JP2018131360A - Bonding method of magnesium fluoride crystal substance - Google Patents
Bonding method of magnesium fluoride crystal substance Download PDFInfo
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- JP2018131360A JP2018131360A JP2017026513A JP2017026513A JP2018131360A JP 2018131360 A JP2018131360 A JP 2018131360A JP 2017026513 A JP2017026513 A JP 2017026513A JP 2017026513 A JP2017026513 A JP 2017026513A JP 2018131360 A JP2018131360 A JP 2018131360A
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- magnesium fluoride
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- 239000013078 crystal Substances 0.000 title claims abstract description 57
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 title claims abstract description 38
- 229910001635 magnesium fluoride Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims description 14
- 239000000126 substance Substances 0.000 title abstract description 13
- 125000006850 spacer group Chemical group 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 6
- 229920000742 Cotton Polymers 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000005304 joining Methods 0.000 claims description 11
- 230000013011 mating Effects 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 abstract description 13
- 239000010431 corundum Substances 0.000 abstract description 13
- 230000003287 optical effect Effects 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000960 laser cooling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
本発明は、超低屈折光学材料として知られるフッ化マグネシウム（ＭｇＦ2）結晶体の接合方法に関する。 The present invention relates to a method for joining magnesium fluoride (MgF 2 ) crystals known as an ultra-low refractive optical material.
パーティクルカウンターなどに組み込む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 to be incorporated in a particle counter or the like, a plurality of plate-like synthetic corundum pieces are prepared, and these synthetic corundum pieces are joined together. 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. 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、フッ化マグネシウム（ＭｇＦ2）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 magnesium fluoride (MgF 2 ) crystals are joined.
上記課題を解決するため、本発明に係るフッ化マグネシウム（ＭｇＦ2）結晶体片の接合方法は、互いに接合するフッ化マグネシウム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-mentioned problem, a method for joining magnesium fluoride (MgF 2 ) crystal pieces according to the present invention is such that the surfaces of magnesium fluoride crystal pieces to be joined together are joined together, and the crystal pieces in this combined state The interference fringe disappears on the mating surface by pressing one end side of the substrate more strongly than the other end side to form an interference fringe on the mating surface and heating the crystal piece at a temperature below the melting point of the crystal in this state. 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。図１は２つのフッ化マグネシウム結晶体片を重ね合わせた状態の側面図、図２は一方のフッ化マグネシウム結晶体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つのフッ化マグネシウム結晶体片１、２を用意する。 Embodiments of the present invention will be described below with reference to the accompanying drawings. FIG. 1 is a side view showing a state in which two magnesium fluoride crystal pieces are superposed, and FIG. 2 is a plan view showing a state in which a spacer is placed on the end of one magnesium fluoride crystal piece. Magnesium fluoride crystal pieces 1 and 2 are prepared.
これらフッ化マグネシウム結晶体片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つのフッ化マグネシウム結晶体片を重ねているが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 magnesium fluoride crystal pieces 1 and 2 were cut out from the crystal block, and then the surfaces to be joined were polished and then washed to confirm that there was no fine dust or the like on the joined surfaces. In the illustrated example, two magnesium fluoride crystal pieces are stacked, but three or more synthetic corundum pieces can be stacked and bonded simultaneously.
フッ化マグネシウム結晶体片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、互いのフッ化マグネシウム結晶体片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 magnesium fluoride crystal pieces 1 and 2 are stacked, it is not necessary to make the axes, ridge lines, and axis angles of the crystals completely coincide with each other. The angular deviation is preferably within 5 °.
フッ化マグネシウム結晶体片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 sides of the magnesium fluoride crystal pieces 1 and 2 are 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.
フッ化マグネシウム結晶体片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フッ化マグネシウム結晶体片１、２の他端側に作用する圧力によって潰れることで、フッ化マグネシウム結晶体片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 magnesium fluoride crystal 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 magnesium fluoride crystal pieces 1 and 2 during the heat treatment after the temporary bonding, so that the optical at the other end side of the magnesium fluoride crystal pieces 1 and 2 is reduced. Any material that does not interfere with the contact or chemical pressure contact state may be used.
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は重ね合わせたフッ化マグネシウム結晶体片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、重ね合わせたフッ化マグネシウム結晶体片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 of the superposed magnesium fluoride crystal pieces 1 and 2 is pressed. As is apparent from this photograph, the superposed magnesium fluoride crystal pieces 1 and 2 are shown in FIG. Interference fringes derived from minute gaps on the joint surface 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、フッ化マグネシウム結晶体片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 joined state allows the magnesium fluoride crystal pieces 1 and 2 to It is possible to determine in advance whether or not the minute gap on the joint surface is in an appropriate range. In this embodiment, five stripes are observed per unit length.
以上の仮接合状態のフッ化マグネシウム結晶体片をフッ化マグネシウ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、フッ化マグネシウム結晶体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 above-mentioned temporarily bonded magnesium fluoride crystal piece is heated to a temperature below the melting point of magnesium fluoride and held for a certain period of time.
Then, the optical contact or the chemical pressure contact state advances from the one end side already in the optical contact or chemical pressure contact state toward the other end side, and along with this progress, between the magnesium fluoride crystal pieces. The existing gas is completely eliminated, and the entire bonding surface is in an optical contact or chemical pressure contact state.
図４（ａ）は３つのフッ化マグネシウム結晶体を同時に接合した構造体の正面の写真、（ｂ）は同構造体の背面の写真であり、これらの写真から接合後には上記の干渉縞が全く観察されず、光学的な境界面が認められないことが分かる。 Fig. 4 (a) is a photograph of the front of the structure in which three magnesium fluoride crystals are bonded simultaneously, and (b) is a photograph of the back of the structure. It is not observed at all, and it can be seen that no optical interface is recognized.
実施例ではフッ化マグネシウム結晶体片同士を接合した例を示したが、本発明方法はフッ化マグネシウム結晶体と合成コランダム片、或いはフッ化マグネシウム結晶体とフッ化カルシウム結晶体片との接合にも応用することができる。 In the examples, magnesium fluoride crystal pieces were joined to each other. However, the method of the present invention can be used to join magnesium fluoride crystals and synthetic corundum pieces, or magnesium fluoride crystals and calcium fluoride crystal pieces. Can also be applied.
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.
１、２…フッ化マグネシウム結晶体片、３…スペーサ、４…押圧治具。
1, 2 ... Magnesium fluoride crystal piece, 3 ... spacer, 4 ... pressing jig.
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| JP2017026513A JP6892198B2 (en) | 2017-02-16 | 2017-02-16 | Joining method of magnesium fluoride crystals |
| PCT/JP2017/009149 WO2017154950A1 (en) | 2016-03-08 | 2017-03-08 | Method for joining crystal body |
| EP17763290.8A EP3428326B1 (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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