JP3502616B2 - Rubber composition and rubber molded product obtained by molding the same - Google Patents

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a rubber composition containing a fluororubber elastomer as a main component, and a rubber molded product obtained by molding the rubber composition.

[0002]

2. Description of the Related Art Semiconductor manufacturing processes include various processes such as vacuum treatment, high heat treatment, treatment using acid, alkali and organic solvent. Therefore, not only the rubber part such as the seal of the semiconductor manufacturing apparatus itself, but also the rubber part for various equipment used in the periphery thereof, for example, the wafer suction membrane used for fixing the semiconductor wafer during transportation or polishing, Air bag for wafer fixing,
Seals for clamp joints, vacuum equipment seals, and clean box seals are required to have at least heat resistance and plasma resistance. As a rubber material having both the heat resistance and the plasma resistance at the same time, for example, a fluororubber elastomer is known, and has been widely used conventionally for the rubber portion in the above-mentioned semiconductor manufacturing apparatus and its peripheral equipment.

On the other hand, extremely high cleanliness is required for semiconductor manufacturing. The requirement for cleanliness extends not only to the control of semiconductor manufacturing processes, but also to the semiconductor manufacturing apparatus itself as well as the above-mentioned various devices used in the periphery thereof. Parts for semiconductor manufacturing are limited in the degree to which they can be cleaned by washing after being incorporated into a manufacturing apparatus or the like, and it is required that they be highly cleaned before being incorporated into the apparatus or the like. Contamination that is a particular problem in semiconductor manufacturing is dust such as fine particles called particles and metal compounds. Contamination by these dusts adversely affects fine etching processing and leads to product defects as wafer surface contaminants. Therefore, the removal of these contaminants is a major issue from the viewpoint of improving the product yield.

Therefore, it is required that the rubber portion of the above-mentioned semiconductor manufacturing apparatus and its peripheral equipment does not generate wafer surface contaminants that would lead to product defects. However, the fluororubber elastomer is usually blended with a polyol crosslinking agent or an amine crosslinking agent, and in addition to these crosslinking agents, magnesium oxide, calcium hydroxide, lead oxide, barium sulfate for promoting crosslinking,
An acid acceptor such as titanium oxide or zinc oxide is mixed. In addition, carbon black is usually added to the fluororubber elastomer as a reinforcing agent to improve mechanical properties such as compression set. Therefore, when the fluororubber elastomer is worn, the rubber pieces, the acid acceptor, the carbon black, etc. produced by the abrasion are scattered to generate dust, and the semiconductor product or the semiconductor manufacturing apparatus,
Furthermore, the peripheral equipment may be contaminated.

[0005]

SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and its purpose is to:
A rubber molded product containing a fluororubber elastomer as a main component, which has heat resistance and plasma resistance, has improved wear resistance, and generates little dust even when worn, especially a metal compound, and To provide a rubber composition.

[0006]

The present inventors have completed the present invention as a result of intensive research to solve the above problems. The present invention is as follows. (1) 1 part by weight to 10 parts by weight of an organic peroxide, 1 part by weight to 10 parts by weight of a crosslinking aid, and a content of silicon dioxide of 99% or more based on 100 parts by weight of a fluororubber elastomer. Semiconductor containing 1 to 50 parts by weight of silica
A rubber composition for a body manufacturing apparatus or peripheral equipment thereof. (2) The fluororubber-based elastomer is a hexafluoropropylene-vinylidene fluoride copolymer and hexafluoropropylene-vinylidene fluoride-
The rubber composition as described in (1) above, which is at least one selected from tetrafluoroethylene copolymers. (3) The above (1), wherein the silica is dry silica, or
(2) The rubber composition as described above. (4) The content of the metal element is less than 100 ppm
The rubber composition (5) according to any one of (1) to (3) above, which does not contain carbon black (1) to
The rubber composition according to any one of (4). ( 6 ) A semiconductor manufacturing apparatus or a peripheral machine thereof, which is obtained by molding the rubber composition according to any one of (1) to (5 ) above.
A rubber molded product that is a rubber member for dexterity .

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below.
The rubber composition of the present invention contains a fluororubber elastomer as a main component, and contains silica, an organic peroxide and a crosslinking aid in respective amounts within a specific range. The fluororubber elastomer used in the present invention is not particularly limited, and hexafluoropropylene-vinylidene fluoride copolymer, hexafluoropropylene-
Vinylidene fluoride-tetrafluoroethylene copolymer, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, tetrafluoroethylene-propylene copolymer and the like, various conventionally known fluororubber elastomers can be used, but will be described later. As the generation of dust during plasma irradiation is low,
Among the above, particularly, hexafluoropropylene-vinylidene fluoride copolymer, hexafluoropropylene-
Vinylidene fluoride-tetrafluoroethylene copolymer is preferred. Among them, in particular, the hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer, which contains the "tetrafluoroethylene" component, is particularly excellent in abrasion resistance and cannot generate dust of a metal compound. Is preferred. In the present invention, the fluororubber elastomer may be used alone, or two or more kinds (for example, hexafluoropropylene-vinylidene fluoride copolymer and hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer). It may be a blend with a polymer).

The rubber composition of the present invention comprises silicon dioxide (Si
O ₂ ) contains 99% or more, preferably 99.5% or more of silica. The silica refers to an inorganic substance containing silicon dioxide as a main component, which has been widely used as an inorganic filler for rubber and an inorganic reinforcing agent, which is also called white carbon. As the silica in the present invention, either wet silica or dry silica can be used, and a combination system of both may be used, but with wet silica containing water,
It is preferable to use dry silica because it may foam during vulcanization molding or during use. When the content of silicon dioxide in the silica is less than 99%, the compounds such as Al, Fe, Ti and Na contained as impurities in the silica are
There is a problem that the rubber molding obtained by molding the rubber composition becomes dust due to abrasion. When the content of silicon dioxide in the silica is less than 99%, the vulcanization rate of the rubber becomes slow and the moldability is deteriorated.

The silicon dioxide in the present invention is 99
% Or more of silica is commercially available, for example, Aerosil 200 (manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content:
Aerosil TT600 (manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 99.8% or higher), Aerosil S (manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 9)
9.8% or more), Aerosil "O" (manufactured by Nippon Aerosil, silicon dioxide content: 99.8% or more), Aerosil AL 0111/200 (manufactured by Nippon Aerosil, silicon dioxide content: 99.3% or more) ), Aerosil 2491
(Manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 99.8%
Above), Aerosil 130 (manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 99.8% or more), Aerosil 300
(Manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 99.8%
Above), Aerosil 380 (manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 99.8% or more), Aerosil OX50
(Manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 99.8%
Above), Aerosil MOX80 (manufactured by Nippon Aerosil,
Silicon dioxide content: 99.3% or more), Aerosil MO
X170 (manufactured by Nippon Aerosil Co., Ltd., silicon dioxide content: 9
9.3% or more) such as dry silica, for example Syloid A
L-1 (Fuji Devison Chemical Co., Ltd., silicon dioxide content: 9
9.6%), Syloid 72 (Fuji Davison Chemical Co., Ltd., silicon dioxide content rate: 99.2%), Syloid 73 (Fuji Davison Chemical Co., Ltd., silicon dioxide content rate: 99.2%), Sy
Wet silica such as loid 75 (manufactured by Fuji Devison Chemical Co., Ltd., silicon dioxide content: 99.3%), Syloid 161 (manufactured by Fuji Devison Chemical Co., Ltd., silicon dioxide content: 99.3%) may be used.

In the rubber composition of the present invention, the silicon dioxide in silica is, for example, described in "Additives for Plastics and Rubber Practical Handbook" [published by Kagaku Kogyo Co., Ltd.], p.
It can be quantified by the following method described on page 585. First, about 3 g of anhydrous sodium carbonate is added to 0.5 g of the sample, and the sample is melted in a platinum crucible. After cooling, the contents are transferred to an evaporating dish, about 50 ml of water are added and 15 ml to 20 ml of concentrated hydrochloric acid are added and melted. Evaporate to dryness on a water bath,
Heat at 150 ° C. for about 1 hour. After the evaporating dish has cooled slightly, the contents are moistened with 10 ml of concentrated hydrochloric acid, and after 1-2 minutes, water is added to make 500 ml, and the mixture is thoroughly stirred with a glass rod to dissolve the solid matter. After heating for about 5 minutes on a water bath, the insoluble silicic acid is filtered off. First, wash with concentrated hydrochloric acid (1:99),
Then do it in boiling water. The filtrate and washing liquid are evaporated to dryness again, and silicic acid is recovered in the same manner as the previous time. In this case, use a new filter paper. Combine with the previous precipitation, put in a platinum crucible, dry with a flame as small as possible, weaken the flame a little and incinerate the filter paper. After the filter paper is completely incinerated, it is ignited at 1000 ° C. and weighed as silicon dioxide. Then add a small amount of water to wet the residue, add 2-3 drops of sulfuric acid (1: 1) and hydrofluoric acid 5
Add ml to 10 ml and evaporate to dryness. Gradually raise the temperature, and finally ignite at 1000 ° C. to volatilize the silicic acid and obtain the amount of impurities for correction.

In the present invention, the silica is blended in an amount of 1 to 50 parts by weight, preferably 2 to 30 parts by weight, based on 100 parts by weight of the fluororubber elastomer. If the amount of silica is less than 1 part by weight with respect to 100 parts by weight of the fluororubber elastomer, it is extremely difficult to mix the organic peroxide and the crosslinking aid, and the viscosity of the rubber is low. There is a problem that the moldability of rubber is poor. When the amount of silica is more than 50 parts by weight based on 100 parts by weight of the fluororubber elastomer,
Machines such as compression set, where the viscosity of the rubber becomes too high and mixing work is not possible, the moldability of the rubber is poor, and the molded rubber has a type A durometer hardness of more than 95 and loses rubber elasticity. There is a problem that the dynamic strength is reduced.

In the present invention, the particle size is preferably 5 μm to 50 μm, more preferably 10 μm to 3 μm.
0 μm silica is used. The particle size of the silica is measured, for example, by the following method. First, the silica particles to be measured are put into an organic liquid such as ethanol or water, ultrasonic waves of about 35 kHz to 40 kHz are applied, and dispersion treatment is performed for about 2 minutes. The amount of the particulate matter to be measured is such that the laser transmittance (ratio of the output light amount to the incident light amount) of the dispersion liquid after the dispersion treatment is 70% to 90%. Next, this dispersion is applied to a Microtrac particle size analyzer, and the particle size of each particle is measured by scattering laser light. In addition, the Microtrac particle size analyzer calculates the particle size distribution of the spherical particle group having the theoretical intensity closest to the observed scattering intensity distribution. That is, the particles are assumed to be spheres having a cross-sectional circle with the same area as the projected image obtained by irradiation with laser light, and the diameter of this cross-sectional circle (sphere equivalent diameter) is measured as the particle diameter.

In the rubber composition of the present invention, 1 part by weight to 10 parts by weight, preferably 1 part by weight to 8 parts by weight of organic peroxide is further compounded with 100 parts by weight of the fluororubber elastomer. When the compounding amount of the organic peroxide is less than 1 part by weight with respect to 100 parts by weight of the fluororubber elastomer, the compression set of the rubber molded product obtained by molding the rubber composition becomes too large. There is a defect. When the compounding amount of the organic peroxide exceeds 10 parts by weight with respect to 100 parts by weight of the fluororubber elastomer,
There is a problem that the processability of rubber becomes poor, and the rubber molded product obtained by molding is also inferior in mechanical properties.

The organic peroxide used in the present invention can be used without particular limitation as long as it is an organic peroxide which is generally blended with rubber as a crosslinking agent. The organic peroxide is not particularly limited, but for example, benzoyl peroxide, 1,1-bis (t-butylperoxy) -3,3,5-trimethylcyclohexane,
1,1-bis (t-butylperoxy) cyclododecane, n-butyl-4,4-bis (t-butylperoxy) valerate, dicumyl peroxide, t-butylperoxybenzoate, 1,3-bis (T-Butylperoxyisopropyl) benzene, 2,5-dimethyl-
2,5-di (t-butylperoxy) hexane, 2,5
One or more selected from -dimethyl-2,5-di (t-butylperoxy) hexyne-3 and the like.

Furthermore, the rubber composition of the present invention contains 1 part by weight to 1 part by weight per 100 parts by weight of the fluororubber elastomer.
0 parts by weight, preferably 2 parts by weight to 6 parts by weight of a crosslinking aid are blended. If the amount of the crosslinking aid compounded is less than 1 part by weight based on 100 parts by weight of the fluororubber elastomer, the rubber will not be vulcanized. If the compounding amount of the cross-linking aid exceeds 10 parts by weight with respect to 100 parts by weight of the fluororubber elastomer, the processability of the rubber deteriorates, and further the obtained rubber molded product has poor mechanical properties.

The cross-linking aid used in the present invention can be used without particular limitation as long as it is generally added to rubber as a cross-linking aid. For example, N, N-m-phenylene dimaleimide, triallyl cyan Nurate, diallyl fumarate, diallyl phthalate, tetraallyloxyethane, ethylene glycol acrylate, triethylene glycol acrylate, triethylene glycol methacrylate, tetraethylene glycol dimethacrylate, polyethylene glycol dimethacrylate, trimethylolpropene trimethacrylate 1 type or 2 or more types.

The rubber composition of the present invention as described above is kneaded using a conventionally known kneader such as intermix, kneader, Banbury mixer, or an open roll, and then injection molding machine, compression molding machine, extrusion molding. It can be molded into a desired shape using a machine or the like.

The rubber molded product of the present invention thus obtained contains a fluororubber elastomer as a main component, and contains silica, an organic peroxide and a cross-linking aid in respective amounts within the respective specified ranges as described above. . First, in the rubber molded product of the present invention, silica containing 99% or more of silicon dioxide is used in an amount of 1 per 100 parts by weight of the fluororubber elastomer.
By containing 50 parts by weight to 50 parts by weight, the abrasion resistance and tensile strength of the obtained rubber molded article are improved, and the abrasion resistance is reduced. As a result, the rubber molded product of the present invention is less likely to be worn as compared with the conventional rubber molded product containing a fluororubber elastomer as a main component, and therefore dust such as rubber pieces due to the wear is less likely to be generated. Further, in the present invention, since high-purity silica containing 99% or more of silicon dioxide is used, a conventional rubber molded product using silica containing a compound such as Al, Fe, Ti and Na as impurities. In contrast, even if the rubber molded product is worn, it is possible to prevent these impurities from scattering as dust, and reduce the generation of dust that is disliked in the semiconductor manufacturing apparatus and its peripheral equipment.

In addition, the rubber molded product of the present invention contains, as essential components, high-purity silica, an organic peroxide and a cross-linking aid in specific blending amounts with respect to the fluororubber elastomer. Thus, in the present invention, the compatibility of the fluororubber elastomer and silicon dioxide,
Also, due to the interaction between the organic peroxide and the cross-linking aid, a more precise vulcanization is achieved as compared with a rubber molded product which does not have the above-mentioned constituents as essential components, and silica exhibits a reinforcing property close to that of carbon black. Therefore, it is possible to provide a rubber molded product having excellent mechanical properties such as compression set without adding carbon black as a reinforcing agent. Therefore, the rubber molded article of the present invention does not need to contain carbon black for the purpose of improving mechanical strength as in the conventional case,
Even if the rubber molded product is worn, it is possible to prevent the carbon black from scattering as dust, which also reduces the generation of dust that is disliked in the semiconductor manufacturing apparatus and its peripheral equipment.

Further, in the present invention, since an organic peroxide is used as a cross-linking agent without using a polyol cross-linking agent or an amine cross-linking agent, magnesium oxide, calcium hydroxide, lead oxide, barium sulfate for promoting cross-linking is used. It is not necessary to add an acid acceptor such as titanium oxide or zinc oxide.
Therefore, also from this point, the rubber molded article of the present invention,
Even if it is worn, it is possible to prevent these acid acceptors from scattering as dust.

As described above, the rubber molded product of the present invention is less likely to be worn as compared with the conventional rubber molded product, and as a result, dust is less likely to be generated including the rubber pieces, and at the same time, the carbon black and the acid acceptor can be obtained. Since it is realized with a composition that does not contain impurities such as silica as much as possible, dust is not easily generated even if it is worn. Such a rubber molded article of the present invention can be particularly suitably used as a rubber portion in a semiconductor manufacturing apparatus or its peripheral equipment that requires extremely high cleanliness.

In the present invention, the above-mentioned composition makes it possible to realize a rubber molded product containing no metal element of 100 ppm or more. When the metal element is in the state of a metal oxide, an organic metal compound or the like in the rubber molded product, it is less than 100 ppm when converted to only the metal element in these compounds. As a result, worn rubber pieces and metal compound dust (particles)
Among them, it is possible to realize a rubber molded product that can particularly reduce the generation of dust of a metal compound that adversely affects the semiconductor electrically.

The metal element in such a rubber molded product is a conventionally known ICP-AES (IC).
P-AES ； Inductively Coupled Plasma Automatic Emissi
on Spectrometry) and inductively coupled plasma mass spectrometer (I
CP-MS; Inductively CoupledPlasma Mass Spectrometr
y), graphite furnace atomic absorption spectrometer (GFAAS; Graphite
Furnace Atomic Absorption Spectrometry) or the like can be used to perform the quantification by a procedure usually performed in the art.

The rubber molded article of the present invention has the effect of producing less dust even when it is worn as described above, but has the various properties conventionally possessed by fluororubber elastomers such as heat resistance and plasma resistance. Needless to say, it has both.

Further, in the rubber molded product of the present invention, silica containing 99% or more of silicon dioxide is contained in an amount of 1 part by weight to 100 parts by weight of the fluororubber elastomer.
By containing 50 parts by weight, there is an effect that it is unlikely to adhere to metals and resins. That is, even if the rubber molded product of the present invention is used as a seal for a metal or resin mating member, it will not stick to the mating member due to long-term use. The seal is not something that is installed once and continues to exert its sealing function as it is, but it has a life due to deterioration of rubber, etc. Therefore, it is assumed that it will be replaced with a new one after a certain period of time. Then used. In the rubber molded product of the present invention, since the adhesion to the mating member is low, a part of the seal remains on the mating member at the time of this removal, which may cause contamination of surrounding equipment. It can be prevented. Since the rubber molded product of the present invention also has such an effect, it is particularly useful in the application as a rubber portion in a semiconductor manufacturing apparatus or its peripheral equipment in which the above-mentioned contamination may have a serious adverse effect.

The rubber molded product of the present invention is preferably obtained from the above rubber composition through primary vulcanization and secondary vulcanization. The primary vulcanization and secondary vulcanization are preferably performed at 140 ° C. to 200 ° C. for 2 minutes to 60 minutes for primary vulcanization, and 150 ° C. to 250 ° C. for secondary vulcanization.
It is preferable that the treatment is performed for 30 minutes to 24 hours.

By carrying out the primary vulcanization and the secondary vulcanization under the above-mentioned conditions, a rubber molded product having a further reduced gas generating property can be obtained. This is because the substance having a low boiling point in the rubber is volatilized by performing the secondary vulcanization under the above temperature and time conditions. Further, the rubber molded product obtained through the primary vulcanization and the secondary vulcanization under the above conditions is more improved in compression set than the rubber molded product obtained under the conditions other than the above conditions.

The shape and size of the rubber molded product of the present invention are appropriately selected depending on the purpose depending on the application and are not particularly limited. The rubber molded product of the present invention has both heat resistance and plasma resistance, has improved wear resistance, and has less dust generated even when worn, and therefore has a rubber property such as a seal for a semiconductor manufacturing apparatus itself. Not only the parts,
For example, semiconductors such as membranes for adsorbing wafers used for fixing semiconductor wafers during transportation and polishing, air bags for fixing wafers, seals for clamp joints, seals for vacuum equipment and seals for clean boxes. It can be suitably used for a conventionally known rubber portion in various equipments for manufacturing.

When the above-mentioned membrane or air bag is formed from the rubber composition of the present invention (the rubber molded product is the above-mentioned membrane or air bag), it is required to further have sufficient tear resistance and resilience. It In the present invention, the tear resistance measured according to the measuring method defined in JIS K 6252 (crescent dumbbell) is, for example, 40 kN / by being formed through primary vulcanization and secondary vulcanization under the above-mentioned conditions. It is about m. In addition, the resilience measured according to the measurement method specified in JIS K 6262 (50 at a measurement temperature of 25 ° C.
% Stretch and hold for 10 minutes, then release and 10 minutes later the restorability (permanent elongation) is about 2% to 5%, for example. As described above, in the present invention, it is possible to realize a rubber molded product having both tear resistance and resilience sufficient for use in the above-mentioned membrane and air bag.

Further, the rubber composition of the present invention is used to form a seal for semiconductor manufacturing equipment itself, a seal for a clamp joint, a vacuum facility, a clean box, and other peripheral devices (the above-mentioned seals are rubber molded products). In this case, it is required to have mechanical properties such as hardness, tensile strength, elongation, and compression set for exhibiting good sealing properties. In the present invention, the type A durometer hardness measured according to the measuring method specified in JIS K 6253 is, for example, about 65 to 90, by forming through primary vulcanization and secondary vulcanization under the above-mentioned conditions. JIS K
The tensile strength measured according to the measuring method prescribed in 6251 is, for example, about 10 MPa to 30 MPa, JI
The elongation measured according to the measuring method specified in SK 6251 is, for example, about 300% to 600%, JI
The compression set (70 hours at 200 ° C.) measured according to the measuring method specified in SK 6262 is realized at, for example, about 15% to 30%.

[0031]

EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to the following examples. Example 1 As a fluororubber elastomer, a hexafluoropropylene-vinylidene fluoride copolymer (Dayer G8
01, manufactured by Daikin Co., Ltd., organic peroxide (Perhexa 25)
B, manufactured by NOF CORPORATION, a crosslinking aid (TAIC, manufactured by Nippon Kasei), and silica (Aerosil 200, manufactured by Nippon Aerosil, silicon dioxide content rate: 99.8%, particle size: 12μ).
m) was used to prepare a rubber composition with the following compounding ratio. (Ratio of rubber composition) 100 parts by weight of fluororubber elastomer 1.8 parts by weight of organic peroxide 4.5 parts by weight of cross-linking agent 4.5 parts by weight of silica 10 parts by weight of the rubber composition blended as described above with an open roll After kneading and preparing, primary vulcanization at 150 ° C for 30 minutes,
Then, after secondary vulcanization at 180 ° C. for 4 hours, a rubber molded product sample was obtained.

Example 2 A rubber molded product was obtained in the same manner as in Example 1 except that a hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer (Dayer G902, manufactured by Daikin) was used as the fluororubber elastomer. I got a sample of.

Example 3 A rubber molded product sample was obtained in the same manner as in Example 1 except that 30 parts by weight of silica was added to 100 parts by weight of the fluororubber elastomer.

Comparative Example 1 Instead of the above silica (Aerosil 200, manufactured by Nippon Aerosil), silica (Carplex # 1120, manufactured by Shionogi Pharmaceutical Co., Ltd., silicon dioxide content: 91.5%, particle diameter: 8 μ)
A rubber molded product sample was obtained in the same manner as in Example 1 except that m) was used.

Comparative Example 2 Hexafluoropropylene-vinylidene fluoride copolymer (Viton E6) was used as a fluororubber elastomer.
0C, manufactured by DuPont, containing a polyol crosslinking agent), crosslinking aid (Calbit, manufactured by Omi Chemical Co., Ltd.), carbon black (MT carbon black, manufactured by Canon Curve Limited), and acid acceptor (Magnesia # 30, Kyowa). (Manufactured by Kagaku) was used to prepare a rubber composition at the following compounding ratio. (Ratio of rubber composition) 100 parts by weight of fluororubber elastomer 6 parts by weight of crosslinking aid 6 parts by weight of carbon black 20 parts by weight of acid acceptor 3 parts by weight The rubber composition prepared as described above is kneaded by an open roll. After that, primary vulcanization at 170 ° C. for 15 minutes,
Then, after secondary vulcanization at 230 ° C. for 24 hours, a rubber molded product sample was obtained.

Comparative Example 3 Instead of carbon black, silica (Aerosil 20
0, made by Nippon Aerosil, silicon dioxide content rate: 99.8
%, Particle size: 12 μm), a sample of a rubber molded product was obtained in the same manner as in Comparative Example 2 except that primary vulcanization was performed at 170 ° C. for 30 minutes and then secondary vulcanization at 230 ° C. for 24 hours. Got

Comparative Example 4 Instead of the above silica (Carplex # 1120, manufactured by Shionogi Pharmaceutical Co., Ltd.), silica (Hisil 233, manufactured by Harbic Co., Ltd., silicon dioxide content rate: 87.0%, particle size: 20 μ)
A rubber molded product sample was obtained in the same manner as in Comparative Example 1 except that m) was used.

[Evaluation of Dust Generation (Content of Metal Element)] An inductively coupled plasma emission spectroscopic analyzer (SPS-4000) was used for each sample of the rubber moldings obtained in Examples 1 to 3 and Comparative Examples 1 to 4. Type, manufactured by Seiko Denshi Kogyo Co., Ltd.), an inductively coupled plasma mass spectrometer (HP4500 model, Yokogawa Analytical Systems Co., Ltd.), and a graphite furnace atomic absorption spectrometer (Z-5700 model, Hitachi, Ltd.). The metal element contained in the sample at 100 ppm or more was confirmed. As a result, with respect to the samples of Examples 1 and 2, 100 ppm was obtained using any analyzer.
The metal elements contained above were not detected. Comparative Example 1
Fe was detected in the sample. For the sample of Comparative Example 2, Ba, Mg, Ca, Co, K,
V and Sr were detected. For the sample of Comparative Example 3, Ba, Mg, and Ca were detected. Fe and Na were detected in the sample of Comparative Example 4.

[Performance Test 1 (General Properties)] Examples 1 to 3
For each sample of the rubber molded product obtained in Comparative Examples 1 to 4, the type A durometer hardness (JIS K 6
253), tensile strength (MPa) (JIS K 6
251), elongation (%) (according to JIS K 6251) and compression set (%) at 200 ° C. for 70 hours (according to JIS K 6262) were measured.

[Performance Test 2 (Abrasion Resistance)] Examples 1 to 3
And, for each sample of the rubber moldings obtained in Comparative Examples 1 to 4, the wear amount was measured under the following conditions using a constant tension type wear tester. First, the mating metal plate was reciprocated by driving the crankshaft, and the sample was slid on the mating metal plate while applying a load in a direction perpendicular to the reciprocating direction of the mating metal plate. The thrust of the air cylinder was used for the action of the contact load between the sample and the mating metal plate. The conditions were as follows. -Sample: cylindrical (diameter = 6.3 mm, height = 8 mm) -Mating metal plate material: SS41 -Mating metal plate surface roughness: 3.2S -Reciprocating direction: Reciprocating at right angles to the finishing direction of the mating metal plate Motion-Drive speed: 60 cpm-Stroke: 10 mm-Load: 0.8 MPa-Number of operations: 100,000 cycles-With or without lubrication: None-Temperature: Normal temperature wear = [(W1-W2) / S] / A [W1: Sample weight before test (g), W2: sample weight after test (g), S: specific gravity of sample, A: bottom area of sample (mm
² )] was used to calculate each wear amount (mm).

[Performance Test 3 (Plasma Resistance)] Example 1
3 to 3 and Comparative Examples 1 to 4 respectively, O-ring samples (AS 568-214 standard) were prepared, and the samples were irradiated with plasma under the following conditions, and the weight change amount (%) of the samples before and after plasma irradiation was measured. ) Was investigated. Plasma irradiation atmosphere: oxygen plasma or CF ₄ plasma discharge power: 150 W · Frequency: 13.56 MHz · Pressure: 40 Pa · irradiation time: Table 1 shows the results of three hours performance test 1-3.

[0042]

[Table 1]

[0043]

As is apparent from the above description, according to the present invention, heat resistance and plasma resistance are maintained, abrasion resistance is improved, and dust is generated even when abrasion is generated, particularly metal. It is possible to provide a rubber molded product containing a fluororubber-based elastomer as a main component, which hardly generates a compound, and a rubber composition therefor.

─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Junichi Tsujimoto 1-8-30, Tenmabashi, Kita-ku, Osaka City, Osaka Prefecture OAP Tower Mitsubishi Cable Industries, Ltd. Kansai Branch Office (72) Inventor Iwata Tsukio Minoshima, Arita, Wakayama Prefecture No. 663 Mitsubishi Cable Industries Co., Ltd., within the Minoshima Works (56) Reference JP-A-6-49310 (JP, A) JP-A-5-339456 (JP, A) JP-A-4-275342 (JP, A) (58) ) Fields surveyed (Int.Cl. ⁷ , DB name) C08L 15/02 C08L 27/12-27/20

Claims (6)

(57) [Claims] 1. An organic peroxide of 1 part by weight to 10 parts by weight, a crosslinking aid of 1 part by weight to 10 parts by weight, and a silicon dioxide content of 9 parts by weight based on 100 parts by weight of a fluororubber elastomer.
A rubber composition for semiconductor manufacturing equipment or its peripheral equipment, containing 1 to 50 parts by weight of 9% or more silica. 2. The fluororubber elastomer is at least one selected from a hexafluoropropylene-vinylidene fluoride copolymer and a hexafluoropropylene-vinylidene fluoride-tetrafluoroethylene copolymer. Rubber composition. 3. The silica as claimed in claim 1, which is dry silica.
Alternatively, the rubber composition according to item 2. 4. When the content of the metal element is less than 100 ppm,
The rubber composition according to any one of claims 1 to 3. 5. The method according to claim 1, which does not contain carbon black.
The rubber composition according to any one of to 4. 6. obtained by molding the rubber composition according to any one of claims 1-5, or around for semiconductor manufacturing equipment
A rubber molded product that is a rubber member for equipment .