CN113861598A - FFKM sealing ring for wafer processing process cavity application system and preparation method thereof - Google Patents
FFKM sealing ring for wafer processing process cavity application system and preparation method thereof Download PDFInfo
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- CN113861598A CN113861598A CN202111242082.7A CN202111242082A CN113861598A CN 113861598 A CN113861598 A CN 113861598A CN 202111242082 A CN202111242082 A CN 202111242082A CN 113861598 A CN113861598 A CN 113861598A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
- B29B7/726—Measuring properties of mixture, e.g. temperature or density
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/26—Sealing devices, e.g. packaging for pistons or pipe joints
- B29L2031/265—Packings, Gaskets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- Oral & Maxillofacial Surgery (AREA)
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- Physics & Mathematics (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Sealing Material Composition (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses an FFKM sealing ring for a wafer processing process cavity application system and a preparation method thereof, belonging to the field of semiconductor chip manufacturing. The FFKM sealing ring is prepared from the following raw materials in parts by weight: 100 parts of FFKM virgin rubber and 1.5 parts of TR 1310.5. The FFKM sealing ring has the advantages of high physical and mechanical properties, excellent pressure change performance, super-strong medium resistance, excellent cleanliness, good plasma resistance, easy mixing and vulcanization molding of FFKM rubber, long scorching time, easy production operation and the like, and is widely used for sealing a cavity application system in a wafer processing process.
Description
Technical Field
The invention belongs to the technical field of semiconductor chip manufacturing, and particularly relates to an FFKM sealing ring for a wafer processing process cavity application system and a preparation method thereof.
Background
In the field of semiconductor chip fabrication, wafer processing is typically exposed to extreme plasma radiation, heat, and chemical media (O)2、CF4、NF3、SF6) In the environment. Wafer processing has high environmental cleanliness requirements. For semiconductor manufacturers, it is an important task to isolate the gases, extractables, and particulate contaminants generated during the seal interpretation process. If the common fluorine-containing rubber is used as the sealing ring for the cavity application system of the wafer processing process, the harsh general environmental requirements are difficult to meet, the pollution to the wafer and the molded chip is easy to cause, and the product quality is damaged.
The FFKM sealing ring is an important component of a cavity application system in a wafer processing process, is one of important environmental control indexes of wafer processing, develops the FFKM sealing ring with independent intellectual property rights, can break through monopoly of foreign technologies, fills up the technical blank of the FFKM sealing ring at home and abroad, enables domestic intelligent products to be used as safe and reliable 'Chinese cores', and has great strategic significance in improving the international competitiveness of national industry.
Disclosure of Invention
The present invention provides an FFKM seal ring for a cavity application system in a wafer processing process and a method for manufacturing the same.
The invention discloses an FFKM sealing ring for a cavity application system of a wafer processing process, which is prepared from the following raw materials in parts by weight:
100 parts of FFKM virgin rubber and 1.5 parts of TR 1310.5; preferably 100 parts of FFKM virgin rubber and 1.0-1310.7 parts of TR.
In some preferred embodiments of the invention, the FFKM raw gum has a F content of 70-75% by mole.
In some preferred embodiments of the present invention, the FFKM seal ring is free of filler material. The filling material may be: carbon black, white carbon black, GO and the like.
The second aspect of the present invention discloses a method for preparing the FFKM sealing ring according to the first aspect, comprising the steps of:
s11, mixing the FFKM raw rubber with TR131, and cooling to obtain FFKM rubber compound;
s12, performing extrusion preforming to obtain the rubber rope;
s13, placing the sealing ring mould in a vulcanizing machine for preheating, placing the cut rubber rope in the mould, and carrying out pressure vulcanization molding;
s14, trimming the formed sealing ring;
and S15, heating for secondary vulcanization, and cooling to obtain the FFKM sealing ring.
In some preferred embodiments of the present invention, three-pack two-roll mill mixing is used, preferably at a temperature of 40 ℃ to 80 ℃.
In some preferred embodiments of the present invention, in S11, the roll shaft is kept water-feeding and cooled during the mixing, and the roll ratio is preferably (1.0: 1.2) - (1.0: 2.0).
In some preferred embodiments of the present invention, in S12, the extrusion preform is a single screw extruder extrusion; the preferred extrusion temperature is 23-80 ℃ and the working pressure is 5-15 Mpa.
In some preferred embodiments of the present invention, in S13, the press vulcanization is formed into a one-stage vulcanization in a press vulcanizer, preferably under the vulcanization conditions of 150 ℃ and 175 ℃, 60-600S and 10-20 MPa.
In some preferred embodiments of the present invention, in S15, the conditions of the secondary vulcanization are 200-240 ℃ and 8-24 h.
In some preferred embodiments of the present invention, in S15, the secondary vulcanization is pressure vulcanization under nitrogen medium, preferably 0.1-0.6 MPa.
In some preferred embodiments of the present invention, in S15, the temperature is raised to 200-240 ℃ for 2.5 h; 200 and 240 ℃ is cooled to room temperature for 2.5 h.
The FFKM is full fluorine ether rubber, and the TR131 is high-density polyethylene.
The beneficial technical effects of the invention are as follows:
the invention adopts a certain amount of FFKM virgin rubber and auxiliary materials to match according to a ratio, and the materials are mixed on an open mill to obtain the novel FFKM rubber compound for the sealing ring for gas supply at the equipment end of the wafer processing process with excellent performance, and then the FFKM rubber compound is subjected to one-stage and two-stage vulcanization molding to form the finished product of the FFKM sealing ring. The FFKM sealing ring has the advantages of high physical and mechanical properties, excellent pressure-variable performance, super-strong medium resistance, excellent cleanliness, good plasma resistance, easy mixing and vulcanization molding of the FFKM rubber, long scorching time, easy production operation and the like, and is widely used for sealing a cavity application system in wafer processing procedures.
The FFKM sealing ring for the wafer processing procedure cavity application system has the advantages that the raw materials are simple in component, the filling material is not contained, the performance of the sealing ring product is regulated and controlled through the specifically selected raw materials and the specific proportion of the raw materials, the preparation method has no obvious steps which are difficult to control, the obtained FFKM sealing ring is excellent in performance, and the use of the wafer processing procedure cavity application system can be met.
Drawings
Fig. 1 is an EDS test chart of an FFKM seal ring according to an embodiment of the present invention;
fig. 2 is a TG test chart of an FFKM seal ring according to an embodiment of the present invention.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The examples and comparative examples were, unless otherwise specified, parallel tests in which the components, the component contents, the production steps, and the production parameters were the same.
The FFKM virgin rubber is perfluoroether rubber, wherein the molar content of F is 70-75%; the TR131 is high-density polyethylene.
Example 1:
a novel FFKM sealing ring for a wafer processing procedure cavity application system is prepared from the following components in parts by weight:
100 parts of FFKM virgin rubber and 1310.7 parts of TR.
The preparation method comprises the following steps:
preparing the FFKM virgin rubber and the auxiliary materials in proportion, conveying the mixture into an open mill, performing thin-pass mixing in a three-pack two-roll mode, and cooling a lower sheet to obtain the FFKM rubber compound of the sealing ring for gas supply at the end of the wafer processing equipment. The mixing temperature is 55 ℃, the roll shafts are kept to be filled with water for cooling, and the speed ratio of the two roll shafts is 1: 1.27.
placing the rubber compound into a single-screw extruder to perform into a rubber rope, wherein the temperature of the extruder head is 65 ℃. The working pressure of the extruder is 5 Mpa.
And placing the seal ring mold in a vulcanizing machine for preheating. And putting the cut rubber rope into a die, overlapping the rubber rope end to end, and pressurizing for one section to perform vulcanization molding. The vulcanization conditions are as follows: 170 ℃ 300s 15 MPa.
And (4) trimming the first-section formed sealing ring, and then putting the trimmed sealing ring into a second-section vulcanization oven. The oven was flushed with nitrogen under a pressure of 0.2 MPa. And (c) beginning temperature control (the temperature treatment procedure is that a: the room temperature is increased to 200 ℃, the temperature is increased to room temperature by 2.5 h.b: the temperature is maintained at 200 ℃ and 16 h.c: the temperature is reduced to the room temperature by 200 ℃ for 2.5 h), carrying out secondary vulcanization, and then taking out the finished product.
The FFKM sealing ring has the following test performances:
the results of the obtained FFKM seal ring, EDS test and TG test are shown in fig. 1 and fig. 2.
Example 2:
a novel FFKM sealing ring for a wafer processing procedure cavity application system is prepared from the following components in parts by weight:
100 parts of FFKM virgin rubber and 1311 parts of TR.
The preparation method comprises the following steps:
preparing the FFKM virgin rubber and the auxiliary materials in proportion, conveying the mixture into an open mill, performing thin-pass mixing in a three-pack two-roll mode, and cooling a lower sheet to obtain the FFKM rubber compound of the sealing ring for gas supply at the end of the wafer processing equipment. The mixing temperature is 55 ℃, the roll shafts are kept to be filled with water for cooling, and the speed ratio of the two roll shafts is 1: 1.27.
placing the rubber compound into a single-screw extruder to perform into a rubber rope, wherein the temperature of the extruder head is 65 ℃. The working pressure of the extruder is 5 Mpa.
And placing the seal ring mold in a vulcanizing machine for preheating. And putting the cut rubber rope into a die, overlapping the rubber rope end to end, and pressurizing for one section to perform vulcanization molding. The vulcanization conditions are as follows: 175 ℃ 500s 15 MPa.
And (4) trimming the first-section formed sealing ring, and then putting the trimmed sealing ring into a second-section vulcanization oven. The oven was flushed with nitrogen gas under a pressure of 0.3 MPa. And (c) beginning temperature control (the temperature treatment procedure is that a: the room temperature is increased to 220 ℃, the temperature is increased to room temperature by 2.5 h.b: the temperature is maintained at 200 ℃, the temperature is increased to 24: 24 h.c: 220 ℃, the temperature is reduced to room temperature by 2.5 h), and then taking out the finished product.
The FFKM sealing ring has the following test performances:
example 3:
the difference from example 1 is that FFKM virgin rubber is 100 parts, TR 1310.5 parts.
Example 4:
the difference from example 1 is that FFKM virgin rubber is 100 parts, TR 1311.5 parts.
Example 5:
the difference from example 1 is that FFKM virgin rubber is 100 parts, TR 1310.3 parts.
Example 6:
the difference from example 1 is that FFKM virgin rubber is 100 parts, TR 1312 parts.
In the FFKM seal ring for the novel wafer processing process chamber application system of examples 3-6, in the formulation, when the FFKM virgin rubber is 100 parts and the TR 1310.5-1.5 parts, the seal ring hardness is above 65sha, the tensile strength is above 13MPa, the elongation at break is above 160%, the pressure change (25%, 22h, 270 ℃) is above 30%, the seal member is resistant to media (O2, CF4, NF3, SF6) (200 ℃ for 72h), and the product appearance is unchanged and has no cracks. Among them, TR131 is preferably 0.7 to 1.0, and most preferably TR131 is 1.0. When the FFKM virgin rubber is 100 parts and TR131 is less than 0.5 or more than 1.5, for example, 0.3 part of example 5 and 2 parts of example 6, the above properties are partially or totally remarkably deteriorated.
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (10)
1. The FFKM sealing ring for the cavity application system in the wafer processing process is characterized in that the prepared raw materials comprise the following components in parts by weight:
100 parts of FFKM virgin rubber and 1.5 parts of TR 1310.5; preferably 100 parts of FFKM virgin rubber and 1.0-1310.7 parts of TR.
2. The FFKM seal ring of claim 1 wherein the FFKM raw rubber has a F content of 70-75 mol%.
3. The FFKM seal ring of claim 1 or claim 2 wherein the FFKM seal ring is free of filler material.
4. A method for preparing an FFKM seal ring according to any one of claims 1 to 3, comprising the steps of:
s11, mixing the FFKM raw rubber with TR131, and cooling to obtain FFKM rubber compound;
s12, performing extrusion preforming to obtain the rubber rope;
s13, placing the sealing ring mould in a vulcanizing machine for preheating, placing the cut rubber rope in the mould, and carrying out pressure vulcanization molding;
s14, trimming the formed sealing ring;
and S15, heating for secondary vulcanization, and cooling to obtain the FFKM sealing ring.
5. The method according to claim 4, characterized in that in S11, the mixing is carried out in an open mill by adopting three-pack two-roll thin-pass mixing, and the mixing temperature is preferably 40-80 ℃;
and/or in S11, the roll shaft is kept water-flowing and cooled during mixing, and the ratio of the roll speed to the roll speed is preferably (1.0: 1.2) - (1.0: 2.0).
6. The method according to any one of claims 4 or 5, wherein in S12, the extrusion preform is a single screw extruder extrusion molding; the preferred extrusion temperature is 23-80 ℃ and the working pressure is 5-15 Mpa.
7. The method according to any one of claims 4 to 6, wherein in S13, the press vulcanization molding is one-stage vulcanization in a press vulcanizer, preferably under the vulcanization conditions of 150 ℃ and 175 ℃, 60 to 600S and 10 to 20 MPa.
8. The method as claimed in any one of claims 4 to 7, wherein in S15, the conditions of the secondary vulcanization are 200 ℃ and 240 ℃ and 8-24 h.
9. The process according to any one of claims 4 to 8, wherein in S15, the secondary vulcanization is carried out under pressure under a nitrogen medium, preferably at a nitrogen pressure of 0.1 to 0.6 MPa.
10. The method according to any one of claims 4-9, wherein in S15, the temperature is raised to 200 ℃ and 240 ℃ for 2.5 h; 200 and 240 ℃ is cooled to room temperature for 2.5 h.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111081163 | 2021-09-15 | ||
| CN2021110811633 | 2021-09-15 |
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| Publication Number | Publication Date |
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| CN113861598A true CN113861598A (en) | 2021-12-31 |
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| CN202111242082.7A Pending CN113861598A (en) | 2021-09-15 | 2021-10-25 | FFKM sealing ring for wafer processing process cavity application system and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0517627A (en) * | 1991-07-09 | 1993-01-26 | Nippon Valqua Ind Ltd | Lubricating rubber composition and lubricating rubber molding made therefrom |
| CN101120435A (en) * | 2005-02-15 | 2008-02-06 | 日本华尔卡工业株式会社 | Seal material for semiconductor production apparatus |
| US20190367372A1 (en) * | 2018-05-31 | 2019-12-05 | Nanotek Instruments, Inc. | Process for producing graphene foam-based sealing materials |
| CN111925615A (en) * | 2020-07-10 | 2020-11-13 | 上海如实密封科技有限公司 | High-strength high-modulus perfluoroether rubber material and preparation method and application thereof |
-
2021
- 2021-10-25 CN CN202111242082.7A patent/CN113861598A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0517627A (en) * | 1991-07-09 | 1993-01-26 | Nippon Valqua Ind Ltd | Lubricating rubber composition and lubricating rubber molding made therefrom |
| CN101120435A (en) * | 2005-02-15 | 2008-02-06 | 日本华尔卡工业株式会社 | Seal material for semiconductor production apparatus |
| US20190367372A1 (en) * | 2018-05-31 | 2019-12-05 | Nanotek Instruments, Inc. | Process for producing graphene foam-based sealing materials |
| CN111925615A (en) * | 2020-07-10 | 2020-11-13 | 上海如实密封科技有限公司 | High-strength high-modulus perfluoroether rubber material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周大纲等编著: "《土工合成材料制造技术及性能》", 31 March 2001, 中国轻工业出版社 * |
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