CN112646352B - High-performance conductive polyphenyl ether/polystyrene alloy material and preparation method and application thereof - Google Patents
High-performance conductive polyphenyl ether/polystyrene alloy material and preparation method and application thereof Download PDFInfo
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- CN112646352B CN112646352B CN202011576148.1A CN202011576148A CN112646352B CN 112646352 B CN112646352 B CN 112646352B CN 202011576148 A CN202011576148 A CN 202011576148A CN 112646352 B CN112646352 B CN 112646352B
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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
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
- C08L71/12—Polyphenylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses a high-performance conductive polyphenyl ether/polystyrene alloy material and a preparation method and application thereof, wherein the high-performance conductive polyphenyl ether/polystyrene alloy material comprises the following components in parts by weight: 30-75 parts of PPO resin; 10-15 parts of PS resin; 5-15 parts of carbon fiber; 5-25 parts of talcum powder. According to the invention, the carbon fiber and the talcum powder are added into the polyphenyl ether/polystyrene alloy and have synergistic effect, so that the conductive stability and the dimensional stability of the material can be well improved, the prepared high-performance conductive polyphenyl ether/polystyrene alloy material still has lower surface resistivity and good dimensional retention rate under a high-temperature condition, the problem of poor surface resistivity stability of the conventional conductive material is solved, the application of the polyphenyl ether composite material is further widened, and the polyphenyl ether/polystyrene alloy material is particularly suitable for the field of electronic packaging.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a high-performance conductive polyphenyl ether/polystyrene alloy material and a preparation method and application thereof.
Background
The PPO/PS alloy formed by blending the PPO and the PS has excellent mechanical property and heat resistance, and is widely applied in the field of electronic packaging (such as IC (integrated circuit) trays). In the packaging process of the IC chip, the IC chip and the tray are generally required to be placed in a high-temperature environment for baking so as to remove moisture on the IC chip and fix the IC chip on the tray through high temperature, so that the material is required to have better dimensional stability and not to deform after being baked at high temperature; in addition, the IC tray is required to have surface conductivity that does not short the IC chip and does not generate electrostatic accumulation, that is, the surface resistivity of the material is required to be maintained within a narrow range.
With the continuous improvement of packaging technology, the requirement on the conductivity of materials is higher and higher, and in order to improve the conductivity of materials, components such as carbon nanotubes, carbon fibers, graphene, conductive carbon black and the like can be generally added into the materials. However, the surface resistivity of the conventional conductive material is not very stable, and is often influenced by the temperature, the injection speed and the pressure during the injection molding process, so that the application of the material is limited. Therefore, the conductive stability and the dimensional stability of the material are improved, the requirements of the electronic packaging field on the material are met, and the main research direction of the invention is.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a high-performance conductive polyphenyl ether/polystyrene alloy material which has stable surface resistivity and higher dimensional stability.
The invention also aims to provide a preparation method of the high-performance conductive polyphenylene oxide/polystyrene alloy material.
The invention is realized by the following technical scheme:
a high-performance conductive polyphenyl ether/polystyrene alloy material comprises the following components in parts by weight:
30-75 parts of PPO resin;
0-15 parts of PS resin;
5-15 parts of carbon fiber;
5-25 parts of talcum powder.
The PPO resin of the invention can be selected from at least one of low-viscosity resin, medium-viscosity resin or high-viscosity resin; preferably, the intrinsic viscosity of the PPO resin is 35-55 cm3(ii) in terms of/g. The intrinsic viscosity is measured according to the standard ASTM D182-2016.
The melt flow rate of the PS resin is 1.0-7.5 g/10min at 220 ℃ under the condition of 10 kg. The melt flow rate was determined with reference to the standard GB/T-3682.1-2018.
The carbon fiber has a length of 3-6 mm and a bulk density of 200-500 g/l. The stability of the material in the manufacturing process can be influenced by the fact that the bulk density of the carbon fibers is too low; too high a packing density adversely affects the dispersibility of the carbon fibers in the matrix, and thus the conductive stability of the material. Preferably, the bulk density of the carbon fiber is 300-400 g/l.
The conductive stability and the dimensional stability of the material are related to the retention length of the carbon fibers in the material, and the talc powder can control the retention length of the carbon fibers in the matrix resin within a smaller range to a certain extent, so that the conductive stability and the dimensional stability of the material are improved.
According to the performance requirements of the material, the high-performance conductive polyphenyl ether/polystyrene alloy material further comprises 0-50 parts by weight of additives; the additive includes at least one of an antioxidant or a lubricant.
The antioxidant is at least one selected from phosphite antioxidant, sulfuric acid-containing antioxidant or phenol antioxidant; specifically, it may be at least one selected from 2,4, 6-tri-tert-butylphenol, 2' -methylenebis (4-methyl-6-tert-butylphenol), pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] or tris (nonylphenyl) phosphite or tris (2, 4-di-tert-butylphenyl) phosphite.
The lubricant is at least one selected from stearic acid, stearate, aromatic amine and fluoride; specifically, it may be selected from at least one of N, N' -ethylene bis stearamide, octadecanoic acid, calcium stearate, poly (1, 1,2,3,3, 3-hexafluoro-1-propene), poly (1, 1-difluoroethylene), polytetrafluoroethylene or a copolymer of 1,1,2,3,3, 3-hexafluoro-1-propene, 1-difluoroethylene and tetrafluoroethylene;
preferably, the lubricant is selected from 1,1,2,3,3, 3-hexafluoro-1-propylene, copolymer of 1, 1-difluoroethylene and tetrafluoroethylene, and the lubricant can improve the conductive stability of the PPO/PS material to a certain extent.
The invention also provides a preparation method of the high-performance conductive polyphenyl ether/polystyrene alloy material, which comprises the following steps:
according to the proportion, PPO resin and PS resin are uniformly mixed and then put into a double-screw extruder, carbon fiber enters the double-screw extruder through a first side feeding port, the carbon fiber enters the double-screw extruder through a second side feeding port, and the high-performance conductive polyphenyl ether/polystyrene alloy material is prepared through extrusion, cooling and granulation; wherein the temperature of each zone of a screw cylinder of the double-screw extruder is 200-270 ℃.
The invention also provides application of the high-performance conductive polyphenyl ether/polystyrene alloy material, which can be used in the field of electronic packaging or the field of automobile parts.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, researches show that the carbon fiber and the talcum powder with specific bulk density are added into the polyphenyl ether/polystyrene alloy and have synergistic effect, so that the conductive stability and the dimensional stability of the material can be well improved, the prepared high-performance conductive polyphenyl ether/polystyrene alloy material still has lower surface resistivity and good dimensional retention rate under the high-temperature condition, the problem of poor surface resistivity stability of the conventional conductive material is solved, the application of the polyphenyl ether composite material is further widened, and the polyphenyl ether/polystyrene alloy material is particularly suitable for the field of electronic packaging.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
The starting materials used for the examples according to the invention and for the comparative examples are now commercially available, but are not limited to these materials:
PPO resin 1: intrinsic viscosity of 45cm3/g；
PPO resin 2: intrinsic viscosity of 60cm3/g；
PS resin 1: the melt flow rate at 220 ℃ under 10kg is 3.5 g/10 min;
PS resin 2: the melt flow rate at 220 ℃ under 10kg is 7.0 g/10 min;
carbon fiber 1: the length is 3mm, and the bulk density is 350 g/l;
carbon fiber 2: the length is 6mm, and the bulk density is 450 g/l;
carbon fiber 3: the length is 3mm, and the bulk density is 100 g/l;
talc powder: purchasing in market;
barium sulfate: purchasing in market;
lubricant 1: n, N' -ethylene bis stearamide;
and lubricant 2: copolymers of 1,1,2,3,3, 3-hexafluoro-1-propene, 1-difluoroethylene and tetrafluoroethylene;
antioxidant: pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Preparation of examples and comparative examples:
according to the proportion shown in the table 1, PPO resin and PS resin are uniformly mixed and then put into a double-screw extruder, carbon fiber enters the double-screw extruder through a first side feeding port, the carbon fiber enters the double-screw extruder through a second side feeding port, and the high-performance conductive polyphenyl ether/polystyrene alloy material is prepared through extrusion, cooling and granulation; wherein the temperature of the barrel 1-12 zone of the double-screw extruder is 200 ℃, 250 ℃, 270 ℃ and 270 ℃.
Relevant performance test methods or standards:
dimensional shrinkage: the dimensional shrinkage is measured after baking for 1h at 120 ℃ according to the reference standard ISO 2577-2007;
surface resistivity: reference standard ASTM D257-07;
deviation in surface resistivity: testing surface resistance by using a 3mm injection molding square plate, testing 5 groups of data of each sample, and respectively calculating standard deviation S and average value 'x, wherein the deviation = S/' x
Table 1: distribution ratio (in parts by weight) of each component in examples 1 to 6 and comparative examples 1 to 3 and related performance test
| Components | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| PPO resin 1 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | ||
| PPO resin 2 | 55 | 47 | ||||||||
| PS resin 1 | 15 | 15 | 15 | 15 | 10 | 15 | 15 | 15 | 15 | |
| PS resin 2 | 12 | |||||||||
| Carbon fiber 1 | 9 | 9 | 7 | 11 | 13 | 9 | / | 9 | ||
| Carbon fiber 2 | 9 | |||||||||
| Carbon fiber 3 | 9 | |||||||||
| Talcum powder | 15 | 15 | 15 | 15 | 20 | 25 | 15 | / | 15 | |
| Barium sulfate | 15 | |||||||||
| Lubricant 1 | 0.3 | / | 0.3 | 0.3 | 0.3 | 0.3 | ||||
| Lubricant 2 | 0.3 | 0.3 | 0.3 | / | 0.3 | |||||
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 | / | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Dimensional shrinkage after baking at 120 ℃ for 1h | 0.15% | 0.14% | 0.15% | 0.21% | 0.08% | 0.06% | 0.18% | 0.28% | 0.65% | 0.31% |
| Surface resistivity/omega | 106 | 105 | 105 | 106 | 105 | 104 | 107 | 106 | >1012 | 106 |
| Deviation of surface resistivity | 0.80 | 0.12 | 0.60 | 0.45 | 0.97 | 0.08 | 3.50 | 2.24 | - | 2.18 |
As can be seen from the above examples and comparative examples, the conductive polyphenylene oxide/polystyrene alloy material prepared by the synergistic effect of the carbon fiber and the talcum powder has the advantages of low dimensional shrinkage rate under high temperature, low surface resistivity, small surface resistivity deviation, and good dimensional stability and conductive stability.
In comparative example 1, carbon fibers having too low a bulk density were used, and the material had large variations in surface resistivity and unstable conductivity as compared with example 1. Compared with the embodiment 1, the comparative example 2 has the advantages that no talcum powder is added, the dimensional stability of the material is poor, the deviation of the surface resistivity is large, and the conductivity is unstable; comparative example 3 compared to example 1, without the addition of carbon fibers, the material had a surface resistivity greater than1012The conductivity is poor; comparative example 4, addition of other inorganic fillers did not have an effect of improving the conductive stability and dimensional stability of the material.
Claims (9)
1. A high-performance conductive polyphenyl ether/polystyrene alloy material is characterized by comprising the following components in parts by weight:
30-75 parts of PPO resin;
10-15 parts of PS resin;
5-15 parts of carbon fiber;
5-25 parts of talcum powder;
the length of the carbon fiber is 3-6 mm, and the bulk density is 200-500 g/l.
2. The high-performance conductive polyphenylene oxide/polystyrene alloy material as claimed in claim 1, wherein the intrinsic viscosity of the PPO resin is 35-55 cm3/g。
3. The high-performance conductive polyphenylene ether/polystyrene alloy material as claimed in claim 1, wherein the melt flow rate of the PS resin at 220 ℃ and 10kg is 1.0-7.5 g/10 min.
4. The high-performance conductive polyphenylene ether/polystyrene alloy material as claimed in claim 1, wherein the bulk density of the carbon fiber is 300 to 400 g/l.
5. The high-performance conductive polyphenylene ether/polystyrene alloy material as claimed in claim 1, further comprising 0-50 parts by weight of an additive; the additive includes at least one of an antioxidant or a lubricant.
6. The high-performance conductive polyphenylene ether/polystyrene alloy material according to claim 5, wherein said antioxidant is selected from at least one of 2,4, 6-tri-tert-butylphenol, 2' -methylenebis (4-methyl-6-tert-butylphenol), pentaerythrityl tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (nonylphenyl) phosphite or tris (2, 4-di-tert-butylphenyl) phosphite; the lubricant is selected from at least one of N, N' -ethylene bis-stearamide, octadecanoic acid, stearate, poly (1, 1,2,3,3, 3-hexafluoro-1-propene), poly (1, 1-difluoroethylene), polytetrafluoroethylene or a copolymer of 1,1,2,3,3, 3-hexafluoro-1-propene, 1-difluoroethylene and tetrafluoroethylene.
7. The high-performance conductive polyphenylene ether/polystyrene alloy material according to claim 6, wherein said lubricant is selected from the group consisting of 1,1,2,3,3, 3-hexafluoro-1-propene, a copolymer of 1, 1-difluoroethylene and tetrafluoroethylene.
8. The preparation method of the high-performance conductive polyphenylene ether/polystyrene alloy material as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
according to the proportion, the PPO resin and the PS resin are uniformly mixed and then put into a double-screw extruder, carbon fiber enters the double-screw extruder through a first side feeding port, talcum powder enters the double-screw extruder through a second side feeding port, and the high-performance conductive polyphenyl ether/polystyrene alloy material is prepared through extrusion, cooling and granulation; wherein the temperature of each zone of a screw cylinder of the double-screw extruder is 200-270 ℃.
9. The use of the high-performance conductive polyphenylene ether/polystyrene alloy material according to any one of claims 1 to 7, wherein the material is used in the field of electronic packaging or in the field of automobile parts.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03250047A (en) * | 1990-02-28 | 1991-11-07 | Nippon G Ii Plast Kk | Conductive resin composition |
| EP0564660A1 (en) * | 1991-10-25 | 1993-10-13 | MITSUI TOATSU CHEMICALS, Inc. | Tray for integrated circuits |
| JPH1045979A (en) * | 1996-08-08 | 1998-02-17 | Sumitomo Chem Co Ltd | Thermoplastic resin composition |
| JP2003041131A (en) * | 2001-05-21 | 2003-02-13 | Teijin Chem Ltd | Thermoplastic resin composition and molded product of chassis |
| CN111117203A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特伴泰材料科技有限公司 | Conductive, high-mechanical-property and low-warpage fiber-reinforced polyphenyl ether composite material and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03250047A (en) * | 1990-02-28 | 1991-11-07 | Nippon G Ii Plast Kk | Conductive resin composition |
| EP0564660A1 (en) * | 1991-10-25 | 1993-10-13 | MITSUI TOATSU CHEMICALS, Inc. | Tray for integrated circuits |
| JPH1045979A (en) * | 1996-08-08 | 1998-02-17 | Sumitomo Chem Co Ltd | Thermoplastic resin composition |
| JP2003041131A (en) * | 2001-05-21 | 2003-02-13 | Teijin Chem Ltd | Thermoplastic resin composition and molded product of chassis |
| CN111117203A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特伴泰材料科技有限公司 | Conductive, high-mechanical-property and low-warpage fiber-reinforced polyphenyl ether composite material and preparation method thereof |
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