JP2017160067A - Method for jointing crystal substance - Google Patents
Method for jointing crystal substance Download PDFInfo
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- JP2017160067A JP2017160067A JP2016043989A JP2016043989A JP2017160067A JP 2017160067 A JP2017160067 A JP 2017160067A JP 2016043989 A JP2016043989 A JP 2016043989A JP 2016043989 A JP2016043989 A JP 2016043989A JP 2017160067 A JP2017160067 A JP 2017160067A
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- 239000013078 crystal Substances 0.000 title claims description 34
- 238000000034 method Methods 0.000 title claims description 20
- 239000000126 substance Substances 0.000 title abstract description 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 44
- 239000010431 corundum Substances 0.000 claims abstract description 44
- 125000006850 spacer group Chemical group 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229920000742 Cotton Polymers 0.000 claims abstract description 4
- 238000005304 joining Methods 0.000 claims description 19
- 230000013011 mating Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 13
- 229910001634 calcium fluoride Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000000960 laser cooling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
Description
本発明は、フッ酸等の液中に含まれる微粒子を測定する微粒子計に組み込まれるフローセルの材料として用いられる合成コランダム（Ａｌ2Ｏ3）や光学部品として用いられるフッ化カルシウム（ＣａＦ2）などの結晶体の接合方法に関する。 The present invention relates to synthetic corundum (Al 2 O 3 ) used as a material for a flow cell incorporated in a micrometer for measuring fine particles contained in a liquid such as hydrofluoric acid, calcium fluoride (CaF 2 ) used as an optical component, etc. The present invention relates to a method for bonding crystals.
合成コランダム製のフローセルを製造するには、板状の合成コランダム片を複数用意し、これら合成コランダム片を接合することで得ている。ここで、接着剤を用いたのでは接合面において境界面ができてしまい、光が屈折したり反射してしまう。また、熱融着させた場合には、接合面に気泡が封じ込められるなどの問題もある。 In order to manufacture a flow cell made of synthetic corundum, a plurality of plate-like synthetic corundum pieces are prepared, and these synthetic corundum pieces are joined. Here, if an adhesive is used, a boundary surface is formed on the joint surface, and light is refracted or reflected. In addition, when heat-sealing, there is a problem that bubbles are contained in the joint surface.
そこで、本出願人は特許文献１〜３を提案した。特許文献１〜３に開示される接合方法は基本的には同じであり、先ず結晶ブロックから合成コランダム片を切り出し、この切り出した合成コランダム片の接合面を研磨し、研磨した面同士を合わせ、合わせた状態の２枚の合成コランダム片の一端部側を強く押し付け、２枚の合成コランダム片の間隔を干渉縞ができる程度とし、この状態で２枚の合成コランダム片を合成コランダムの融点（２０３０℃）以下に加熱することで、一端側から他端側に向かって徐々に密着状態となるようにしたものである。 Therefore, the present applicant has proposed Patent Documents 1 to 3. The bonding methods disclosed in Patent Documents 1 to 3 are basically the same, first cut out a synthetic corundum piece from the crystal block, polish the bonded surface of the cut out synthetic corundum piece, and match the polished surfaces together, The two synthetic corundum pieces in the combined state are strongly pressed against one end side so that the distance between the two synthetic corundum pieces is such that interference fringes can be formed. In this state, the two synthetic corundum pieces are melted with the melting point of the synthetic corundum (2030). C.) or less, by gradually heating from one end side to the other end side, a close contact state is obtained.
上記において、強く押し付けた状態の一端部側ではオプティカルコンタクト状態或いは化学的加圧密着状態になっており、加熱によって干渉縞がなくなるので、この密着状態が他端側まで連続すると考えられる。そして、このように接合された合成コランダム片同士は光学的な境界面が存在せず、極めて優れた三次元構造体が得られる。 In the above, one end side of the strongly pressed state is in an optical contact state or a chemical pressure contact state, and interference fringes are eliminated by heating, so this contact state is considered to continue to the other end side. And the synthetic | combination corundum pieces joined in this way do not have an optical interface, and an extremely excellent three-dimensional structure is obtained.
特許文献１〜３に開示される方法によって製造された接合体は、耐薬品性に優れ、接合面が剥離したり接合面で屈折或いは反射する等の不具合がない反面、歩留りが十分ではないという問題がある。 The joined body manufactured by the method disclosed in Patent Documents 1 to 3 has excellent chemical resistance, and there is no problem such as peeling or reflection or reflection at the joining surface, but the yield is not sufficient. There's a problem.
歩留りが十分ではない原因としては、一端部側を他端側よりも強く押し付けることで、接合面同士の間に干渉縞ができる程度の隙間を形成するようにしているが、他端側は何ら拘束していないため、他端側における合成コランダム片同士の間に形成される微細な隙間が一定でないことが考えられる。
この問題は、フッ化カルシウム（ＣａＦ2）などの結晶体を接合する場合にも生じる。
The reason why the yield is not sufficient is to press the one end side more strongly than the other end side so that a gap is formed between the joint surfaces so that interference fringes are formed. Since it is not restrained, it is considered that the fine gap formed between the synthetic corundum pieces on the other end side is not constant.
This problem also occurs when a crystal such as calcium fluoride (CaF 2 ) is joined.
上記課題を解決するため、本発明に係る結晶体片の接合方法は、互いに接合する合成コランダムやフッ化カルシウムなどの結晶体片の接合する面を合わせ、この合わせた状態の結晶体片の一端側を他端側よりも強く押圧して合わせ面に干渉縞を形成し、この状態で結晶体片を結晶体の融点以下の温度で加熱することで、前記合わせ面を干渉縞が消失した完全な接合状態とする接合方法であって、前記互いに接合する結晶体片の他端側間に加熱時の圧力で圧潰可能な材質からなる微細なスペーサを介在させるようにした。 In order to solve the above-described problem, the crystal piece joining method according to the present invention includes a method of joining crystal face pieces such as synthetic corundum and calcium fluoride joined together, and one end of the crystal pieces in the combined state. The interference fringes are formed on the mating surfaces by pressing the side more strongly than the other end side, and in this state, the crystal fragments are heated at a temperature equal to or lower than the melting point of the crystals to completely eliminate the interference fringes on the mating surfaces. In this joining method, a fine spacer made of a material that can be crushed by pressure during heating is interposed between the other ends of the crystal pieces to be joined together.
前記スペーサとしては、熱処理によって干渉縞が消失するのを妨げることがないもの、つまり接合する結晶体片同士がオプティカルコンタクト或いは化学的加圧密着状態となることを妨げない程度の圧潰性（弾性、柔らかさ）を有することが必要である。 The spacer does not prevent the interference fringes from disappearing by the heat treatment, that is, the collapsibility (elasticity) to such an extent that the crystal pieces to be bonded do not interfere with the optical contact or the chemical pressure contact state. Softness).
スペーサの一例としては綿繊維が挙げられるが、これに限定されるものではない。またスペーサの大きさは必要な干渉縞を形成するものであるから、合成コランダム片の接合長さによって異なるが、概ね１５〜６０μｍの径である。 An example of the spacer is cotton fiber, but is not limited thereto. Further, since the size of the spacer forms a necessary interference fringe, it has a diameter of about 15 to 60 μm, though it varies depending on the joining length of the synthetic corundum piece.
また、本発明に係る接合方法においては、接合する結晶体片の一端側を押圧した仮接合の状態で、合わせた状態の結晶体片の単位長さ当たりの縞の本数によって、加熱処理前に仮接合状態の良否を判断することができる。 Further, in the bonding method according to the present invention, in the temporary bonding state in which one end side of the crystal pieces to be bonded is pressed, the number of stripes per unit length of the combined crystal pieces is determined before the heat treatment. The quality of the temporarily joined state can be determined.
また、合わせた状態の結晶体片の一端部の押圧箇所は幅方向の一部のみとすることも可能である。 Moreover, it is also possible to make only the part of the width direction the press location of the one end part of the crystal body piece of the match | combined state.
本発明によれば、結晶体片同士を接着剤を用いずに、一端側を他端側よりも強く押圧した状態での熱処理によって接合するに際し、他端側の結晶体片間の間隔をスペーサによって正確にコントロールできるため、歩留りを高めることができる。 According to the present invention, when bonding crystal pieces to each other by heat treatment in a state where one end side is pressed more strongly than the other end side without using an adhesive, the interval between the crystal pieces on the other end side is set as a spacer. Because it can be controlled accurately, the yield can be increased.
また、熱処理する前の仮接合の状態で、接合される結晶体片の接合面間に形成される干渉縞の単位長さあたりの本数によって、仮接合の状態の良否を判定できるため、更に歩留りを高めることができる。 Moreover, since the number of interference fringes per unit length formed between the bonding surfaces of the crystal pieces to be bonded can be determined in the temporary bonding state before the heat treatment, the quality of the temporary bonding state can be determined. Can be increased.
更に、合わせた状態の結晶体片の一端部の押圧箇所を幅方向全部ではなく幅方向の一部のみとすることで、押圧治具の跡が付く箇所が一部のみになり、接合後の不適合部分が少なくなり、材料の無駄がなくなる。 Furthermore, by making only one part in the width direction, not the entire pressed part of the one end of the crystal pieces in the combined state, the part where the mark of the pressing jig is attached becomes only a part, and after joining There are fewer non-conforming parts and there is no waste of material.
以下に本発明の実施の形態を添付図面に基づいて説明する。尚、図示例では結晶体として合成コランダムについて説明する。
図１は２つの合成コランダム片を重ね合わせた状態の側面図、図２は一方の合成コランダム片の端部にスペーサを載置した状態の平面図であり、先ず２つの合成コランダム片１、２を用意する。
Embodiments of the present invention will be described below with reference to the accompanying drawings. In the illustrated example, synthetic corundum will be described as a crystal.
FIG. 1 is a side view showing a state in which two synthetic corundum pieces are superposed, and FIG. 2 is a plan view showing a state in which a spacer is placed on the end of one synthetic corundum piece. Prepare.
これら合成コランダム片１、２は結晶ブロックから切り出した後に、接合される面を研磨した後に洗浄し、微細なゴミなどが接合面にないことを確認したものである。尚、図示例では２つの合成コランダム片を重ねているが３つ以上の合成コランダム片を重ねて同時に接合することもできる。 These synthetic corundum pieces 1 and 2 were cut out from the crystal block, and then the surfaces to be joined were polished and then washed, and it was confirmed that there was no fine dust on the joined surfaces. In the illustrated example, two synthetic corundum pieces are overlapped, but three or more synthetic corundum pieces can be overlapped and joined simultaneously.
合成コランダム片１、２を重ねる際には結晶の軸、稜線及び軸角を完全に一致させる必要はなく、互いの合成コランダム片１、２の結晶の軸、稜線及び軸角のズレが５°以内とするのが好ましい。 When the synthetic corundum pieces 1 and 2 are stacked, it is not necessary to make the crystal axes, ridge lines, and axis angles coincide with each other. It is preferable to be within.
合成コランダム片１、２の一端側は治具４によって強く押圧或いは挟持されている。治具４による押圧箇所は幅方向の全域としてもよいが図示例のように幅方向の中央の一部のみとすることで、接合後の不適合部分を少なくしている。 One end side of the synthetic corundum pieces 1 and 2 is strongly pressed or clamped by the jig 4. Although the pressing part by the jig 4 may be the entire area in the width direction, only a part of the center in the width direction is used as in the illustrated example, thereby reducing non-conforming parts after joining.
合成コランダム片１、２の他端側の接合面間にはスペーサ３が介在している。このスペーサ３は図では分かりやすくするため実際よりは大きく示しているが、実施例では直径が３０μｍの綿繊維を用いている。スペーサ３は、仮接合後の熱処理の際に合成コランダム片１、２の他端側に作用する圧力によって潰れることで、合成コランダム片１、２の他端側でのオプティカルコンタクト或いは化学的加圧密着状態の妨げにならないものであればよい。 A spacer 3 is interposed between the joint surfaces on the other end side of the synthetic corundum pieces 1 and 2. The spacer 3 is shown larger than the actual size for the sake of clarity in the figure, but in the embodiment, a cotton fiber having a diameter of 30 μm is used. The spacer 3 is crushed by the pressure acting on the other end side of the synthetic corundum pieces 1 and 2 during the heat treatment after the temporary joining, so that the optical contact or the chemical pressure density on the other end side of the synthetic corundum pieces 1 and 2 is collapsed. Anything that does not interfere with the wearing state is acceptable.
スペーサ３としては、ゲルビーズなども使用することができるが、仮接合後の熱処理の際に大量にガスを発生するものは、接合面に気泡が残る可能性があるので好ましくない。 Gel beads or the like can be used as the spacer 3, but those that generate a large amount of gas during the heat treatment after temporary bonding are not preferable because bubbles may remain on the bonding surface.
図３は重ね合わせた合成コランダム片１、２の一端部を押圧した状態の平面写真であり、この写真からも明らかなように、重ね合わせた合成コランダム片１、２の接合面の微細な隙間に由来する干渉縞が観察される。 FIG. 3 is a plan view showing a state in which one end portion of the superimposed synthetic corundum pieces 1 and 2 is pressed. As is clear from this photograph, a fine gap in the joint surface of the superimposed synthetic corundum pieces 1 and 2 is shown. Interference fringes originating from are observed.
上記干渉縞の間隔は接合面の微細な隙間の大きさに比例するため、仮接合状態での単位長さあたりの干渉縞の本数をカウントすることにより、合成コランダム片１、２の接合面の微細な隙間が適切な範囲にあるか否かを、前もって判断することができる。この実施例にあっては単位長さあたりに５本の縞が観察される。 Since the interval between the interference fringes is proportional to the size of the minute gaps on the joint surface, counting the number of interference fringes per unit length in the temporary joint state allows the joint surface of the synthetic corundum pieces 1 and 2 to be It can be determined in advance whether or not the minute gap is in an appropriate range. In this embodiment, five stripes are observed per unit length.
以上の仮接合状態の合成コランダム片をコランダムの融点以下の温度まで加熱し一定時間保持する。
すると、既にオプティカルコンタクト或いは化学的加圧密着状態にある一端側から他端側に向かってオプティカルコンタクト或いは化学的加圧密着状態が進行し、この進行に併せて、合成コランダム片間に存在するガスは完全に排除され、接合面全体がオプティカルコンタクト或いは化学的加圧密着状態となる。
The synthetic corundum piece in the above temporarily joined state is heated to a temperature below the melting point of the corundum and held for a certain period of time.
Then, the optical contact or the chemical pressure contact state advances from one end side already in the optical contact or chemical pressure contact state to the other end side, and the gas existing between the synthetic corundum pieces along with this progress. Is completely eliminated, and the entire joining surface is in an optical contact or chemical pressure contact state.
図４（ａ）は接合前の２つの合成コランダム片の写真、（ｂ）は接合後の写真であり、図４（ａ）では２つの合成コランダム片が紙面垂直方向に重なったものが１６対映っている。各対において、中心部には流体を通すための通路が形成されている。この通路を挟んで左右の部分は接合される面であり、熱処理前は干渉縞が観察される。
また熱処理後を示す（ｂ）の写真には、全ての試験片において、上記の干渉縞が全く観察されず、光学的な境界面を認められなかった。
4A is a photograph of two synthetic corundum pieces before joining, and FIG. 4B is a photograph after joining. In FIG. 4A, 16 pairs of two synthetic corundum pieces overlapped in the direction perpendicular to the paper surface. It is reflected. In each pair, a passage for allowing fluid to pass is formed in the center. The left and right portions sandwiching this passage are surfaces to be joined, and interference fringes are observed before heat treatment.
Moreover, in the photograph of (b) which shows after heat processing, in all the test pieces, the above-mentioned interference fringes were not observed at all and no optical boundary surface was recognized.
図５は本発明方法によって製造した三次元構造体を示しており、この三次元構造体５は、合成コランダム片からなるベースプレート５ａとこのベースプレート５ａの辺に沿って接合される４枚のサイドプレート５ｂ、５ｃ、５ｄ、５ｅからなり、ベースプレート５ａと各サイドプレート５ｂ、５ｃ、５ｄ、５ｅ及び各サイドプレート同士の突合せ部において、本発明方法を適用することで、１度の熱処理により三次元構造体５が製造される。 FIG. 5 shows a three-dimensional structure manufactured by the method of the present invention. The three-dimensional structure 5 includes a base plate 5a made of a synthetic corundum piece and four side plates joined along the sides of the base plate 5a. 5b, 5c, 5d, and 5e, and the base plate 5a and the side plates 5b, 5c, 5d, and 5e, and the butt portions between the side plates are applied with the method of the present invention so that the three-dimensional structure is obtained by a single heat treatment. The body 5 is manufactured.
本発明方法は微粒子計に組み込まれるフローセルに限らず、レンズ、プリズムなどの各種光学部品、硬度が要求される機械部品、接合面が密閉状態にある特性を利用した真空容器、例えば可変波長レーザの較正、光スペクトラムアナライザの較正、ガス分析器の較正、波長計の較正、周波数標準、安定した周波数源、磁気光学トラップ法を用いた原子のレーザ冷却などに用いられるガス封入ガラスセルや高真空ガラスチャンバなどに応用することができる。 The method of the present invention is not limited to a flow cell incorporated in a particle meter, but includes various optical parts such as lenses and prisms, mechanical parts that require hardness, and vacuum containers that use characteristics in which the joint surface is sealed, such as a variable wavelength laser. Gas-filled glass cell and high vacuum glass used for calibration, optical spectrum analyzer calibration, gas analyzer calibration, wavelength meter calibration, frequency standard, stable frequency source, laser cooling of atoms using magneto-optical trap method, etc. It can be applied to a chamber or the like.
また、本発明方法は、合成コランダムに限らずフッ化カルシウムなどの結晶体の接合にも用いることができる。 In addition, the method of the present invention can be used not only for synthetic corundum but also for bonding crystal bodies such as calcium fluoride.
１、２…合成コランダム片、３…スペーサ、４…押圧治具、５…三次元構造体。
1, 2 ... synthetic corundum piece, 3 ... spacer, 4 ... pressing jig, 5 ... 3D structure.
Claims (5)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
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| JP2016043989A JP6113881B1 (en) | 2016-03-08 | 2016-03-08 | Crystal joining method |
| EP17763290.8A EP3428326B1 (en) | 2016-03-08 | 2017-03-08 | Method for joining crystal body |
| PCT/JP2017/009149 WO2017154950A1 (en) | 2016-03-08 | 2017-03-08 | Method for joining crystal body |
| US15/767,497 US10519567B2 (en) | 2016-03-08 | 2017-03-08 | Bonding method of crystal body |
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| JP2016043989A JP6113881B1 (en) | 2016-03-08 | 2016-03-08 | Crystal joining method |
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| JP6113881B1 JP6113881B1 (en) | 2017-04-12 |
| JP2017160067A true JP2017160067A (en) | 2017-09-14 |
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| JP3499717B2 (en) * | 1997-06-24 | 2004-02-23 | 株式会社 ジャパンセル | Synthetic corundum joining method and synthetic corundum cell manufacturing method |
| JP4251462B2 (en) * | 1998-12-22 | 2009-04-08 | 株式会社ジャパンセル | Synthetic corundum joining method, synthetic corundum cell manufacturing method and synthetic corundum |
| JP4224336B2 (en) * | 2002-07-19 | 2009-02-12 | リオン株式会社 | Synthetic corundum cell |
| WO2015098927A1 (en) * | 2013-12-25 | 2015-07-02 | 株式会社ニコン | Calcium fluoride member, method for producing same, and method for pressure-bonding calcium fluoride crystal |
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