Fluoroether elastomer composition as well as preparation method and application thereof
By combining the crosslinking agent with a specific structure in the fluoroether elastomer composition with fluoroether rubber containing vulcanized point monomer, the problem of preforming vulcanization at low temperature and low pressure is solved, and low energy consumption and high Rate vulcanization molding is suitable for sealing ring applications of electrostatic suction cups.
Patent Information
- Application Number
- CN202411431488.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-14
- Publication Date
- 2025-02-14
AI Technical Summary
The prior art is difficult to perform preformed vulcanization of fluoroelastomer compositions at low temperatures and low pressures, resulting in the vulcanization conditions not suitable for the processing of electrostatic suction cups.
The crosslinking agent with a specific structure is used to cooperate with fluoroether rubber containing vulcanized point monomers to reduce the vulcanization temperature and vulcanization pressure during preforming the fluoroether elastomer composition, and achieve the conditions at 120-140°C and 1-3MPa. Perform heating vulcanization once.
It realizes rapid vulcanization and molding at low temperature and low pressure, has the characteristics of low energy consumption and fast vulcanization rate, and is suitable for protecting the sealing ring of the electrostatic suction cup, and is used in the field of semiconductor technology.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fluoroether elastomer compositions, and in particular to a fluoroether elastomer composition and a preparation method and application thereof. Background Art
[0002] The demand for localization of semiconductor industry product technology is constantly increasing, and the process improvement of the semiconductor industry is also constantly being improved, and the demand for sealing of equipment used in the semiconductor industry is also constantly changing. Electrostatic chucks are used in semiconductor processes as silicon wafer clamping tools in semiconductor processes. Silicon wafers are used as upper electrodes. Compared with mechanical chucks, vacuum chucks have good temperature regulation, more uniform force, and can reduce the edge effect of silicon wafers. They are widely used in advanced semiconductor processes. However, there is a gap in the middle of the electrostatic chuck, which is easily etched by plasma during use. At present, corrosion-resistant rubber sealing rings are used to cover the electrostatic chuck, but the rubber sealing ring and the electrostatic chuck need to be vulcanized together during the processing process, which requires the rubber sealing ring to have a low vulcanization temperature and a small vulcanization pressure during the initial vulcanization (preforming). At present, FFKM rubber uses double two five as a vulcanizing agent, and it needs to be vulcanized and molded at a high temperature and high pressure of 150°C and greater than 5MPa to have a certain practicality; but the vulcanization conditions of 150°C and high temperature and high pressure above 5MPa are not suitable for electrostatic chucks.
[0003] A Chinese patent with patent application number CN202011275931.4 discloses a low-temperature resistant perfluoroether rubber composition, a preparation method and application thereof, which uses perfluoroether rubber, liquid fluoroelastomer, a cross-linking agent and an accelerator. However, the patent discloses a one-stage vulcanization temperature of 180°C and a vulcanization time of 10 minutes. The disclosed perfluoroether rubber composition has low-temperature resistance, but no technical solution for one-stage vulcanization at low temperature is provided.
[0004] Therefore, providing a fluoroether elastomer composition that can be preformed at low temperature and low pressure is a major technical problem that needs to be solved at present. Summary of the invention
[0005] The first aspect of the present invention provides a fluoroether elastomer composition, the raw materials for its preparation include: fluoroether rubber, a crosslinking aid, and a crosslinking agent; the vulcanization temperature of the fluoroether elastomer composition for one-time heating vulcanization is lower than 150°C, and the vulcanization pressure is less than 5MPa.
[0006] The structural formula of the cross-linking agent includes at least one of Formula I and Formula II.
[0007]
[0008] In the cross-linking agent structural formula I and II, the substituent R is selected from one or more combinations of alkanes, aliphatic cycloalkyls, olefins, and aromatic hydrocarbons.
[0009] In the cross-linking agent structural formula I and II, the substituent R' is selected from one or more combinations of olefins, aliphatic cycloalkyls, alkanes, and aromatic hydrocarbons.
[0010] In one embodiment, the raw materials for its preparation include, by weight: 90-110 parts of fluoroether rubber, 1-2 parts of auxiliary cross-linking agent, and 0.5-1.5 parts of cross-linking agent.
[0011] In one embodiment, the fluoroether elastomer composition is subjected to a single heating vulcanization at a vulcanization temperature of 120-140° C., a vulcanization pressure of 1-3 MPa, and a vulcanization time of 8-15 min.
[0012] In one embodiment, the vulcanization temperature of the fluoroether elastomer composition for one-time heating vulcanization includes but is not limited to 120°C, 125°C, 130°C, 135°C, 140°C, the vulcanization pressure includes but is not limited to 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa, and the vulcanization time includes but is not limited to 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min.
[0013] In one embodiment, the fluoroether elastomer composition is subjected to a single heating vulcanization at a vulcanization temperature of 130° C., a vulcanization pressure of 2 MPa, and a vulcanization time of 10 min.
[0014] In one embodiment, the raw materials for its preparation include, by weight: 100 parts of fluoroether rubber, 1.5 parts of auxiliary cross-linking agent, and 1.0 part of cross-linking agent.
[0015] In one embodiment, the fluoroether rubber is a polymer consisting of a curing site monomer (CSM), a perfluoroalkyl vinyl ether (PAVE), and tetrafluoroethylene (TFE).
[0016] In one embodiment, the sulfurization site monomer can be connected to a halogen atom or an olefin. The halogen atom includes Cl, Br, and I.
[0017] In a preferred embodiment, the cross-linking agent is selected from at least one of benzoyl peroxide, tert-butyl perbenzoate, tert-butyl peroxyisopropyl carbonate, and tert-butyl peroxy(2-ethylhexanoate).
[0018] In a preferred embodiment, the cross-linking agent is benzoyl peroxide.
[0019] In a preferred embodiment, the cross-linking agent is tert-butyl perbenzoate.
[0020] In a preferred embodiment, the cross-linking agent is tert-butyl peroxyisopropyl carbonate.
[0021] In a preferred embodiment, the crosslinking agent is tert-butyl peroxy(2-ethylhexanoate).
[0022] In order to reduce the vulcanization temperature and vulcanization pressure during the preforming of the fluoroether elastomer composition, the inventors found in the experimental process that the crosslinking agent has a structural formula including at least one of Formula I and Formula II. In the crosslinking agent structural formula, the substituent R is selected from a combination of one or more of alkanes, aliphatic cycloalkyls, alkenes, and aromatic hydrocarbons; the substituent R' is selected from a combination of one or more of alkenes, aliphatic cycloalkyls, alkanes, and aromatic hydrocarbons, and the fluoroether rubber containing a vulcanization point monomer is used to obtain a fluoroether elastomer composition that can be preformed at low temperature and low pressure.
[0023] In one embodiment, the auxiliary cross-linking agent includes at least one of triallyl cyanurate and triallyl isocyanurate.
[0024] In one embodiment, the auxiliary cross-linking agent is triallyl cyanurate.
[0025] In one embodiment, the auxiliary cross-linking agent is triallyl isocyanurate.
[0026] A second aspect of the present invention provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0027] A cross-linking aid and a cross-linking agent are added to the fluoroether rubber to obtain a fluoroether elastomer composition.
[0028] In one embodiment, the method for preparing the fluoroether elastomer composition comprises the following steps:
[0029] Adjust the roller distance of the mixing mill to 0.6-1.0mm, put the fluoroether rubber into the mixing mill to soften it and wrap it around the roller, add the cross-linking agent, cut the rubber left and right and mix it, add the cross-linking agent after mixing evenly, adjust the roller distance to 0.2mm, pass it through 5-10 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which is parked for more than 12 hours for use.
[0030] In one embodiment, the method for preparing the fluoroether elastomer composition comprises the following steps:
[0031] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for more than 12 hours for use.
[0032] A third aspect of the present invention provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0033] In one embodiment, the sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0034] In one embodiment, the heating vulcanization includes primary heating vulcanization and secondary heating vulcanization, and the vulcanization temperature of the primary heating vulcanization is lower than 150° C. and the vulcanization pressure is lower than 5 MPa.
[0035] In one embodiment, the vulcanization temperature of the one-time heating vulcanization is 120-140° C., the vulcanization pressure is 1-3 MPa, and the vulcanization time is 8-15 min.
[0036] The one-time heating and vulcanization is a preforming process.
[0037] In one embodiment, the vulcanization temperature of the one-time heating vulcanization includes but is not limited to 120°C, 125°C, 130°C, 135°C, 140°C, the vulcanization pressure includes but is not limited to 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa, and the vulcanization time includes but is not limited to 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min.
[0038] In one embodiment, the vulcanization temperature of the one-time heating vulcanization is 130° C., the vulcanization pressure is 2 MPa, and the vulcanization time is 10 min.
[0039] In one embodiment, the primary heating vulcanization is to place the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product; the secondary heating vulcanization is to place the primary vulcanized product in an oven for secondary vulcanization after it is parked for 8 hours, and the oven temperature is raised from 25°C to 230°C for 4 hours, and maintained at 230°C for 4 hours, and then cooled to 25°C to prepare a sealing ring.
[0040] Beneficial Effects
[0041] 1. The fluoroether elastomer composition provided by the present invention can be preformed at low temperature and low pressure, and has the characteristics of low energy consumption and fast vulcanization rate.
[0042] 2. The sealing ring obtained by using the fluoroether elastomer composition provided by the present invention is suitable for protecting electrostatic chucks and is applied to the field of semiconductor technology.
[0043] 3. The fluoroether elastomer composition provided by the present invention has good physical and mechanical properties, and the compression permanent deformation at high temperature is less than 30%, and is suitable for the field of semiconductor technology.
[0044] 4. In the present application, a cross-linking agent with a specific structure is used in combination with a fluoroether rubber containing a vulcanization point monomer, so as to reduce the vulcanization temperature and the vulcanization pressure during the preforming of the fluoroether elastomer composition. DETAILED DESCRIPTION
[0045] The purchase sources or models of the raw materials used in the following examples are shown in Table 1:
[0046] Table 1
[0047]
[0048] Example 1
[0049] A first aspect of the present embodiment provides a fluoroether elastomer composition, wherein the raw materials for its preparation include, by weight: 100 parts of fluoroether rubber, 1.5 parts of a co-crosslinking agent, and 1.0 part of a crosslinking agent.
[0050] The auxiliary cross-linking agent is triallyl isocyanurate.
[0051] The cross-linking agent is tert-butyl peroxyisopropyl carbonate.
[0052] A second aspect of the present embodiment provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0053] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0054] A third aspect of the present embodiment provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0055] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0056] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 130° C., the vulcanization pressure is 2 MPa, and the vulcanization time is 10 min; the secondary heating vulcanization is to park the primary vulcanized product for 8 hours, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25° C. to 230° C., the heating time is 4 hours, and it is kept at 230° C. for 4 hours, and then the temperature is lowered to 25° C. to prepare a sealing ring.
[0057] Example 2
[0058] A first aspect of the present embodiment provides a fluoroether elastomer composition, wherein the raw materials for its preparation include, by weight: 100 parts of fluoroether rubber, 1.5 parts of a co-crosslinking agent, and 1.0 part of a crosslinking agent.
[0059] The auxiliary cross-linking agent is triallyl isocyanurate.
[0060] The cross-linking agent is tert-butyl perbenzoate.
[0061] A second aspect of the present embodiment provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0062] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0063] A third aspect of the present embodiment provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0064] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0065] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 130° C., the vulcanization pressure is 2 MPa, and the vulcanization time is 10 min; the secondary heating vulcanization is to park the primary vulcanized product for 8 hours, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25° C. to 230° C., the heating time is 4 hours, and it is kept at 230° C. for 4 hours, and then the temperature is lowered to 25° C. to prepare a sealing ring.
[0066] Example 3
[0067] A first aspect of the present embodiment provides a fluoroether elastomer composition, wherein the raw materials for its preparation include, by weight: 100 parts of fluoroether rubber, 1.5 parts of a co-crosslinking agent, and 1.0 part of a crosslinking agent.
[0068] The auxiliary cross-linking agent is triallyl isocyanurate.
[0069] The crosslinking agent is tert-butyl peroxy(2-ethylhexanoate).
[0070] A second aspect of the present embodiment provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0071] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0072] A third aspect of the present embodiment provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0073] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0074] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 130° C., the vulcanization pressure is 2 MPa, and the vulcanization time is 10 min; the secondary heating vulcanization is to park the primary vulcanized product for 8 hours, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25° C. to 230° C., the heating time is 4 hours, and it is kept at 230° C. for 4 hours, and then the temperature is lowered to 25° C. to prepare a sealing ring.
[0075] Example 4
[0076] A first aspect of the present embodiment provides a fluoroether elastomer composition, wherein the raw materials for its preparation include, by weight: 100 parts of fluoroether rubber, 1.5 parts of a co-crosslinking agent, and 1.0 part of a crosslinking agent.
[0077] The auxiliary cross-linking agent is triallyl isocyanurate.
[0078] The cross-linking agent is benzoyl peroxide.
[0079] A second aspect of the present embodiment provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0080] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0081] A third aspect of the present embodiment provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0082] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0083] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 130° C., the vulcanization pressure is 2 MPa, and the vulcanization time is 10 min; the secondary heating vulcanization is to park the primary vulcanized product for 8 hours, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25° C. to 230° C., the heating time is 4 hours, and it is kept at 230° C. for 4 hours, and then the temperature is lowered to 25° C. to prepare a sealing ring.
[0084] Comparative Example 1
[0085] Comparative Example 1 The first aspect provides a fluoroether elastomer composition, and its preparation raw materials include, by weight: 100 parts of fluoroether rubber, 1.5 parts of auxiliary cross-linking agent, and 1.0 part of cross-linking agent.
[0086] The auxiliary cross-linking agent is triallyl isocyanurate.
[0087] The cross-linking agent is 2,5-bis(tert-butyl)-2,5-dimethylhexane.
[0088] Comparative Example 1 The second aspect provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0089] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0090] Comparative Example 1 The third aspect provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0091] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0092] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 130° C., the vulcanization pressure is 2 MPa, and the vulcanization time is 10 min; the secondary heating vulcanization is to park the primary vulcanized product for 8 hours, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25° C. to 230° C., the heating time is 4 hours, and it is kept at 230° C. for 4 hours, and then the temperature is lowered to 25° C. to prepare a sealing ring.
[0093] Comparative Example 2
[0094] Comparative Example 2 The first aspect provides a fluoroether elastomer composition, and its preparation raw materials include, by weight: 100 parts of fluoroether rubber, 1.5 parts of auxiliary cross-linking agent, and 1.0 part of cross-linking agent.
[0095] The auxiliary cross-linking agent is triallyl isocyanurate.
[0096] The cross-linking agent is 2,5-bis(tert-butyl)-2,5-dimethylhexane.
[0097] Comparative Example 2 The second aspect provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0098] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0099] Comparative Example 2 The third aspect provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0100] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0101] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 170°C, the vulcanization pressure is 8MPa, and the vulcanization time is 10min; the secondary heating vulcanization is to park the primary vulcanized product for 8h, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25°C to 230°C, the heating time is 4h, and it is kept at 230°C for 4h, and then the temperature is lowered to 25°C to prepare a sealing ring.
[0102] Comparative Example 3
[0103] Comparative Example 3 The first aspect provides a fluoroether elastomer composition, and its preparation raw materials include, by weight: 100 parts of fluoroether rubber, 1.5 parts of auxiliary cross-linking agent, and 1.0 part of cross-linking agent.
[0104] The auxiliary cross-linking agent is triallyl isocyanurate.
[0105] The cross-linking agent is 2,5-dimethyl-2,5-di(tert-butylperoxy)-3-hexyne.
[0106] Comparative Example 3 The second aspect provides a method for preparing a fluoroether elastomer composition, comprising the following steps:
[0107] Adjust the roller distance of the mixing mill to 0.6mm, put the fluoroether rubber into the mixing mill to soften it and make it wrap around the roller, add the cross-linking agent, cut the rubber left and right and mix it, after mixing evenly, add the cross-linking agent, adjust the roller distance to 0.2mm, pass it 8 times, continue to adjust the roller distance to 1.0mm, and produce a sheet to obtain the fluoroether elastomer composition, which should be parked for 12 hours for use.
[0108] Comparative Example 3 The third aspect provides an application of a fluoroether elastomer composition, wherein the fluoroether elastomer composition is applied in the field of semiconductor technology.
[0109] The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
[0110] The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization; the primary heating vulcanization is to put the fluoroether elastomer composition into a mold, and place the mold in a flat vulcanizer for primary heating vulcanization to obtain a primary vulcanized product, the vulcanization temperature of the primary heating vulcanization is 170°C, the vulcanization pressure is 8MPa, and the vulcanization time is 10min; the secondary heating vulcanization is to park the primary vulcanized product for 8h, then place it in an oven for secondary vulcanization, the oven temperature is raised from 25°C to 230°C, the heating time is 4h, and it is kept at 230°C for 4h, and then the temperature is lowered to 25°C to prepare a sealing ring.
[0111] Performance Test:
[0112] (1) Vulcanization characteristic parameter test:
[0113] The fluoroether elastomer compositions provided in Examples 1-4 and Comparative Examples 1-3 were respectively tested for their vulcanization characteristic parameters in accordance with "GBT16584-1996 Determination of Vulcanization Characteristics of Rubber Using a Rotorless Vulcanizer". The vulcanization temperature in the rotorless vulcanizer was set to 120°C and the vulcanization time was set to 30 min. The vulcanization characteristic parameters included TS2, TC50, TC90, ML, and MH. The test results are shown in Table 2.
[0114] (2) Hardness test:
[0115] After heating and vulcanization, the fluoroether elastomer compositions provided in Examples 1-4 and Comparative Examples 1-3 were respectively measured for their Shore A hardness in accordance with GBT 531.1-2008 Test method for indentation hardness of vulcanized rubber or thermoplastic rubber Part 1 - Shore hardness tester method (Shore hardness) standard. The test results are shown in Table 2.
[0116] (3) Tensile properties test:
[0117] After heating and vulcanizing, the fluoroether elastomer compositions provided in Examples 1-4 and Comparative Examples 1-3 were tested for tensile strength, 100% modulus, and elongation at break according to GBT 528-2009 Determination of tensile stress-strain properties of vulcanized rubber or thermoplastic rubber. The test results are shown in Table 2.
[0118] (4) Compression set test:
[0119] After the fluoroether elastomer compositions provided in Examples 1-4 and Comparative Examples 2-3 were heated and vulcanized, the compression set at high temperature was tested in accordance with GBT7759.1-2015 Determination of compression set of vulcanized rubber or thermoplastic rubber Part 1: At room temperature and high temperature conditions. The test results are shown in Table 2.
[0120] The sealing ring prepared by the fluoroether elastomer composition provided in Comparative Example 1 had a cracking problem, and the compression permanent deformation was not detected.
[0121] Table 2
[0122]
[0123]
[0124] It can be seen from the test data in Table 2 that when the fluoroether elastomer composition contains the cross-linking agent provided in the present application, the vulcanization temperature and the vulcanization pressure can be reduced, the vulcanization rate is moderate, and the MH value is moderate. Moreover, the composition can be vulcanized and formed when the vulcanization temperature is lower than 150°C and the vulcanization pressure is less than 5MPa during the first heating vulcanization. The composition has good physical properties and the compression permanent deformation at high temperature is less than 30%. The obtained sealing ring is suitable for protecting electrostatic chucks and is applied to the field of semiconductor technology. When 2,5-bis(tert-butyl)-2,5-dimethylhexane or 2,5-dimethyl-2,5-di(tert-butylperoxy)-3-hexyne is used, high temperature and high pressure vulcanization is required during the first heating vulcanization to obtain a practical sealing ring.
Claims
1. A fluoroether elastomer composition, characterized in that The raw materials for its preparation include: fluoroether rubber, auxiliary crosslinking agent, and crosslinking agent; the vulcanization temperature of the fluoroether elastomer composition for one-time heating vulcanization is lower than 150°C, and the vulcanization pressure is lower than 5MPa; The structural formula of the cross-linking agent includes at least one of Formula I and Formula II; The substituent R in Formula I and Formula II is selected from one or more combinations of alkanes, aliphatic cycloalkyls, olefins, and aromatic hydrocarbons; The substituent R' in the formula I and formula II is selected from one or more combinations of olefins, aliphatic cycloalkyls, alkanes, and aromatic hydrocarbons.
2. The fluoroether elastomer composition according to claim 1, characterized in that The raw materials for its preparation include, by weight: 90-110 parts of fluoroether rubber, 1-2 parts of auxiliary cross-linking agent, and 0.5-1.5 parts of cross-linking agent.
3. The fluoroether elastomer composition according to claim 1, characterized in that The vulcanization temperature of the fluoroether elastomer composition for primary heating vulcanization is 120-140°C.
4. The fluoroether elastomer composition according to claim 1, characterized in that The vulcanization pressure of the fluoroether elastomer composition during the primary heating vulcanization is 1-3 MPa.
5. The fluoroether elastomer composition according to any one of claims 1 to 4, characterized in that The auxiliary cross-linking agent includes at least one of triallyl cyanurate and triallyl isocyanurate.
6. A method for preparing the fluoroether elastomer composition according to any one of claims 1 to 5, characterized in that: The following steps are involved: A cross-linking aid and a cross-linking agent are added to the fluoroether rubber to obtain a fluoroether elastomer composition.
7. Use of the fluoroether elastomer composition according to any one of claims 1 to 5, characterized in that: The fluoroether elastomer composition is applied in the field of semiconductor technology.
8. The use of the fluoroether elastomer composition according to claim 7, characterized in that: The sealing ring formed by the fluoroether elastomer composition after being heated and vulcanized is used to protect the electrostatic chuck.
9. The use of the fluoroether elastomer composition according to claim 8, characterized in that: The heating vulcanization includes primary heating vulcanization and secondary heating vulcanization. The vulcanization temperature of the primary heating vulcanization is lower than 150° C. and the vulcanization pressure is lower than 5 MPa.
10. The use of the fluoroether elastomer composition according to claim 9, characterized in that: The vulcanization temperature of the one-time heating vulcanization is 120-140° C., and the vulcanization pressure is 1-3 MPa.
Citation Information
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