JP2018194085A - Gate seal structure for semiconductor manufacturing device, and manufacturing method thereof - Google Patents

Abstract

PROBLEM TO BE SOLVED: To securely fix a fluororubber sealing member inside an annular groove formed in a metal plate-shaped member. SOLUTION: A gate for a semiconductor manufacturing apparatus including a metal plate-shaped member 10a having an annular groove 5 formed on its surface and a fluororubber annular seal member 15 provided inside the annular groove 5. In the seal structure 20, the average roughness Rc of the roughness curve element is 50 μm to 500 μm, and the skewness Rsk of the roughness curve is -3 to 0.5 on at least a part of the inner surface of the annular groove 5. The rough surface portion R is provided, and the seal member 15 is joined to the rough surface portion R of the annular groove 5. [Selection diagram] Fig. 2

Description

  The present invention relates to a gate seal structure for a semiconductor manufacturing apparatus and a manufacturing method thereof.

  Many semiconductor manufacturing apparatuses have a vacuum chamber. The vacuum chamber is provided with a gate for taking in and out an object to be processed such as a wafer. The gate is provided with a seal structure that opens and closes the gate. The seal structure includes, for example, a metal plate-like member having an annular groove formed on the surface thereof, and a fluororubber seal member provided inside the annular groove. Here, although fluororubber is excellent in chemical resistance, it is difficult to adhere to a metal surface with an adhesive, for example, due to its properties.

  Therefore, for example, Patent Document 1 proposes that the adhesive layer is a two-layer structure including a vulcanized adhesive layer containing a silane coupling agent and a fluororubber layer.

JP 2000-272045 A

  By the way, in a conventional gate seal structure for a semiconductor manufacturing apparatus, when a metal plate-like member and a fluororubber seal member are fixed by vulcanization adhesion using an adhesive, the adhesion of fluororubber is extremely low. Therefore, the adhesive force between the plate-like member and the seal member is low, and the seal member may fall off due to, for example, the gate opening / closing operation. Therefore, there is a demand for a gate seal structure for a semiconductor manufacturing apparatus in which a fluororubber seal member fixed inside an annular groove formed in a metal plate-like member does not fall off even when the gate is opened and closed.

  The present invention has been made in view of such points, and the object of the present invention is to securely fix a fluororubber seal member inside an annular groove formed in a metal plate member. is there.

  In order to achieve the above object, a gate seal structure for a semiconductor manufacturing apparatus according to the present invention includes a metal plate-like member having an annular groove formed on a surface thereof, and a fluoro rubber provided inside the annular groove. A gate seal structure for a semiconductor manufacturing apparatus comprising an annular seal member made of an annular groove, wherein at least part of the inner surface of the annular groove has an average roughness Rc of a roughness curve element of 50 μm to 500 μm. Further, a rough surface portion having a roughness curve skewness Rsk of −3 to 0.5 is provided, and the sealing member is bonded to the rough surface portion of the annular groove.

  According to said structure, the rough surface part which has predetermined | prescribed roughness is provided in at least one part of the inner surface of the annular groove in the surface of a metal plate-shaped member. Here, the rough surface portion having a predetermined roughness has a roughness curve element having an average roughness Rc of 50 μm to 500 μm (preferably 80 μm to 400 μm, more preferably 100 μm to 300 μm), and a roughness meaning a degree of distortion. Since the skewness Rsk of the curve is −3 to 0.5 (preferably −1.5 to 0.4, more preferably −1.0 to 0.3), the rough surface portion of the inner surface of the annular groove and the seal member Are joined in a deeply fitted state, and the rough surface portion of the inner surface of the annular groove and the seal member can be reliably fixed. Therefore, the fluororubber sealing member can be reliably fixed inside the annular groove formed in the metal plate member. Here, when Rc is smaller than 50 μm, since the fitting between the rough surface portion of the inner surface of the annular groove and the seal member becomes shallow, the anchor effect of fitting the rough surface portion of the inner surface of the annular groove and the seal member is ineffective. It will be enough. Further, when Rc is larger than 500 μm, it becomes difficult to completely fill the concave portion of the rough surface portion of the inner surface of the annular groove with the seal member, and the fitting of the rough surface portion of the inner surface of the annular groove and the seal member becomes difficult. Therefore, the anchor effect for fitting the rough surface portion of the inner surface of the annular groove and the seal member becomes insufficient. Further, when Rsk is smaller than −3, it becomes difficult to completely fill the concave portion of the rough surface portion of the inner surface of the annular groove with the seal member, and the rough surface portion of the inner surface of the annular groove and the seal member are fitted. Since the fit becomes shallow, the anchor effect of fitting the rough surface portion of the inner surface of the annular groove and the seal member becomes insufficient. In addition, when Rsk is larger than 0.5, the seal member can be easily removed from the rough surface portion of the inner surface of the annular groove, so that the anchor effect of fitting the rough surface portion of the inner surface of the annular groove and the seal member is insufficient. Become.

  Further, the kurtosis (Rku) of the roughness curve meaning the kurtosis of the rough surface portion is preferably 1.5 to 5.0, more preferably 2.0 to 4.0. Here, when Rku is 1.5 or more, it becomes difficult for the sealing member to come off from the rough surface portion of the inner surface of the annular groove. Further, when Rku is 5.0 or less, stress concentration starting from the apex of the convex portion in the rough surface portion of the inner surface of the annular groove is less likely to occur, and therefore the peel strength between the rough surface portion and the seal member is low. Stabilize. Furthermore, the average length (Rsm) of the roughness curve element of the rough surface portion is preferably 10 μm to 100 μm, and more preferably 20 μm to 70 μm. Here, when Rsm is 10 μm to 100 μm, the peel strength within the fixed interface between the rough surface portion and the seal member is stabilized.

  The peel strength between the rough surface portion of the annular groove and the seal member according to JIS K6256-2 may be higher than the material breaking strength of the seal member.

  According to said structure, since the peeling state of the rough surface part of the inner surface of an annular groove and a sealing member is destruction of a seal member, a sealing member is thickness of a plate-shaped member with respect to the rough surface part of the inner surface of an annular groove. Even if it is going to be peeled in the vertical direction, at least a part of the seal member is destroyed before the rough surface portion of the inner surface of the annular groove and the seal member are peeled off. As a result, separation between the rough surface portion of the inner surface of the annular groove and the fluororubber seal member is suppressed, so that the fluororubber seal member is formed inside the annular groove formed in the metal plate member. Can be securely fixed.

Note that the gate seal structure for a semiconductor manufacturing apparatus having the above-described structure has a transmission amount in a helium leak test (JIS Z2331) by a vacuum envelope method, for example, 1.0 × 10 ⁻⁷ Pa · m ³ / s to Since it is about 1.0 × 10 ⁻⁵ Pa · m ³ / s, it has the same level of sealing performance as a gate seal structure using an adhesive.

  Moreover, the gate seal structure for a semiconductor manufacturing apparatus having the above-described configuration can be manufactured by the following manufacturing method.

  A method for manufacturing a gate seal structure for a semiconductor manufacturing apparatus according to the present invention, comprising: irradiating at least a part of an inner surface of a circular groove of a metal plate having a circular groove formed on a surface thereof; A plate-shaped member manufacturing step of forming a plate-shaped member by forming a rough surface portion having an average roughness Rc of the roughness curve element of 50 μm to 500 μm and a skewness Rsk of the roughness curve of −3 to 0.5; A molding composition preparation step for preparing a fluorine-containing elastomer composition as a molding composition, and after the molding composition is disposed inside the annular groove of the plate-like member, the molding composition is And a molding step of forming a seal member inside the annular groove of the plate-like member by heating and pressurizing between the plate-like member and the molding die.

  You may provide the reheating process which reheats the said sealing member after the said shaping | molding process.

  According to the present invention, the average roughness Rc of the roughness curve element is 50 μm to 500 μm and the skewness Rsk of the roughness curve is −3 on at least a part of the inner surface of the annular groove of the metal plate member. A rough surface portion of ~ 0.5 is provided, and the seal member is joined to the rough surface portion, so that the fluoro rubber seal member is securely fixed inside the annular groove formed in the metal plate member. can do.

1 is a plan view of a gate seal structure for a semiconductor manufacturing apparatus according to a first embodiment of the present invention. It is sectional drawing of the gate seal structure for semiconductor manufacturing apparatuses along the II-II line | wire in FIG. It is sectional drawing of the plate-shaped member which comprises the 1st modification of the gate seal structure for semiconductor manufacturing apparatuses concerning the 1st Embodiment of this invention. It is sectional drawing of the plate-shaped member which comprises the 2nd modification of the gate seal structure for semiconductor manufacturing apparatuses concerning the 1st Embodiment of this invention. It is sectional drawing of the plate-shaped member which comprises the 3rd modification of the gate seal structure for semiconductor manufacturing apparatuses which concerns on the 1st Embodiment of this invention. It is sectional drawing of the plate-shaped member which comprises the 4th modification of the gate seal structure for semiconductor manufacturing apparatuses which concerns on the 1st Embodiment of this invention. It is sectional drawing which shows the plate-shaped member preparation process in the manufacturing method of the gate seal structure for semiconductor manufacturing apparatuses which concerns on the 1st Embodiment of this invention. It is sectional drawing which shows the formation process in the manufacturing method of the gate seal structure for semiconductor manufacturing apparatuses concerning the 1st Embodiment of this invention. In Example 1 of the 1st Embodiment of this invention, it is a roughness curve of the rough surface part formed in the aluminum plate. In the comparative example 1 of the 1st Embodiment of this invention, it is the roughness curve of the rough surface part formed in the aluminum plate. In the comparative example 2 of the 1st Embodiment of this invention, it is a roughness curve of the rough surface part formed in the aluminum plate.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. The present invention is not limited to the following embodiments.

<< First Embodiment >>
1 to 11 show a first embodiment of a gate seal structure for a semiconductor manufacturing apparatus according to the present invention. Here, FIG. 1 is a plan view of the gate seal structure 20 for the semiconductor manufacturing apparatus of the present embodiment, and FIG. 2 is a view of the gate seal structure 20 taken along the line II-II in FIG. It is sectional drawing. 3 to 6 are cross-sectional views of the plate-like member 10b constituting the first to fourth modifications of the gate seal structure 20.

  As shown in FIGS. 1 and 2, the gate seal structure 20 includes a substantially rectangular plate-like member 10a and a seal member 15 (see FIG. 2) provided inside an annular groove 5 described later on the surface of the plate-like member 10a. 1).

  Each corner of the plate-like member 10a is subjected to R processing as shown in FIG. Further, as shown in FIGS. 1 and 2, an annular groove 5 is formed in a frame shape along the periphery of one surface of the plate-like member 10a. Here, the plate-like member 10a is made of a metal such as aluminum, an aluminum alloy, or stainless steel, for example.

  At least a part of the inner surface of the annular groove 5 has an average roughness Rc of 50 μm to 500 μm and a roughness curve skewness Rsk of −3 to 0.5, as shown in FIG. A rough surface portion R is provided. Here, as shown in FIG. 7 to be described later, the rough surface portion R can be formed by irradiating the inner surface of the annular groove 5 of the metal plate 10 serving as the plate member 10a with the laser light L. In the present embodiment, as shown in FIG. 2, the configuration in which the rough surface portion R is provided on the entire bottom surface 5a of the annular groove 5 is illustrated, but the rough surface portion R is, for example, in the width direction of the annular groove 5 and / or Alternatively, it may be provided on a part of the bottom surface 5a of the annular groove 5 such as a part in the circumferential direction. Moreover, in this embodiment, although the plate-shaped member 10a with which the side surface 5b of the annular groove 5 stood up was illustrated, as shown in FIGS. 3-6, the plate-like member 10a inclined the side surface 5b of the annular groove 5 The plate-like member 10b may be used. Here, in the plate-like member 10b of FIG. 3, the rough surface portion R is provided on the entire bottom surface 5a and the entire side surface 5b of the annular groove 5. Further, in the plate-like member 10b of FIG. 4, the rough surface portion R is provided on the entire side surface 5b of the annular groove 5. Further, in the plate-like member 10b of FIG. 5, the rough surface portion R is provided at the center portion of the bottom surface 5a of the annular groove 5 and the upper portion of the side surface 5b. Moreover, in the plate-shaped member 10b of FIG. 6, the rough surface part R is provided in the upper part of the bottom face 5a of the annular groove 5, and the side surface 5b. Thus, according to the plate-like member 10b, for example, the side surface 5b of the annular groove 5 can be easily irradiated with a laser beam for roughening, so that not only the bottom surface 5a but also the side surface 5b of the annular groove 5 can be easily formed. If the surface can be roughened and a desired effect can be obtained, the area where the rough surface portion R is provided can be reduced.

  As shown in FIG. 1, the seal member 15 is provided in an annular shape (frame shape), and is made of, for example, fluororubber obtained by vulcanizing a fluorine-containing elastomer composition. Here, the lower portion of the seal member 15 is joined to a rough surface portion R provided on the inner surface of the annular groove 5 of the plate-like member 10a.

  As the fluorine-containing elastomer constituting the fluorine-containing elastomer composition, known ones can be used. Hexafluoropropylene-vinylidene fluoride copolymer, hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer Tetrafluoroethylene-perfluoroalkyl ether copolymers are preferred, and hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymers and tetrafluoroethylene-perfluoroalkyl ether copolymers are particularly preferred.

  The fluorine-containing elastomer composition contains a vulcanizing agent (crosslinking agent) for vulcanizing the fluorine-containing elastomer. Here, as the vulcanizing agent, for example, a polyol vulcanizing agent or an organic peroxide vulcanizing agent can be appropriately selected and used in accordance with the fluorine-containing elastomer to be used.

  The fluorine-containing elastomer composition may contain a crosslinking aid. Here, as the crosslinking aid, quinone dioxime (p-quinone dioxime etc.), methacrylate (triethylene glycol dimethacrylate, methyl methacrylate, trimethylolpropane trimethacrylate etc.), allyl (diallyl phthalate) , Triallyl cyanurate, triallyl isocyanurate, triallyl trimellitate, etc.), maleimide (maleimide, phenylmaleimide, N, N′-m-phenylenebismaleimide, etc.), maleic anhydride, divinylbenzene, vinyltoluene, It is selected from polyfunctional unsaturated compounds such as 1,2-polybutadiene and the like, and can be used alone or in combination of two or more.

  The fluorine-containing elastomer composition may contain a filler. Here, as the filler, carbon black, barium sulfate, silica, aluminum oxide, aluminum silicate, titanium dioxide, or the like can be used. From the oxygen plasma resistance, barium sulfate, silica, aluminum oxide, aluminum silicate, carbon dioxide, etc. Titanium or the like can be used. These fillers may be used in combination. Among these fillers, barium sulfate and silica are preferable, and silica is more preferable. Here, among the silica, synthetic amorphous silica such as dry silica and wet silica is preferable, dry silica such as hydrophilic dry silica and hydrophobic dry silica is more preferable, and hydrophobic dry silica is more preferable.

  In addition, a stabilizer, a plasticizer, a lubricant, a processing aid, and the like may be added to the fluorine-containing elastomer composition.

  The specific compounding example of the said fluorine-containing elastomer composition is shown below.

-Polyol vulcanization system-
The fluorine-containing elastomer composition is a polyol-vulcanizable fluorine-containing elastomer (for example, a polyol-vulcanizable hexafluoropropylene-vinylidene fluoride copolymer and / or a polyol-vulcanizable hexafluoropropylene-vinylidene fluoride-tetra. A composition obtained by blending 30 parts by weight to 100 parts by weight of barium sulfate with 100 parts by weight of fluoroethylene copolymer) is preferred, and sulfuric acid with respect to 100 parts by weight of the fluorine-containing elastomer capable of polyol vulcanization. A composition obtained by blending 30 to 100 parts by weight of barium and 0.5 to 30 parts by weight of tetrafluoroethylene resin is more preferable. Here, when the blending amount of the tetrafluoroethylene resin is less than 0.5 parts by weight, the effect of improving the plasma resistance is small, and when it exceeds 30 parts by weight, mechanical properties such as tensile strength and elongation are exhibited. It tends to decrease. Therefore, a more preferable blending amount of the tetrafluoroethylene resin is 1 to 20 parts by weight. Moreover, as a polyol vulcanizing agent, a well-known thing can be used, for example, bisphenol AF is used. The polyol vulcanizing agent is preferably blended in an amount of 0.5 to 5 parts by weight, more preferably 1 to 2 parts by weight, based on 100 parts by weight of the fluorinated elastomer capable of polyol vulcanization. As the accelerator and acid acceptor, quaternary phosphonium salts, quaternary ammonium salts, calcium hydroxide, magnesium oxide and the like are used.

  The fluorine-containing elastomer composition may contain a filler, and as the filler, carbon black, silica, titanium oxide, lead oxide, zinc oxide, magnesium oxide, diatomaceous earth, alumina, calcium oxide, oxidation Oxides such as iron, tin oxide, antimony oxide, ferrites, hydroxides such as magnesium hydroxide, aluminum hydroxide, calcium hydroxide, basic magnesium carbonate, calcium carbonate, barium carbonate, magnesium carbonate, zinc carbonate, dosonite , Carbonates such as hydrotalcite, sulfates such as barium sulfate and calcium sulfate, aluminum silicate (clay, karionite, pyrophyllite), magnesium silicate (talc), calcium silicate (wollastonite, zonotlite), Clay, montmorillonite, bentona DOO, activated clay, silicates such as mica, aluminum nitride, boron nitride, and a nitride such as silicon nitride. These fillers can be used alone or in combination of two or more.

-Peroxide vulcanization system-
The fluorine-containing elastomer composition is preferably a composition obtained by blending a peroxide vulcanizing agent such as an organic peroxide with a peroxide-vulcanizable fluorine-containing elastomer. Here, the organic peroxide vulcanizing agent can be used without particular limitation as long as it is generally used as an elastomer vulcanizing agent. For example, dibenzoyl peroxide, 1,1-bis ( t-butylperoxy) -3,3,5-trimethylcyclohexane, 1,1-bis (t-butylperoxy) cyclododecane, n-butyl-4,4-bis (t-butylperoxy) valerate, dic Milperoxide, t-butylperoxybenzoate, 1,3-bis (t-butylperoxyisopropyl) benzene, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, 2,5- Examples thereof include dimethyl-2,5-di (t-butylperoxy) hexyne-3, and one or two or more of these can be selected and used.

  The amount of the organic peroxide vulcanizing agent is preferably 0.5 to 10 parts by weight, more preferably 1 to 5 parts by weight, based on 100 parts by weight of the peroxide-crosslinkable fluorine-containing elastomer. Parts, more preferably 1.5 to 3 parts by weight. Here, when the blending amount of the organic peroxide vulcanizing agent is 0.5 parts by weight or more, it is preferable in terms of compression set of a rubber member obtained by vulcanizing the fluorine-containing elastomer composition. When the blending amount of the oxide vulcanizing agent is 10 parts by weight or less, it is preferable in terms of moldability of the fluorine-containing elastomer composition.

  The fluorine-containing elastomer composition may contain a crosslinking aid in addition to the organic peroxide vulcanizing agent. Here, the crosslinking aid can be used without particular limitation as long as it is generally used as a crosslinking aid for elastomers. For example, quinone dioxime (p-quinone dioxime, etc.), methacrylate (Triethylene glycol dimethacrylate, methyl methacrylate, trimethylolpropane trimethacrylate, etc.), allyl (diallyl phthalate, triallyl cyanurate, triallyl isocyanurate, triallyl trimellitate, etc.), maleimide (maleimide, phenylmaleimide, N, N′-m-phenylene bismaleimide, etc.), maleic anhydride, divinylbenzene, vinyltoluene, or monomers having a plurality of carbon-carbon unsaturated groups such as 1,2-polybutadiene (polyfunctional monomers). One of these or Can be selected and used over seeds, it can be preferably used triallyl isocyanurate.

  The content of the crosslinking aid is preferably 1 part by weight to 10 parts by weight, more preferably 2 parts by weight to 6 parts by weight, and still more preferably 2 parts per 100 parts by weight of the fluorine-containing elastomer capable of peroxide crosslinking. .5 to 4 parts by weight. Here, when the content of the crosslinking aid is 1 part by weight or more, it is preferable in terms of compression set characteristics of a rubber member obtained by vulcanizing the fluorine-containing elastomer composition. Moreover, it is preferable at the point of the moldability of the fluorine-containing elastomer composition of this invention that content of a crosslinking adjuvant is 10 weight part or less.

  The fluorine-containing elastomer composition may further contain a filler. In the elastomer composition, the filler is used for the purpose of reinforcing the elastomer, increasing the weight, improving processability, and the like.

  Examples of the filler include synthetic fibers such as polyacrylonitrile, nylon, and polyester, wood powder, pulp, cork powder, polystyrene latex, urea-formaldehyde particles, polyethylene-powder synthetic resins, polytetrafluoroethylene, tetrafluoro, and the like. Organic fillers such as fluororesin powders such as ethylene / perfluoroalkyl vinyl ether copolymer, tetrafluoroethylene / hexafluoropropylene copolymer, polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride, carbon black, white Silica such as carbon, silicic acid, diatomaceous earth, calcined diatomaceous earth, quartzite, quartz sand, cristobalite, calcium silicate, magnesium silicate, aluminum silicate, kaolinite, kaolin clay (kaori And quartz), calcined clay (metakaolin), talc, muscovite, sericite, wollastonite, serpentine, pyrophyllite and other silicates, aluminum oxide, titanium oxide, magnesium oxide, zinc oxide and other metal oxides And inorganic fillers such as carbonates, such as calcium carbonate, magnesium carbonate, barium carbonate, and dolomite. Among these, carbon black, graphite, silicic acid, aluminum oxide, titanium oxide, magnesium oxide, zinc oxide, calcium silicate, magnesium silicate, aluminum silicate, barium sulfate, calcium sulfate, calcium carbonate, magnesium carbonate, barium carbonate Inorganic fillers such as, and fluororesin powder are preferably used, and silicic acid is more preferably used. In addition, 1 type, or 2 or more types can be selected and used for a fluorine-containing elastomer composition from these fillers.

  As said silicic acid, if it is generally used as a filler of an elastomer, it can select and use 1 type (s) or 2 or more types without a restriction | limiting in particular.

The SiO ₂ purity of the silicic acid is not particularly limited, but is preferably 99% or more. Here, when the fluorine-containing elastomer composition contains silicic acid having a SiO ₂ purity of 99% or more, when a sealing member obtained by vulcanizing this is used for manufacturing a semiconductor or a flat panel display, a rubber component Metal contamination due to the impurity components (heavy metal, arsenic, magnesium, calcium, sodium, etc.) is extremely difficult to occur.

  As the silicic acid, synthetic amorphous silica such as dry silica and wet silica is preferable, dry silica such as hydrophilic dry silica and hydrophobic dry silica is more preferable, and hydrophobic dry silica is more preferable. The average primary particle size of silicic acid is not particularly limited, but is preferably 5 nm to 500 nm, more preferably 7 nm to 100 nm. Here, when the average primary particle diameter of silicic acid is 5 nm or more, it is preferable from the viewpoint of dispersibility of the fluorine-containing elastomer composition, and when the average primary particle diameter of silicic acid is 500 nm or less, the fluorine-containing elastomer composition is This is preferable from the viewpoint of physical strength of the rubber member obtained by vulcanization. In addition, an average primary particle diameter is the value calculated | required from the diameter of the electron micrograph of 3000-5000 silicic acid particles, and measuring those.

Specific surface area of the silica is not particularly limited, it is preferably ^{20m 2} / ^g~500m 2 / g, more preferably ^{30m 2} / ^g~400m 2 / g. Here, when the specific surface area of silicic acid is 20 m ² / g or more, it is preferable from the viewpoint of physical strength of a rubber member obtained by vulcanizing the fluorine-containing elastomer composition, and is 500 m ² / g or less. From the viewpoint of moldability of the fluorine-containing elastomer composition. The specific surface area is a value measured by the BET method.

  A commercially available product can be used as the silicic acid. Here, the commercially available products include “Aerosil OX50”, “Aerosil 50”, “Aerosil 90G”, “Aerosil 130”, “Aerosil 200”, “Aerosil 300”, “Aerosil R380”, “Aerosil R972”, “ "Aerosil R974", "Aerosil R976", "Aerosil RY50", "Aerosil NAX50", "Aerosil NX90G", "Aerosil RX200", "Aerosil RX300" (above, manufactured by Nippon Aerosil Co., Ltd.), "Nip seal AQ", "Nip seal" VN3 "," Nip seal LP "," Nip seal ER "," Nip seal NS "," Nip seal NA "," Nip seal KQ "," Nip seal KM "," Nip seal KP "," Nip seal E-75 "," Nip seal E-743 " "Nip seal E-150J", "Nip seal E-170", "Nip seal E-200", "Nip seal K-500", "Nip seal L-250", "Nip seal G-300" (above, Tosoh Silica Corporation Manufactured). In the said fluorine-containing elastomer composition, 1 type (s) or 2 or more types can be selected and used from said silicic acid.

  The content of the filler is not particularly limited, but is preferably 1 part by weight to 100 parts by weight, more preferably 2 parts by weight to 60 parts by weight, with respect to 100 parts by weight of the fluorine-containing elastomer capable of peroxide crosslinking. More preferably, it is 2.5 to 40 parts by weight. Here, when the content of the filler is 1 part by weight or more, it is preferable from the viewpoint of mixing processability of the fluorine-containing elastomer composition, and when it is 100 parts by weight or less, the point of molding processability of the fluorine-containing elastomer composition. Is preferable.

  Examples of the fluorine-containing elastomer composition include an anti-aging agent (for example, an amine-based anti-aging agent (phenyl-1-naphthylamine, octylated diphenylamine, etc.), a phenol-based anti-aging agent (mono (α-methylbenzyl) phenol, 2,6-di-t-butyl-4-methylphenol, etc.), imidazole anti-aging agents (2-mercaptobenzimidazole, 2-mercaptomethylbenzimidazole etc.), etc.), plasticizers (for example, phthalic acid plasticizers) (Dioctyl phthalate, etc.), adipic acid type plasticizer (dioctyl adipate, etc.), sebacic acid type plasticizer (dioctyl sebacate, etc.), trimellitic acid type plasticizer (trimellitate, etc.), polymerization type plasticizer (eg, polyether) Or polymerization plasticizers such as polyester)), processing aids (eg stearic acid or A metal salt thereof, may be added as necessary palmitic acid or a metal salt thereof, a compounding agent that is commonly used in paraffin wax) such as rubber industry. In addition, the addition amount of each compounding agent can be appropriately set as necessary as long as the object of the present invention is not impaired.

-Tetrafluoroethylene-perfluoroalkyl ether copolymer system-
The fluorine-containing elastomer composition is preferably a composition obtained by blending a crosslinkable tetrafluoroethylene-perfluoroalkyl ether copolymer having a cured site with a curing agent and a filler.

  When the tetrafluoroethylene-perfluoroalkyl ether copolymer contains a copolymer unit of a nitrile-containing cure site monomer, a curing system based on an organotin compound can be used. Here, suitable organotin compounds include allyl-, propargyl-, triphenyl-, and allenyltin curing agents. Tetraalkyltin compounds or tetraallyltin compounds are also preferred curing agents for use in combination with nitrile substitution cure sites. The amount of the curing agent to be used varies depending on the degree of crosslinking desired for the final product and the type and concentration of the reactive moiety in the crosslinkable tetrafluoroethylene-perfluoroalkyl ether copolymer. Specifically, the compounding amount of the curing agent is preferably 0.5 to 10 parts by weight, more preferably 1 to 100 parts by weight of the crosslinkable tetrafluoroethylene-perfluoroalkyl ether copolymer. Parts by weight to 4 parts by weight. In the tetrafluoroethylene-perfluoroalkyl ether copolymer containing copolymerized units of a nitrile-containing cure site monomer, the nitrile group is trimerized and a curing agent such as organic tin is present to form an s-triazine ring. By forming, it is considered that the perfluoroelastomer is cross-linked.

  As the curing agent, 4,4 ′-[2,2,2-trifluoro-1- (trifluoromethyl) ethylidene] bis (2-aminophenol), 4,4′-sulfonylbis (2-aminophenol) 3,3′-diaminobenzidine, 3,3 ′, 4,4′-tetraaminobenzophenone, etc., and one or more of these curing agents can be selected and used.

  The content of the curing agent is preferably 0.5 parts by weight to 5 parts by weight and more preferably 1 part by weight to 2 parts by weight with respect to 100 parts by weight of the fluorine-containing elastomer. Here, the content of the curing agent is preferably 0.5 parts by weight or more from the viewpoint of compression set characteristics of a rubber member obtained by vulcanizing the fluorine-containing elastomer composition. Moreover, it is preferable at the point of the moldability of the fluorine-containing elastomer composition of this invention that content of a hardening | curing agent is 5 weight part or less.

  Other curing agents suitable for vulcanizing tetrafluoroethylene-perfluoroalkyl ether copolymers having nitrile cure sites include ammonium, inorganic or organic acid ammonium salts (eg, ammonium perfluorooctanoate). And compounds that decompose to produce ammonia (for example, urea).

  When the curing site is a nitrile, iodine or bromine group, an organic peroxide can be used. As the organic peroxide, those which generate free radicals at the curing temperature are preferable. For example, 2,5-dimethyl-2,5-di (tertiarybutylperoxy) -hexyne-3,2,5 -Dimethyl-2,5-di (tertiary butyl peroxy) -hexane, dicumyl peroxide, dibenzoyl peroxide, tertiary butyl perbenzoate, di [1,3-dimethyl-3- (t-butyl peroxy) 1) -Butyl] carbonate or the like can be selected and used. Here, the compounding amount of the organic peroxide is preferably 1 part by weight to 3 parts by weight with respect to 100 parts by weight of the fluorine-containing elastomer composition. In addition, it is preferable at the point of the compression set characteristic of the rubber member formed by vulcanizing a fluorine-containing elastomer composition that the compounding quantity of an organic peroxide is 1 weight part or more. Moreover, it is preferable at the point of the moldability of the fluorine-containing elastomer composition of this invention that the compounding quantity of an organic peroxide is 3 weight part or less.

  Other materials that are usually blended with the composition as part of the organic peroxide cure system can contain a crosslinking aid.

  As the crosslinking aid, a polyfunctional unsaturated compound is preferable. Here, the blending amount of the crosslinking aid is preferably 0.1 to 10 parts by weight, and more preferably 2 to 5 parts by weight with respect to 100 parts by weight of the fluorine-containing elastomer composition. Examples of the crosslinking aid include triallyl cyanurate, triallyl isocyanurate, tri (methylallyl) isocyanurate, tris (diallylamine) -s-triazine, triallyl phosphite, N, N-diallylacrylamide, hexaalkylphospho Luamide, N, N, N ′, N′-tetraalkyltetraphthalamide, N, N, N ′, N′-tetraallylmalonamide, trivinyl isocyanurate, 2,4,6-trivinylmethyltrisiloxane One or more compounds selected from compounds such as tri (5-norbornene-2-methylene) cyanurate can be used.

  Depending on the curing site present, a double curing system can also be used. For example, a fluorine-containing elastomer having a copolymerized unit of a nitrile-containing cure site monomer can be cured using a combination of the organic peroxide and the crosslinking aid. Specifically, it is preferable to use 0.3 to 5 parts by weight of a crosslinking aid and 0.1 to 10 parts by weight of an organic curing agent with respect to 100 parts by weight of the fluorine-containing elastomer composition.

  Fluorine-containing elastomer compositions include commonly used fillers (for example, carbon black, barium sulfate, silica, aluminum oxide, aluminum silicate and titanium dioxide), stabilizers, plasticizers, lubricants, processing aids, etc. You may mix | blend an additive.

  The gate seal structure 20 described above is configured to close the gate when the surface of the seal member 15 contacts the peripheral edge of the gate provided in the vacuum chamber of the semiconductor manufacturing apparatus.

  Next, the manufacturing method of the gate seal structure 20 of this embodiment is demonstrated. Here, FIGS. 7 and 8 are cross-sectional views showing a plate-shaped member manufacturing process and a molding process in the method for manufacturing the gate seal structure 20. In addition, the manufacturing method of the gate seal structure 20 of this embodiment is provided with a plate-shaped member production process, a molding composition preparation process, and a molding process.

<Plate-shaped member manufacturing process>
First, for example, an aluminum metal plate 10 having an annular groove 5 formed on the surface thereof is prepared. Subsequently, with respect to at least a part of the inner surface of the annular groove 5 of the metal plate 10 (for example, the bottom surface 5a), using a continuous wave or pulse wave laser as shown in FIG. The laser beam L is irradiated at an irradiation speed of about 50000 mm / sec. Thereby, the plate-shaped member 10a which has the rough surface part R in the inner surface of the annular groove 5 is produced. Here, as a continuous wave laser, a known laser can be used. For example, a YVO ₄ laser, a fiber laser (preferably a single mode fiber laser), an excimer laser, a carbon dioxide gas laser, an ultraviolet laser, a YAG laser, a semiconductor. A laser, a glass laser, a ruby laser, a He—Ne laser, a nitrogen laser, a chelate laser, a dye laser, or the like can be used. Moreover, as a pulse wave laser, a well-known thing can be used, for example, a nanosec pulse laser, a millisec pulse laser, etc. can be used. The output of the laser beam is, for example, about 4 W to 4000 W in the case of a continuous wave laser, and about 5000 W to 30000 W in the case of a pulse wave laser. The wavelength of the laser light is, for example, about 300 nm to 1200 nm. The beam diameter of the laser light is, for example, about 5 μm to 200 μm.

<Molding composition preparation process>
For molding by mixing the above-mentioned fluorine-containing elastomer, vulcanizing agent (crosslinking agent, curing agent), filler and other additives by known mixing (kneading) methods such as roll mixing, kneader mixing, and banbury mixing. A fluorine-containing elastomer composition 15a (see FIG. 8) is prepared as a composition. Here, in the fluorine-containing elastomer composition 15a, the minimum value ML of the vulcanization curve at a press temperature (165 ° C.) determined in accordance with JIS K6300-2 is preferably 0.1 kg · cm to 10.0 kg · cm. More preferably 0.5 kg · cm to 5 kg · cm, and still more preferably 1.0 kg · cm to 3.0 kg. cm. If the minimum value ML of the vulcanization curve is 0.1 kg · cm or more, the filling property of the rough surface portion R at the pressing temperature of the fluorine-containing elastomer composition is improved, and the minimum value ML of the vulcanization curve is improved. If it is 10.0 kg or less, the seal molding processability is improved.

<Molding process>
After disposing the fluorine-containing elastomer composition 15a prepared in the molding composition preparation step in the annular groove 5 of the plate member 10a prepared in the plate member preparation step, as shown in FIG. The fluorinated elastomer composition 15a is molded by heating and pressurizing with a molding die M, so that the fluorinated elastomer is filled in the concave portion of the rough surface portion R of the inner surface of the annular groove 5 (vulcanized (crosslinked, cured). ) To form the seal member 15. Further, after the sealing member 15 is removed from the mold M, the sealing member 15 may be reheated to perform secondary vulcanization (crosslinking and curing) of the sealing member 15. Here, the hardness of the formed sealing member 15 is preferably A60 to A90 with a type A durometer, more preferably A65 to A85, and further preferably A70 to A80. In addition, it is preferable that the hardness of the sealing member 15 is A60 or more because rubber remains in the entire concave portion of the rough surface portion R after peeling. Moreover, it is preferable that the hardness of the seal member 15 is A90 or less because the seal member 15 is difficult to break when stress concentration occurs on the surface side edge of the concave portion of the rough surface portion R during peeling.

  As described above, the gate seal structure 20 of the present embodiment can be manufactured.

  Next, a specific experiment will be described. Here, in this experiment, the gate seal of this embodiment is measured by measuring the peel strength between the aluminum plate on which the rough surface portion having a predetermined roughness is formed and the fluoro rubber constituting the seal member bonded thereto. The peel strength between the rough surface portion R on the inner surface of the annular groove 5 in the structure 20 and the seal member 15 was evaluated. 9, 10, and 11 are roughness curves of the rough surface portion formed on the aluminum plate in Example 1, Comparative Example 1, and Comparative Example 2 of the present embodiment.

<Example 1>
First, by irradiating one surface of an aluminum plate having a thickness of 2 mm, a width of 25 mm, and a length of 60 mm, the average roughness Rc of the roughness curve element is 185 μm, and the skewness Rsk of the roughness curve is A rough surface portion (see FIG. 9) of −0.63 was formed. Here, the kurtosis Rku of the roughness curve of the formed rough surface portion was 3.5, and the average length Rsm of the roughness curve element was 50.3 μm. Subsequently, based on JIS K6256-2, hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer having a thickness of 6 mm, a width of 25 mm, and a length of 120 mm is mainly applied to the rough surface portion of the aluminum plate on which the rough surface portion is formed. A test piece (adhesive not used) bonded with fluoro rubber filled into the concave portion of the rough surface by vulcanizing the fluorinated elastomer composition sheet as a component at 165 ° C. for 10 minutes under pressure ) Was produced. Then, when peel strength was measured with respect to the produced test piece based on JIS K6256-2, it was 142 N / 25 mm (destruction of the fluororubber main body). The ML of the fluorine-containing elastomer composition was 1.3 kgf · cm, and the hardness of the fluororubber was 73 with a type A durometer.

<Example 2>
First, in the same manner as in Example 1, a rough surface portion having an average roughness Rc of a roughness curve element of 190 μm and a roughness curve skewness Rsk of −0.38 is formed on one surface of an aluminum plate. did. Here, the kurtosis Rku of the roughness curve of the formed rough surface portion was 2.7, and the average length Rsm of the roughness curve element was 47.9 μm. Subsequently, based on JIS K6256-2, hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer having a thickness of 6 mm, a width of 25 mm, and a length of 120 mm is mainly applied to the rough surface portion of the aluminum plate on which the rough surface portion is formed. A test piece (adhesive not used) bonded with fluoro rubber filled into the concave portion of the rough surface by vulcanizing the fluorinated elastomer composition sheet as a component at 165 ° C. for 10 minutes under pressure ) Was produced. Then, when peel strength was measured with respect to the produced test piece based on JIS K6256-2, it was 133 N / 25mm (destruction of the fluororubber main body).

<Example 3>
First, in the same manner as in Example 1, a rough surface portion having an average roughness Rc of a roughness curve element of 244 μm and a skewness Rsk of a roughness curve of −0.57 is formed on one surface of an aluminum plate. did. Here, the kurtosis Rku of the roughness curve of the formed rough surface portion was 2.9, and the average length Rsm of the roughness curve element was 48.9 μm. Subsequently, on the rough surface portion of the aluminum plate on which the rough surface portion is formed, a tetrafluoroethylene-perfluoroalkyl ether copolymer having a thickness of 6 mm × width of 25 mm × length of 120 mm is a main component based on JIS K6256-2. Fluorine-containing elastomer composition sheet is pressure-pressed at 165 ° C for 10 minutes and vulcanized to produce a test piece (adhesive-free) joined with fluoro rubber filled in the concave portion of the rough surface portion did. Then, when peeling strength was measured with respect to the produced test piece based on JIS K6256-2, it was 70 N / 25mm (destruction of the fluororubber surface). The ML of the fluorine-containing elastomer composition was 7.5 kgf · cm, and the hardness of the fluororubber was 80 with a type A durometer.

<Comparative Example 1>
First, an average roughness Rc of the roughness curve element is 58 μm by irradiating one surface (width 25 mm × length 60 mm) of an aluminum plate having a thickness of 2 mm × width 25 mm × length 60 mm, And the rough surface part (refer FIG. 10) whose skewness Rsk of a roughness curve is -0.43 was formed. Here, the kurtosis Rku of the roughness curve of the formed rough surface portion was 3.7, and the average length Rsm of the roughness curve element was 31.6 μm. Subsequently, based on JIS K6256-2, hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer having a thickness of 6 mm, a width of 25 mm, and a length of 120 mm is mainly applied to the rough surface portion of the aluminum plate on which the rough surface portion is formed. A test piece (adhesive not used) bonded with fluoro rubber filled into the concave portion of the rough surface by vulcanizing the fluorinated elastomer composition sheet as a component at 165 ° C. for 10 minutes under pressure ) Was produced. Then, when peel strength was measured with respect to the produced test piece based on JIS K6256-2, it was 101.1 N / 25mm (interface peeling between an aluminum plate and fluororubber). The ML of the fluorine-containing elastomer composition was 1.3 kgf · cm, and the hardness of the fluororubber was 73 with a type A durometer.

<Comparative Example 2>
First, one surface (width 25 mm × length 60 mm) of an aluminum plate having a thickness of 2 mm × width 25 mm × length 60 mm is surface-treated with an etching solution so that the average roughness Rc of the roughness curve element is 12.2 μm. And a rough surface portion (see FIG. 11) having a roughness curve skewness Rsk of 0.62. Here, the kurtosis Rku of the roughness curve of the formed rough surface portion was 3.8, and the average length Rsm of the roughness curve element was 31.6 μm. Subsequently, on the rough surface portion of the formed aluminum plate, a hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer having a thickness of 6 mm, a width of 25 mm, and a length of 120 mm is mainly composed of JIS K6256-2. Fluorine-containing elastomer composition sheet is pressure-pressed at 165 ° C for 10 minutes and vulcanized to produce a test piece (adhesive-free) joined with fluoro rubber filled in the concave portion of the rough surface portion did. Then, when peel strength was measured with respect to the produced test piece based on JIS K6256-2, it was about 7.2 N / 25 mm. The ML of the fluorine-containing elastomer composition was 1.3 kgf · cm, and the hardness of the fluororubber was 73 with a type A durometer.

  Here, in Examples 1, 2, and 3 and Comparative Examples 1 and 2, the average roughness Rc of the roughness curve element, the skewness Rsk of the roughness curve, the kurtosis Rku of the roughness curve, and the average of the roughness curve elements The length Rsm was determined by analyzing the surface roughness in a 10 × lens line roughness analysis mode using a 3D measurement laser microscope (LEXT OLS4100) manufactured by Olympus Corporation.

  As an experimental result, a rough surface was formed in which the average roughness Rc of the roughness curve element was in the range of 185 μm to 244 μm, and the skewness Rsk of the roughness curve was in the range of −0.63 to −0.38. In Examples 1, 2, and 3, since the destruction of fluororubber was confirmed in the test according to JIS K6256-2, it can be said that the peel strength according to JIS K6256-2 is higher than the material fracture strength of the seal member. On the other hand, in Comparative Example 1 in which the average roughness Rc of the roughness curve element has a rough surface portion smaller than 185 μm, the peel strength according to JIS K6256-2 was a low level (about 110 N / 25 mm or less). Furthermore, in Comparative Example 2 in which a rough surface portion having a skewness RsK of a roughness curve larger than −0.38 was formed, the peel strength according to JIS K6256-2 was extremely low (several tens of N / 25 mm or less).

  As described above, according to the gate seal structure 20 for a semiconductor manufacturing apparatus of the present embodiment, at least a part of the inner surface of the annular groove 5 on the surface of the metal plate member 10a has a predetermined roughness. A rough surface portion R having the following is provided. Here, in the rough surface portion R having a predetermined roughness, the average roughness Rc of the roughness curve element is 50 μm to 500 μm, and the skewness Rsk of the roughness curve meaning the skewness is −3 to 0.5. Therefore, the rough surface portion R of the inner surface of the annular groove 5 and the seal member 15 are joined in a deeply fitted state, and the rough surface portion R of the inner surface of the annular groove 5 and the seal member 15 can be reliably fixed. Therefore, the fluororubber seal member 15 can be reliably fixed inside the annular groove 5 formed in the metal plate member 10a.

  In addition, according to the gate seal structure 20 for a semiconductor manufacturing apparatus of the present embodiment, the peeling state between the rough surface portion R of the inner surface of the annular groove 5 and the seal member 15 is destruction of the seal member 15. Even if the seal member 15 is to be peeled away from the rough surface portion R of the inner surface of the groove 5 in the thickness direction of the plate-like member 10a, before the rough surface portion R of the inner surface of the annular groove 5 and the seal member 15 are separated, At least a part of the seal member 15 is destroyed. As a result, peeling between the rough surface portion R on the inner surface of the annular groove 5 and the fluororubber seal member 15 is suppressed, so that fluorine is contained inside the annular groove 5 formed in the metal plate member 10a. The rubber seal member 15 can be securely fixed.

  Moreover, according to the gate seal structure 20 for a semiconductor manufacturing apparatus of the present embodiment, when the non-roughened surface portion that is not roughened is provided on the inner surface of the annular groove 5 formed in the plate-like member 10a, When the non-rough surface portion and the seal member 15 come into contact with each other, the sealing performance of the gate seal structure 20 can be improved.

<< Other Embodiments >>
In the above embodiment, the gate seal structure including the fluororubber seal member has been exemplified. However, the present invention includes, for example, a gate seal structure including another rubber seal member such as acrylonitrile-butadiene-rubber. It can also be applied to the body.

  As described above, the present invention can securely fix the fluororubber seal member inside the annular groove formed in the metal plate-like member. Useful.

L laser beam M molding die R rough surface portion 5 annular groove 10 metal plates 10a, 10b plate member 15 seal member 15a fluorinated elastomer composition (molding composition)
20 Gate seal structure

Claims (4)

A metal plate-like member having an annular groove formed on the surface;
A gate seal structure for a semiconductor manufacturing apparatus, comprising a fluororubber annular seal member provided inside the annular groove,
At least a part of the inner surface of the annular groove is provided with a rough surface portion having an average roughness Rc of the roughness curve element of 50 μm to 500 μm and a skewness Rsk of the roughness curve of −3 to 0.5,
The gate seal structure for a semiconductor manufacturing apparatus, wherein the seal member is joined to the rough surface portion of the annular groove. The gate seal structure for a semiconductor manufacturing apparatus according to claim 1,
A gate seal structure for a semiconductor manufacturing apparatus, wherein the peel strength between the rough surface portion of the annular groove and the seal member according to JIS K6256-2 is higher than the material breaking strength of the seal member. . A method for manufacturing a gate seal structure for a semiconductor manufacturing apparatus,
By irradiating at least a part of the inner surface of the annular groove of the metal plate with the annular groove formed on the surface, the average roughness Rc of the roughness curve element is 50 μm to 500 μm, and the roughness curve Forming a rough member having a skewness Rsk of −3 to 0.5 to produce a plate member;
A molding composition preparation step of preparing a fluorine-containing elastomer composition as a molding composition;
After the molding composition is disposed inside the annular groove of the plate-like member, the molding composition is heated and pressurized between the plate-like member and the mold, thereby forming the annular shape of the plate-like member. A method for manufacturing a gate seal structure for a semiconductor manufacturing apparatus, comprising: a molding step of forming a seal member inside the groove. In the manufacturing method of the gate-seal structure for semiconductor manufacturing apparatuses described in Claim 3,
A method for manufacturing a gate seal structure for a semiconductor manufacturing apparatus, comprising a reheating step of reheating the sealing member after the molding step.

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