore, it is not necessary to perform a pretreatment such as drying of a sample or metal vapor deposition that damages an object to be observed as in the case of an electron microscope.
【０００７】また、図５（ａ）に示すように、いわゆる
水の窓と呼ばれる２．３〜４．４ｎｍの波長領域では、
水の線吸収係数がＶ字状に低下している。この波長領域
では、軟Ｘ線の水に対する吸収率と、生体を構成するタ
ンパク質などに対する吸収率との差が大きい。つまり、
この波長領域の軟Ｘ線を使用すれば、例えば細胞内に浮
遊する小気管などを観察するときに、コントラストのよ
い観察画像が得られる。Further, as shown in FIG. 5 (a), in the wavelength region of 2.3 to 4.4 nm, which is a so-called water window,
The linear absorption coefficient of water is V-shaped. In this wavelength region, there is a large difference between the absorption rate of water for soft X-rays and the absorption rate of proteins and the like that make up the living body. That is,
If soft X-rays in this wavelength region are used, an observation image with good contrast can be obtained when observing, for example, a small trachea floating in cells.
【０００８】ところで、上述したように軟Ｘ線は種々の
物質に容易に吸収されるので、観察試料を気密封入して
軟Ｘ線光路中に挿入する試料カプセルは、試料層の厚さ
が薄くなるような形状にするとともに、気密を兼ねた観
察窓材の軟Ｘ線の吸収量をできる限り小さくする必要が
ある。従って、この窓材には、軟Ｘ線に対する線吸収係
数が低く且つ膜強度が高い材料、例えば図５（ｂ）の窒
化シリコンＳｉ3Ｎ4などを薄膜形成したものが一般的に
採用されている。By the way, since soft X-rays are easily absorbed by various substances as described above, the sample capsule in which the observation sample is hermetically sealed and inserted into the soft X-ray optical path has a thin sample layer. In addition to such a shape, it is necessary to minimize the amount of soft X-ray absorption of the observation window material that also functions as airtight. Therefore, a material having a low linear absorption coefficient for soft X-rays and a high film strength, for example, a thin film of silicon nitride Si 3 N 4 shown in FIG. 5B is generally adopted as the window material. There is.
【０００９】図６は従来の試料カプセルの構造を示す図
であり、（ａ）は試料カプセルの試料封入部分の平面構
造を示し、（ｂ）は試料容器と試料カプセルの断面構造
を示す。この試料カプセルは、Ｘ線透過窓１０ｃ，１１
ｃを形成した２枚のチップ１０，１１の間に円環状のス
ペーサ１２を挟持し、その内側の密閉空間に観察試料を
装填するものである。チップ１０，１１は、シリコン板
１０ａ，１１ａ上に窒化シリコン薄膜Ｓｉ3Ｎ4１０ｂ，
１１ｂを形成した後、Ｘ線透過窓１０ｃ，１１ｃに対応
する部分のシリコン層をエッチングにより除去したもの
である。ここで、薄膜１０ｂ，１１ｂの張られたＸ線透
過窓１０ｃ，１１ｃは２００μｍ角の正方形であり、そ
の膜厚は０．０５〜０．１μｍである。また、チップ１
０，１１の対向する薄膜面１０ｂ，１１ｂの間に挿入さ
れている円環状のスペーサ１２は試料層の厚さを保持す
るもので、用途に応じて１〜１５μｍの範囲で適切な厚
さのものが選択される。例えば、波長２．３ｎｍの軟Ｘ
線を用い、窒化シリコン薄膜Ｓｉ3Ｎ4１０ｂ，１１ｂの
膜厚をそれぞれ０．１μｍ、試料層（水）の厚さを１０
μｍとすると、それぞれの軟Ｘ線透過率は３９％、１
２．３％となり、全体では約１１％の透過率が確保され
る。6A and 6B are views showing the structure of a conventional sample capsule, in which FIG. 6A shows a planar structure of a sample enclosing portion of the sample capsule, and FIG. 6B shows a sectional structure of a sample container and a sample capsule. This sample capsule has X-ray transmission windows 10c and 11
An annular spacer 12 is sandwiched between two chips 10 and 11 in which c is formed, and an observation sample is loaded into a sealed space inside thereof. The chips 10 and 11 consist of silicon nitride thin film Si 3 N 4 10b, on the silicon plates 10a and 11a, respectively.
After forming 11b, the silicon layer in the portions corresponding to the X-ray transmission windows 10c and 11c is removed by etching. Here, the X-ray transmission windows 10c and 11c in which the thin films 10b and 11b are stretched are squares of 200 μm square, and the thickness thereof is 0.05 to 0.1 μm. Also, chip 1
The annular spacer 12 inserted between the thin film surfaces 10b and 11b facing each other of 0 and 11 holds the thickness of the sample layer, and has an appropriate thickness in the range of 1 to 15 μm depending on the application. Things are selected. For example, soft X with a wavelength of 2.3 nm
Line, the thickness of the silicon nitride thin film Si 3 N 4 10b, 11b is 0.1 μm, and the thickness of the sample layer (water) is 10 μm.
μm, the soft X-ray transmittance of each is 39%, 1
It becomes 2.3%, and the transmittance of about 11% is secured as a whole.
【００１０】一方、スペーサ１２は、表面および裏面に
シール面を有し、２枚のチップ１０，１１と密着して円
環の内側の試料空間の密閉を行う機能を兼ね備えてい
る。また、試料容器１３，１４はねじ１５ａ，１５ｂに
より相互に固定され、Ｏリング１６を介してチップ１
０，１１を対向方向に押圧する。この押圧力により試料
カプセルが真空中で保持される。On the other hand, the spacer 12 has sealing surfaces on the front surface and the back surface, and also has a function of closely contacting the two chips 10 and 11 to seal the sample space inside the ring. The sample containers 13 and 14 are fixed to each other by screws 15a and 15b, and the chip 1 is attached via an O-ring 16.
0 and 11 are pressed in opposite directions. This pressing force holds the sample capsule in vacuum.
【００１１】また、スペーサを超えて（通過して）外側
に試料液が逃げるような場合や、図７（ａ）に示すよう
に円環状のスペーサでない場合は、スペーサ１２Ａ自身
で試料空間を密閉できないので、図７（ｂ）に示すよう
なＯリング１６Ａ，１６Ｂ，１６Ｃを設けてシーリング
を行う試料容器が用いられる。Further, when the sample solution escapes (passes) through the spacer to the outside, or when the sample liquid is not an annular spacer as shown in FIG. 7A, the sample space is hermetically sealed by the spacer 12A itself. Since this is not possible, a sample container for sealing by using O-rings 16A, 16B, 16C as shown in FIG. 7B is used.
【００１２】[0012]
【発明が解決しようとする課題】ところで、従来のＸ線
顕微鏡では、チップ１０上にスペーサ１２を載置して、
その内側に液状の観察試料、例えば培養液中に浮遊させ
た細胞を針の内径が０．２〜０．３ｍｍの注射器で滴定
した後、チップ１１をかぶせ、この試料カプセルを試料
容器１３，１４に納めてねじ１５ａ，１５ｂを固定する
手順で試料を装填している。By the way, in the conventional X-ray microscope, the spacer 12 is placed on the chip 10,
A liquid observation sample inside, for example, cells suspended in a culture medium is titrated with a syringe having an inner diameter of a needle of 0.2 to 0.3 mm, covered with a chip 11, and the sample capsule is covered with sample containers 13 and 14. The sample is loaded according to the procedure in which the screws 15a and 15b are fixed in the housing.
【００１３】しかしながら、図５（ａ）に示すように、
軟Ｘ線の水に対する吸収率と生体を構成するタンパク質
などに対する吸収率との差による観察画像のコントラス
トをよくするため、通常、試料層の厚さを１〜１５μｍ
にしなければならず、滴定した培養液の体積より試料カ
プセル内の試料空間の容積の方が小さく、液流が生じて
培養液が流れ、試料カプセルの外に漏れたり、培養液中
の観察対象物がＸ線透過窓内から移動して観察できなく
なるという問題がある。However, as shown in FIG.
In order to improve the contrast of the observed image due to the difference between the absorption rate of soft X-rays for water and the absorption rate for proteins constituting the living body, the thickness of the sample layer is usually 1 to 15 μm.
Since the volume of the sample space inside the sample capsule is smaller than the volume of the titrated culture solution, a liquid flow occurs and the culture solution flows, leaks out of the sample capsule, and is observed in the culture solution. There is a problem that the object moves from the X-ray transmission window and cannot be observed.
【００１４】この問題を解決するために、Ｘ線透過窓の
面積を大きくすることが考えられる。しかし、そのため
にはＸ線透過窓の剛性を上げる必要があり、Ｘ線透過窓
の剛性を上げるためにはＸ線透過窓の厚みを大きくしな
ければならない。Ｘ線透過窓の厚みを大きくすると、Ｘ
線透過窓におけるＸ線の吸収量が増加し、観察画像が暗
くなってしまうので、Ｘ線透過窓の面積は余り大きくす
ることができない。In order to solve this problem, it can be considered to increase the area of the X-ray transmission window. However, for that purpose, it is necessary to increase the rigidity of the X-ray transmission window, and in order to increase the rigidity of the X-ray transmission window, the thickness of the X-ray transmission window must be increased. If the thickness of the X-ray transmission window is increased, X
Since the amount of X-ray absorption in the X-ray transmission window increases and the observed image becomes dark, the area of the X-ray transmission window cannot be made very large.
【００１５】本発明の目的は、Ｘ線透過窓内に観察対象
物を捕らえ易くして試料装填時の作業性を向上させたＸ
線顕微鏡用試料カプセルを提供することにある。An object of the present invention is to improve the workability when loading a sample by facilitating the capturing of an observation object in the X-ray transmission window.
An object is to provide a sample capsule for a line microscope.
【００１６】[0016]
【課題を解決するための手段】一実施例の構成を示す図
１（ａ），（ｂ）に対応づけて本発明を説明すると、本
発明は、対向させた２枚のＸ線透過窓付平板１０，１１
と、これらの平板１０，１１に挟持されるスペーサ１２
とからなるＸ線顕微鏡用試料カプセルに適用され、平板
１０，１１のＸ線透過窓１０ｃ，１１ｃの周りに試料液
を溜める窪み１０ｄ，１１ｄを設けたことにより、上記
目的を達成する。The present invention will be described with reference to FIGS. 1 (a) and 1 (b) showing the structure of an embodiment. The present invention is provided with two opposed X-ray transmission windows. Flat plate 10,11
And a spacer 12 sandwiched between these flat plates 10 and 11.
The above-mentioned object is achieved by providing the sample capsule for the X-ray microscope, which is composed of and, and providing the recesses 10d and 11d for accumulating the sample liquid around the X-ray transmission windows 10c and 11c of the flat plates 10 and 11, respectively.
【００１７】[0017]
【作用】平板１１上にスペーサ１２を載置し、その内側
に観察対象物１８を含んだ試料液１７を滴定して平板１
１をかぶせると、平板１０，１１上の窪み１０ｄ，１１
ｄに試料液１７が蓄えられる。この結果、試料液１７の
流れが遅くなって試料液１７に含まれる観察対象物１８
が流れて移動することがなくなり、観察対象物１８をＸ
線透過窓１０ｃ，１１ｃ内に捕らえておくことができ
る。The spacer 12 is placed on the flat plate 11, and the sample liquid 17 containing the observation object 18 is titrated inside the spacer 12 to flatten the flat plate 1.
When covered with 1, the depressions 10d, 11 on the flat plates 10, 11
The sample liquid 17 is stored in d. As a result, the flow of the sample liquid 17 is delayed, and the observation object 18 contained in the sample liquid 17
Does not move and the observation object 18
It can be caught in the line transmission windows 10c and 11c.
【００１８】なお、本発明の構成を説明する上記課題を
解決するための手段および作用の項では、本発明を分り
やすくするために実施例の図を用いたが、これにより本
発明が実施例に限定されるものではない。Incidentally, in the section of means and action for solving the above-mentioned problems for explaining the constitution of the present invention, the drawings of the embodiments are used in order to make the present invention easy to understand. It is not limited to.
【００１９】[0019]
【実施例】図１は一実施例の構成を示す図であり、
（ａ）は試料カプセルの断面構造を示し、（ｂ）は片方
のチップ１１を取り除いて試料封入側から見た平面構造
を示す。なお、図６（ａ），（ｂ）に示す同様な構造と
機能を有する部材に対しては同一の符号を付して相違点
を中心に説明する。この試料カプセルは、平板状のチッ
プ１０，１１と円環状のスペーサ１２から構成される。
チップ１０，１１の互いに対向する面のＸ線透過窓１０
ｃ，１１ｃに相当する部分の周りには、試料液１７を溜
める窪み１０ｄ，１１ｄがフォトリソグラフィー法によ
り形成される。なお、この実施例では両方のチップ１
０，１１に試料液１７を溜める窪み１０ｄ，１１ｄを設
けたが、いずれか一方のチップだけに窪みを設けてもよ
い。FIG. 1 is a diagram showing the configuration of an embodiment,
(A) shows the cross-sectional structure of the sample capsule, and (b) shows the planar structure seen from the sample encapsulation side with one chip 11 removed. It should be noted that members having similar structures and functions shown in FIGS. 6A and 6B are designated by the same reference numerals, and description will be made centering on differences. The sample capsule is composed of flat chips 10 and 11 and an annular spacer 12.
X-ray transmission window 10 on the surfaces of chips 10 and 11 facing each other
Cavities 10d and 11d for accumulating the sample liquid 17 are formed around the portions corresponding to c and 11c by a photolithography method. In this embodiment, both chips 1
Although the recesses 10d and 11d for accumulating the sample solution 17 are provided at 0 and 11, the recesses may be provided only on one of the chips.
【００２０】チップ１０上にスペーサ１２を載置し、そ
の内側に観察対象物である細胞１８を含んだ培養液１７
を滴定してチップ１１をかぶせると、チップ１０，１１
上の窪み１０ｄ，１１ｄに培養液１７が蓄えられる。そ
の結果、培養液１７の流れが遅くなり、培養液１７に含
まれる細胞１８がＸ線透過窓１０ｃ，１１ｃ内から流れ
て移動する範囲が制限される。これによって、試料装填
時にＸ線透過窓１０ｃ，１１ｃ内に観察対象物の細胞１
８を捕らえやすくなり、試料装填時の作業性が向上す
る。A spacer 12 is placed on the chip 10, and a culture solution 17 containing cells 18 to be observed is placed inside the spacer 12.
Titrate and cover with tip 11, tip 10, 11
The culture solution 17 is stored in the upper depressions 10d and 11d. As a result, the flow of the culture solution 17 becomes slow, and the range in which the cells 18 contained in the culture solution 17 flow and move from inside the X-ray transmission windows 10c and 11c is limited. As a result, when the sample is loaded, the cells 1 to be observed are placed in the X-ray transmission windows 10c and 11c.
8 can be easily caught, and the workability at the time of loading the sample is improved.
【００２１】図２，３は、フォトリソグラフィー法によ
る図１に示す試料カプセルのチップ１０およびスペーサ
１２の製造方法を示す。なお、以下ではチップ１０とス
ペーサ１２とを同時に製造する場合を示すが、それぞれ
別々に製造してもよい。まず、図２（ａ）に示すよう
に、シリコン（Ｓｉ）基板１０ａの両面にスパッタリン
グ、ＣＶＤ法などによりＳｉＯ2１９のデポジションを
行い、図２（ｂ）に示すように、上面のＳｉＯ2１９上
にレジスト２０をコーティングして、スペーサ部のマス
ク２１ａを用いてフォトリソグラフィーを行う。2 and 3 show a method of manufacturing the chip 10 and the spacer 12 of the sample capsule shown in FIG. 1 by the photolithography method. Although the case where the chip 10 and the spacer 12 are manufactured simultaneously is shown below, they may be manufactured separately. First, as shown in FIG. 2A, the SiO 2 19 is deposited on both surfaces of the silicon (Si) substrate 10a by sputtering, a CVD method or the like, and the SiO 2 on the upper surface is deposited as shown in FIG. 2B. A resist 20 is coated on 19 and photolithography is performed using the mask 21a of the spacer portion.
【００２２】次に、図２（ｃ）に示すように、マスク２
１ａのレジストパターンに従ってＣＨＦ3などの材料ガ
スによりＳｉＯ2１９のドライエッチングを行った後、
図２（ｄ）に示すように、レジスト２０を剥離してＳｉ
Ｏ2１９のパターンに従ってＳｉのドライエッチングを
行う。さらに、図２（ｅ）に示すように、ＳｉＯ2１９
の両面エッチングを行う。Next, as shown in FIG. 2C, the mask 2
After dry etching of SiO 2 19 with a material gas such as CHF 3 according to the resist pattern of 1a,
As shown in FIG. 2D, the resist 20 is removed to remove Si.
Dry etching of Si is performed according to the pattern of O 2 19. Furthermore, as shown in FIG. 2 (e), SiO 2 19
Both sides are etched.
【００２３】次に、図２（ｆ）に示すように、ＣＶＤ法
などによりＳｉ基板１０ａの両面にＸ線透過窓材である
Ｓｉ3Ｎ4１０ｂのデポジションを行い、図３（ａ）に示
すように、上面にレジスト２０をコーティングしてスク
ライブライン部と窪み部のマスク２１ｂを用いてフォト
リソグラフィーを行う。なお、スクライブライン部はＳ
ｉ基板１０ａを試料カプセルの寸法に合せてカットする
ための基準ラインである。さらに、図３（ｂ）に示すよ
うに、マスク２１ｂのレジストパターンに従ってＣＦ4
などの材料ガスによりＳｉ3Ｎ4１０ｂのドライエッチン
グを行い、レジスト２０を剥離する。Next, as shown in FIG. 2 (f), an X-ray transparent window material, Si 3 N 4 10b, is deposited on both surfaces of the Si substrate 10a by the CVD method or the like, and then, as shown in FIG. 3 (a). As shown, the resist 20 is coated on the upper surface and photolithography is performed using the mask 21b for the scribe line portion and the depression portion. The scribe line section is S
It is a reference line for cutting the i substrate 10a according to the size of the sample capsule. Further, as shown in FIG. 3B, CF 4 is formed according to the resist pattern of the mask 21b.
Dry etching of Si 3 N 4 10b is performed by using a material gas such as the above, and the resist 20 is peeled off.
【００２４】その後、図３（ｃ）に示すように、両面に
レジスト２０をコーティングし、下面にＸ線透過窓部の
マスク２１ｃを用いてフォトリソグラフィーを行った
後、図３（ｄ）に示すように、マスク２１ｃのレジスト
パターンに従ってＣＦ4などの材料ガスによりＳｉ3Ｎ4
１０ｂのドライエッチングを行い、レジスト２０を剥離
する。After that, as shown in FIG. 3C, resist 20 is coated on both surfaces, and the lower surface is subjected to photolithography using the mask 21c of the X-ray transmission window portion, and then, shown in FIG. 3D. as, Si 3 N 4 with a material gas such as CF 4 in accordance with the resist pattern of the mask 21c
10b is dry-etched to remove the resist 20.
【００２５】そして、図３（ｅ）に示すように、水酸化
カリウム水溶液（ＫＯＨ）を用いて、Ｓｉ3Ｎ4１０ｂの
パターンに従ってＳｉ基板１０ａのウェットエッチング
を行った後、図３（ｆ）に示すように、スクライブライ
ンに従ってＳｉ基板１０ａより試料カプセルごとにダイ
シングを行ってチップ１０およびスペーサ１２を製造す
る。Then, as shown in FIG. 3E, after wet etching the Si substrate 10a according to the pattern of Si 3 N 4 10b using an aqueous solution of potassium hydroxide (KOH), FIG. As shown in, the dicing is performed for each sample capsule from the Si substrate 10a according to the scribe line to manufacture the chip 10 and the spacer 12.
【００２６】なお、スペーサ部を持たない試料カプセル
やチップ１１の製造手順は図２（ｆ）からの製造方法と
同じ工程であり、説明を省略する。The manufacturing procedure of the sample capsule and the chip 11 having no spacer portion is the same as the manufacturing method from FIG. 2 (f), and the description thereof will be omitted.
【００２７】試料液を溜める窪みの形状は上述した実施
例に限定されず、液溜まりとしての機能を満足するもの
であればどのような形状、大きさ、配置でもよい。The shape of the recess for storing the sample liquid is not limited to the above-mentioned embodiment, and any shape, size and arrangement may be used as long as the function as a liquid reservoir is satisfied.
【００２８】また、平板のＸ線観察窓の周りに設けた窪
みに外部から管を通し、試料カプセル内に断続的または
連続的に試料液を流すことにより、試料液の交換をした
り、異なる溶液を注入してその影響を観察することが可
能となる。Further, by passing a tube from the outside into a recess provided around the X-ray observation window of the flat plate and flowing the sample solution into the sample capsule intermittently or continuously, the sample solution can be exchanged or changed. It is possible to inject the solution and observe its effect.
【００２９】以上の実施例の構成において、チップ１
０，１１が平板を、スペーサ１２がスペーサを、窪み１
０ｄが窪みをそれぞれ構成する。In the configuration of the above embodiment, the chip 1
0 and 11 are flat plates, spacers 12 are spacers, and recess 1
0d constitutes each depression.
【００３０】[0030]
【発明の効果】以上説明したように本発明によれば、平
板のＸ線透過窓の周辺に試料液を溜める窪みを設けたの
で、観察対象物を含んだ試料液を装填する時に、平板上
の窪みに試料液が蓄えられ、試料液の流れが遅くなって
観察対象物が流れて移動することがなくなり、観察対象
物をＸ線透過窓内に捕らえておくことができ、試料装填
時の作業性が向上する。また、平板上に窪みを設けただ
けなので、試料カプセルの構成部品点数が増加せず、試
料カプセル自体の組み立ても容易である。さらに、試料
空間内の接触面がなく、Ｘ線透過窓やその間隔に対する
影響は全くないので、Ｘ線顕微鏡による試料観察像にも
影響がない。As described above, according to the present invention, since the depression for accumulating the sample solution is provided around the X-ray transmission window of the flat plate, when the sample solution containing the observation object is loaded, The sample liquid is stored in the depression of the sample liquid, the flow of the sample liquid slows down, and the observation object does not move and move, and the observation object can be trapped in the X-ray transmission window. Workability is improved. Further, since only the dent is provided on the flat plate, the number of constituent parts of the sample capsule does not increase, and the sample capsule itself can be easily assembled. Further, since there is no contact surface in the sample space and there is no influence on the X-ray transmission window and its interval, there is no influence on the sample observation image by the X-ray microscope.
【図１】一実施例の構造を示す図であり、（ａ）は断面
構造を示し、（ｂ）は片方のチップを取り除いて試料装
填側から見た平面構造を示す。1A and 1B are views showing a structure of one embodiment, FIG. 1A shows a sectional structure, and FIG. 1B shows a planar structure seen from a sample loading side with one chip removed.
【図２】一実施例のチップおよびスペーサの製造方法を
示す図。FIG. 2 is a diagram showing a method of manufacturing a chip and a spacer according to an embodiment.
【図３】一実施例のチップおよびスペーサの製造方法を
示す図。FIG. 3 is a diagram showing a method of manufacturing a chip and a spacer according to an embodiment.
【図４】従来のＸ線顕微鏡の概要を示す図。FIG. 4 is a diagram showing an outline of a conventional X-ray microscope.
【図５】各種物質の軟Ｘ線に対する線吸収係数を示す
図。FIG. 5 is a diagram showing linear absorption coefficients of various substances for soft X-rays.
【図６】従来のＸ線顕微鏡用試料カプセルの構造を示す
図。FIG. 6 is a view showing a structure of a conventional sample capsule for an X-ray microscope.
【図７】他の従来のＸ線顕微鏡用試料カプセルの構造を
示す図。FIG. 7 is a view showing the structure of another conventional sample capsule for an X-ray microscope.
１０，１１ チップ １０ａ，１１ａ シリコン板 １０ｂ，１１ｂ 窒化シリコン薄膜 １０ｃ，１１ｃ Ｘ線透過窓 １０ｄ，１１ｄ 窪み １２ スペーサ １７ 試料液 １８ 観察対象物 １９ ＳｉＯ2 ２０ レジスト 10, 11 Chips 10a, 11a Silicon plates 10b, 11b Silicon nitride thin films 10c, 11c X-ray transmission windows 10d, 11d Recesses 12 Spacers 17 Sample liquid 18 Observation target 19 SiO2 20 Resist
Claims (1)
鏡用試料カプセルにおいて、 前記平板のＸ線透過窓の周りに試料液を溜める窪みを設
けたことを特徴とするＸ線顕微鏡用試料カプセル。1. A sample capsule for an X-ray microscope comprising two opposed flat plates with an X-ray transmission window and spacers sandwiched between these flat plates, wherein a sample liquid is provided around the X-ray transmission window of the flat plate. A sample capsule for an X-ray microscope, which is provided with a recess for accommodating a liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4332024A JPH06180400A (en) | 1992-12-11 | 1992-12-11 | Sample capsule for x-ray microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4332024A JPH06180400A (en) | 1992-12-11 | 1992-12-11 | Sample capsule for x-ray microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06180400A true JPH06180400A (en) | 1994-06-28 |
Family
ID=18250288
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4332024A Pending JPH06180400A (en) | 1992-12-11 | 1992-12-11 | Sample capsule for x-ray microscope |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06180400A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011105421A1 (en) | 2010-02-24 | 2011-09-01 | 独立行政法人産業技術総合研究所 | Member supporting sample for observing x-ray microscopic image, cell containing sample for observing x-ray microscopic image, and x-ray microscope |
| WO2013035292A1 (en) | 2011-09-09 | 2013-03-14 | 独立行政法人産業技術総合研究所 | Sample-containing cell for x-ray microscope and method for observing x-ray microscopic image |
-
1992
- 1992-12-11 JP JP4332024A patent/JPH06180400A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011105421A1 (en) | 2010-02-24 | 2011-09-01 | 独立行政法人産業技術総合研究所 | Member supporting sample for observing x-ray microscopic image, cell containing sample for observing x-ray microscopic image, and x-ray microscope |
| US8891728B2 (en) | 2010-02-24 | 2014-11-18 | National Institute Of Advanced Industrial Science And Technology | Specimen supporting member for X-ray microscope image observation, specimen containing cell for X-ray microscope image observation, and X-ray microscope |
| WO2013035292A1 (en) | 2011-09-09 | 2013-03-14 | 独立行政法人産業技術総合研究所 | Sample-containing cell for x-ray microscope and method for observing x-ray microscopic image |
| US9336918B2 (en) | 2011-09-09 | 2016-05-10 | National Institute Of Advanced Industrial Science And Technology | Sample-containing cell for X-ray microscope and method for observing X-ray microscopic image |
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