CN101016406A - Ultra-clean antistatic resin composition, preparing method thereof, product containing the same and application thereof - Google Patents
Ultra-clean antistatic resin composition, preparing method thereof, product containing the same and application thereof Download PDFInfo
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Abstract
The invention discloses a super clean antistatic resin composition, preparing method and product through utilizing this composition and application in barrier electromagnetic field, which comprises the following parts: 63-98% plastic base material; 1-30% nanometer grade carbon pipe and/or nanometer grade carbon black; 0.1-0.5% coupling agent; 0.1-5% dispersing agent; 0.5-1.5% oxidation resistance agent. This product possesses good electrostatic resistance property and super clean property.
Description
Technical field
The present invention relates to frock clamp material and the used ultra-clean antistatic/conduction/shield engineering plastics of wrapping material in the electrostatic sensitive electronic devices and components assembling procedure, relate in particular to a kind of ultra-clean antistatic resin composition, its preparation method and utilize the product of said composition preparation and the application in shield electromagnetic.
Background technology
Along with the fast development and the semi-conductor of semi-conductor and wafer technologies with wafer is manufacturing is surging forward, the production process of electrostatic sensitive electronic devices and components is also more and more higher to the frock clamp (mainly comprising pallet that is used for splendid attire and transmission electronic element etc.) and the requirement of wrapping material, is mainly reflected in the antistatic performance and the clean performance demands of frock clamp and wrapping material more and more tighter.
Need to use the pallet and the various wrapping material that are used to pack semiconducter device of a large amount of splendid attires and transmission electronic element in semi-conductor and the wafer technologies field, miniaturization, microminiaturization along with semiconducter device, the antistatic performance of employed various frock clamps that contact with semiconducter device and wrapping material must improve constantly in the production process, otherwise the electrostatic damage (this damage is difficult to detect sometimes) that can cause device to be existed when contacting with wrapping material with frock clamp causes serious consequence.And, cause device quality to descend even damage because device is more and more littler, and the clean performance of frock clamp and wrapping material also must improve constantly, otherwise the situation that device is contaminated, stain can occur.
Yet, employed frock clamp and wrapping material mainly utilize various engineering plastics in this field at present, for example polyetherimide or title poly ether imide (PEI), polycarbonate (PC), polyphenylene oxide (PPO) and polyoxymethylene (POM) etc. are difficult to satisfy the antistatic performance and the clean performance requriements that improve constantly in this field.
The material that is using at present normally adds the antistatic performance that electro-conductive fiber, conductive carbon black and metal powder etc. solve material in plastic basis material.With the polyetherimide is example, and as shown in Figure 1, Fig. 1 is the middle electron photomicrograph that adds conductive carbon fibre of the polyetherimide (PEI) of prior art, and columned additive promptly is a conductive carbon fibre among the figure, and all the other are plastic basis materials.
Fig. 2 and Fig. 3 further illustrate the defective of this conventional art.Fig. 2 also is the middle electron photomicrograph that adds conductive carbon fibre of the polyetherimide (PEI) of prior art, circle wherein promptly is a conductive carbon fibre, arrow refers to the enlarged view at conductive carbon fibre position among Fig. 3), show among the figure, around the conductive carbon fibre is nonconducting plastic basis material, and the ununiformity of its distribution leaks.What Fig. 1 and Fig. 2 showed is the photo of different sites in the same sample.Show among Fig. 1, Fig. 2, Fig. 3, conductive carbon fibre skewness in plastic basis material in the prior art, the place that conductive carbon fibre is intensive presents antistatic performance preferably, and the place that conductive carbon fibre is loose then shows insulativity.And the cleanliness of material of the prior art also has much room for improvement.
Summary of the invention
The objective of the invention is in order to overcome the defective that existing frock clamp and wrapping material exist in the semiconductor applications, adopted nano level conductive carbon pipe/nano level conductive carbon black and plastic basis material blend, solved conductive additive targetedly and disperseed uneven problem.Realized the raising of material at antistatic performance and clean aspect of performance.
The invention provides a kind of ultra-clean antistatic resin composition, mainly comprise: plastic basis material 63～98%, nano-scale carbon tube and/or nano grade carbon black 1～30%, coupling agent 0.1～0.5%, dispersion agent 0.1～5%, antioxidant 0.5～1.5%.
According to ultra-clean antistatic resin composition of the present invention, wherein said plastic basis material is selected from the group of being made up of polyetherimide (PEI), polycarbonate (PC), polyphenylene oxide (PPO) and polyoxymethylene (POM), polyolefine.
According to ultra-clean antistatic resin composition of the present invention, wherein said coupling agent is selected from organic chromium complex compound, silane coupling agent, titante coupling agent and zirconium class coupling agent.
According to ultra-clean antistatic resin composition of the present invention, wherein said dispersion agent is selected from paraffin oil, polyethylene wax, oxidized polyethlene wax, fatty acid soaps class, fatty acid ester, fatty acyl amide and ester class according to of the present invention.
According to ultra-clean antistatic resin composition of the present invention, wherein said antioxidant is selected from organophosphite and hindered phenol.
The present invention also provides a kind of preparation method of ultra-clean antistatic resin material, may further comprise the steps:
1) mixes following component: plastic basis material 63～98%, CNT (carbon nano-tube)/carbon black 1～30%, coupling agent 0.1～0.5%, dispersion agent 0.1～5%, antioxidant 0.5～1.5%;
2) utilize dual-screw pelletizer with the mixture pelleting that obtains in the previous step, obtain the ultra-clean antistatic resin material.
The present invention also is provided for the ultra-clean antistatic product of semiconductor applications, and it is formed by ultra-clean antistatic resin composition according to the present invention.In one embodiment, this product is the pallet that is used for splendid attire and transmission electronic element.
The present invention also provides the application of this ultra-clean antistatic resin composition in shield electromagnetic.
Material according to the invention has the good anti-static performance, and nano level conductive carbon pipe/carbon black is evenly distributed in the plastic basis material, and difficult drop-off can reach super clean requirement.And has certain shielding according to material provided by the invention.
Description of drawings
Fig. 1 is the middle electron photomicrograph (SEM, 500 times) that adds conductive carbon fibre of the polyetherimide (PEI) of prior art.
Fig. 2 is middle another electron photomicrograph (SEM, 500 times) that adds conductive carbon fibre of the polyetherimide (PEI) of prior art, and what itself and Fig. 1 showed is the different sites of same sample.
Fig. 3 is the partial enlarged drawing (SEM, 2000 times) of the electron photomicrograph among Fig. 2.
Fig. 4 shows transmission electron microscope according to an embodiment of the invention (TEM) photo.
Fig. 5 shows scanning electron microscope according to an embodiment of the invention (SEM) photo.
Embodiment
Composition
The invention provides a kind of ultra-clean antistatic resin composition, comprising: plastic basis material 63～98%, nano-scale carbon tube and/or carbon black 1～30%, coupling agent 0.1～0.5%, dispersion agent 0.1～5%, antioxidant 0.5～1.5%.Wherein, each components contents is the quality percentage composition based on the total mass of composition, and if no special instructions, content or percentage composition among the application are mass content.
Plastic basis material
Be applicable to that plastic basis material of the present invention is various thermoplastic resins, be preferably thermoplastic engineering plastic, for example polyetherimide or title poly ether imide (PEI), polycarbonate (PC), polyphenylene oxide (PPO) and polyoxymethylene (POM), polyolefine (as polyethylene, polypropylene) etc.As the thermoplastic resin example, can adopt the thermoplastic resin of polyetherimide, polyphenylene oxide, polyoxymethylene, polyethylene, polypropylene, polyvinyl chloride, polyvinylidene chloride, ABS resin, polystyrene, acrylonitrile styrene resin (AS), (methyl) acrylic resin, polyvinyl alcohol, EVA, polyamide resin, polyacetal resin, polycarbonate resin, vibrin, tetrafluoroethylene, fluoro-resin, poly-imines, polyimide etc., and the mixture of these materials.
Thermoplastic resin preferably have with the affinity height of carbon nanotube, have certain-length molecular length, have characteristics such as flexibility.This thermoplastic resin preferably has 10,000 to 1,000,000, more preferably has 50,000 to 300,000 molecular-weight average.In this scope, the thermoplastic resin molecule is bonded with each other, and makes therefore to make even carbon nanotube be dispersed in the resin matrix between the carbon nanotube that molecular resin enters into easily.The various thermoplastic resins that use in the prior art all are applicable to the present invention.According to the present invention, the consumption of thermoplastic resin is 63% to 98% of a material total mass.
Nano-scale carbon tube or nano grade carbon black
Nano-scale carbon tube (being called carbon nanotube or conductive nano carbon pipe again) comprises that single layer structure cylindraceous or these cylindrical structures are configured to canular multilayered structure.That is, carbon nanotube can be made of individual layer, also can be made of multilayer, can also comprise single layer structure and multilayered structure simultaneously.And, can also use part to comprise the carbon material of carbon nanotube structure.The carbon nanotube mean diameter is 0.5 to 200nm, is preferably 20-100nm, and more preferably 30nm is above to 100nm.And carbon nanotube both can be that the fibers straight shape also can be the curved fiber shape.
Single-layer carbon nano-tube or multilayer carbon nanotube can pass through method preparations such as arc-over, laser ablation, vapour deposition.Arc discharge method is under subatmospheric slightly argon of pressure or hydrogen atmosphere, carries out arc-over between the electrode materials made from carbon-point, thereby obtains being piled up in the method for the multilayer carbon nanotube on the negative electrode.In addition, single-layer carbon nano-tube is from catalyzer such as mixed Ni/cobalts carbon-point and after carrying out arc-over, is attached to obtain in the carbon black on the processing vessel medial surface.The laser ablation method is a kind of in argon gas, by making carbon material surface fusion, evaporation to the carbon material surface irradiation intense pulse laser that is mixed with catalyzer such as nickel/cobalt as target, thereby obtains the method for single-layer carbon nano-tube.Vapour deposition process is that hydrocarbon polymers such as pyrolysis benzene, toluene more specifically, can be enumerated flowing catalyst method, Zeolite support catalyst method etc. to form carbon nanotube in gas phase.
Preferably, carbon nanotube carried out surface treatment in advance before mixed with resin material, for example, and by carrying out ion implantation processing, sputter etching processing, plasma treatment etc., to improve and the combining of resin.Make carbon nanotube to be evenly dispersed in the resin matrix.According to the present invention, the addition of carbon nanotube is 1% to 30%.
Nano grade carbon black (nanometer conductive carbon black) is nano level carbon black powder, and its particle diameter is usually below 100 nanometers.It can be by the preparation of micron order carbon black, and the preparation method can be referring to Chinese patent application 200310121138.9.Similar with CNT (carbon nano-tube), carbon is received carbon black and carried out surface treatment in advance before mixed with resin material, for example, and by carrying out ion implantation processing, sputter etching processing, plasma treatment etc., to improve and the combining of resin.The addition of nanometer carbon black is 1% to 30%.
According to the present invention, nano-scale carbon tube and nano grade carbon black can join in the resin combination respectively.Alternatively, both also can join in the resin combination simultaneously.
Coupling agent
Coupling agent is the material with two kinds of groups of different nature, and wherein a part of group can or combine with the molecular resin reaction, and another part group is used for combining with carbon nanotube, thereby strengthens the associativity between resin material and the carbon nanotube.Because material require of the present invention has the good anti-static performance simultaneously, carbon nanotube and resin uniform mixing must be dispersed in the molecular resin with making even carbon nanotube.Material according to the invention must have super clean performance simultaneously, and this requires the stability of each composition in resin in the material necessary very good, and each composition can not permeate to material surface.Therefore, coupling agent is the component of necessity among the present invention, and its add-on is 0.1% to 0.5% of a mass ratio.
The coupling agent that can be used for composition of the present invention comprises: organic chromium complex compound, silane coupling agent, titante coupling agent and zirconium class coupling agent are preferably silane coupling agent.Wherein zirconium class coupling agent is the low-molecular-weight inorganic polymer that contains zirconium aluminate, can change the rheological property of matrix material.Under the situation of needs change rheological, be preferably zirconium class coupling agent.
Dispersion agent
Dispersion agent in the embodiments of the invention be used for changing carbon nanotube at the dispersion effect of plastic basis material to improve antistatic property and super cleanliness.There is multiple dispersion agent in the prior art, for example hydro carbons (paraffin oil, polyethylene wax, oxidized polyethlene wax etc.), fatty acid soaps class, fatty acid ester, fatty acyl amide and ester class etc., those skilled in the art can select as required.
The kind of dispersion agent can be selected as required, so that effectively promote the dispersion effect of carbon nanotube in base material.In the present invention, the usage quantity of dispersion agent is the 0.1-5% of composition total weight.
Antioxidant
Antioxidant is the auxiliary agent that is used to improve the ageing resistance of composition, any suitable antioxidant may be used to the present invention, except having good antioxidant property, be used for antioxidant of the present invention and also must after moulding, have good anti-extractable, otherwise be difficult to the requirement of satisfied super cleanliness.The present invention preferably uses with organophosphite and hindered phenol to the antioxidant system stablizer of main body as antioxidant, and when being used for composition of the present invention, it has good oxidation-resistance and anti-extractable.In the present invention, the usage quantity of antioxidant is about 0.5-1.5% of composition total weight.Those skilled in the art can be according to the consumption of concrete processing condition appropriate change antioxidant.
Before thermoplastic resin and carbon nanotube mix, in the mixing process or afterwards, can be added in other known additives that is adopted in thermoplastic resin molded, for example releasing agent, pigment, fluidizer, strongthener, fire retardant etc.But the additive of adding can not have infringement for the dispersiveness of carbon nanotube and the super cleanliness of material.
Mixing, granulation
Each composition according to composition of the present invention obtains blend by mixing.Blend polymer is meant the mixture that obtains by with two or more composition blend.Mainly physical bond between each component in the blend, but, in the blending and modifying process, also can make and have a small amount of chemical bond between the wherein different polymer macromolecules, for example in the melting mixing process under strong shear action, may produce the macromole fracture a large amount of free radicals, thereby form a small amount of block or graft copolymer because shearing action makes.Therefore, blend is different from general copolymerized macromolecule compound, also is different from polymer blend in general sense.Composition according to the present invention can obtain good dispersiveness and stable after blend.
Blend mainly adopts the preparation of mechanical blending method, is about to each component uniform mixing in mixing equipment (as high-speed mixer, forcing machine).
In blend, the morphological structure of blend has fundamental influence to its performance, and its morphological structure at first is subjected to participating in the restriction of the thermodynamic compatibility between the polymeric constituent of blend, can promote consistency between each component to make each component be in stable mixing state by coupling agent and dispersion agent.
In according to one embodiment of present invention,, with nano-scale carbon tube/nano grade carbon black and plastic basis material and other auxiliary agent mixing granulation, produce the ultra-clean antistatic material through compounding by dual-screw pelletizer.
Utilization is according to ultra-clean antistatic material of the present invention, through inject, extrude, moulding process such as mold pressing, can make products such as the various frock clamps that are used for semiconductor applications and wrapping material, for example be used for the pallet of splendid attire and transferring semiconductor device.This product has good antistatic performance and super clean performance.In product prepared in accordance with the present invention, nano level conductive carbon pipe/carbon black is evenly distributed in the plastic basis material, and difficult drop-off can reach super clean requirement.Conventional art is because of conductive additive skewness in plastic basis material, thereby presents the ununiformity of antistatic performance.And it is little according to conductive additive size in the product of the present invention to nano level, and add suitable coupling agent, dispersion agent, antioxidant etc., solve the distributing homogeneity problem of conductive additive, thereby can reach high-level anti-electrostatic requirement and cleanliness requirement simultaneously.
In addition, material according to the invention can be by increasing the ratio of electrical-conductive nanometer carbon pipe/electrical-conductive nanometer carbon black, and the resistance that reduces matrix material has both electro-magnetic screen function.Evidence utilizes the product of material manufacturing of the present invention to have good electrical conductivity, has certain electro-magnetic screen function.
Technique effect of the present invention
Material according to the invention possesses superior antistatic performance and clean performance simultaneously.Conductive additive is nano level carbon pipe/nano grade carbon black, and it is evenly distributed in the plastic basis material, forms to lead away the electrostatic path.Nano level conductive additive combines closely difficult drop-off with plastic basis material simultaneously.Thereby realize having good anti-static performance and clean performance simultaneously, but also have certain electro-magnetic screen function.
Embodiment
CNT (carbon nano-tube) and nanometer carbon black adopt the product of Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences.Coupling agent adopts the LD series (titanate coupling agent) and the silane coupling agent series of Yangzhou Rieter Perfojet.Dispersion agent adopts the LD404 (acrylic copolymer) of Yangzhou Rieter Perfojet.Antioxidant adopts the antioxidant 1010 (four [methyl-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester) and the antioxidant 168 (tricresyl phosphite (2,4-di-tert-butyl-phenyl ester)) of the big chemical industry company limited in sea, Qingdao.
Embodiment 1
Plastic basis material PEI 75g, CNT (carbon nano-tube) 19.5g, silane coupling agent 0.5g, dispersion agent acrylic copolymer 4g, the antioxidant tricresyl phosphite (2,4-di-tert-butyl-phenyl ester 1g.
Above-mentioned materials by the common double screw pelletizer, with nano-scale carbon tube/nano grade carbon black and plastic basis material and auxiliary agent mixing granulation, is produced the ultra-clean antistatic material through compounding.The particulate material that utilizes embodiment 1 is through injection molding preparation standard model, so that make a service test.The transmission electron microscope of the model of embodiment 1 (TEM) figure shows that CNT (carbon nano-tube) is evenly dispersed in the resin material, as shown in Figure 4.The scanning electron microscope of the model of embodiment 1 (SEM) figure shows that CNT (carbon nano-tube) is evenly dispersed in the resin material, as shown in Figure 5.
Comparative example 1
The PEI product of buying the commercially available existing adding conductive carbon fibre that is used for semiconductor device fabrication as a comparative example.
The antistatic property test, the technical indicator comparing result of the material of the material of embodiment 1 and comparative example 1 sees Table 1.
Table 1
| Technical indicator | Comparative example 1 | The material of embodiment 1 |
| The material surface static voltage | 4 volts | 1 volt |
| Material surface friction voltage | 50 volts | 3 volts |
| The point-to-point resistance of material | 10 8～10 11Ohm | 10 7～10 8Ohm |
| Material fall time | 2 seconds | 0.1 second |
These parameters adopts the standard method of test of ESD S11.11, ASTM D257 and FTMS-101C to measure.
Super clean performance test, the super clean technology index comparing result of the material of the material of embodiment 1 and comparative example 1 sees Table 2.
Table 2
| Technical indicator | Comparative example 1 | Embodiment 1 |
| Liquid particle count test (LPC): granule number/cm 2 | ?28046 | ?2753 |
| Volatile gases test (SHS): μ g/g | ?2.138 | ?0.653 |
Liquid particle count test (LPC) step:
1. prepare clean beaker, add 50 milliliters pure water.
2. the beaker that water will be housed is put into the ultrasonic cleaning cylinder and is shaken and wash one minute, takes out beaker and leaves standstill 10 minutes.
3. with the granule content in the water in the laser liquid grain count instrument mensuration beaker, be decided to be blank value (granule number/milliliter).
4. get same beaker and add 50 milliliters of pure water, put into the model of the demarcation size that will test.
5. repeating step 2,3, the sample value of the sample that obtains testing (granule number/milliliter).
6. result=(sample value-blank value) * water yield/surface area of sample (granule number/unit surface).
Volatile gases test (SHS) step:
1. prepare the quantitative specimen of wanting, weigh.
2. sample is put into the sample preparation chamber of gas chromatograph.
3. set the test procedure of gas chromatograph, comprise temperature and time.
4. enter the test procedure of gas chromatograph, carry out the qualitative and quantitative analysis of the volatile gases collected from the sample chamber.
5. result=quantitative values/example weight (μ g/g).
Embodiment 2
Plastic basis material PC 95g, nanometer carbon black 4g, titanate coupling agent LD125 0.3g, dispersion agent LD404 0.2g, antioxidant four [methyl-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.5g.
Above-mentioned materials by the common double screw pelletizer, with nano-scale carbon tube/nano grade carbon black and plastic basis material and auxiliary agent mixing granulation, is produced the ultra-clean antistatic material through compounding.The particulate material that utilizes this embodiment is through injection molding preparation standard model, so that make a service test.Test-results is shown in table 3 and table 4.
Embodiment 3
Plastic basis material polypropylene 66.7g, carbon nano fiber 28g, silane coupling agent 0.5g, dispersion agent LD404 4g, antioxidant four [methyl-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.8g.
Above-mentioned materials by the common double screw pelletizer, with nano-scale carbon tube/nano grade carbon black and plastic basis material and auxiliary agent mixing granulation, is produced the ultra-clean antistatic material through compounding.The particulate material that utilizes this embodiment is through injection molding preparation standard model, so that make a service test.Test-results is shown in table 3 and table 4
The antistatic property test, the technical indicator comparing result of the material of the material of embodiment 2 and embodiment 3 sees Table 3.
Table 3
| Technical indicator | Embodiment 2 | Embodiment 3 |
| The material surface static voltage | 2 volts | 0.8 volt |
| Material surface friction voltage | 8 volts | 2.5 volt |
| The point-to-point resistance of material | 10 9～10 10Ohm | 10 7～10 8Ohm |
| Material fall time | 1.3 second | 0.1 second |
Super clean performance test, the super clean technology index comparing result of the material of the material of embodiment 2 and embodiment 3 sees Table 4.
Table 4
| Technical indicator | Embodiment 2 | Embodiment 3 |
| Liquid particle count test (LPC): granule number/cm 2 | ?2674 | ?5857 |
| Volatile gases test (SHS): μ g/g | ?0.763 | ?0.819 |
These parameters adopts the test determines identical with embodiment 1.The The above results explanation is according to composition of the present invention and utilize the product of said composition preparation to have good super clean performance and antistatic property.Be appreciated that the product that utilizes composition manufacturing provided by the invention can be used for shield electromagnetic.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a ultra-clean antistatic resin composition mainly comprises: plastic basis material 63～98%, nano-scale carbon tube and/or nano grade carbon black 1～30%, coupling agent 0.1～0.5%, dispersion agent 0.1～5%, antioxidant 0.5～1.5%.
2. ultra-clean antistatic resin composition according to claim 1, wherein said plastic basis material are selected from the group of being made up of polyetherimide (PEI), polycarbonate (PC), polyphenylene oxide (PPO) and polyoxymethylene (POM), polyolefine, polyvinyl chloride, polyvinylidene chloride, ABS resin, polystyrene, acrylonitrile styrene resin (AS), (methyl) acrylic resin, polyvinyl alcohol, polyamide resin, polyacetal resin, polycarbonate resin, vibrin, tetrafluoroethylene, fluoro-resin, poly-imines, polyimide.
3. ultra-clean antistatic resin composition according to claim 1, wherein said coupling agent are selected from organic chromium complex compound, silane coupling agent, titante coupling agent and zirconium class coupling agent.
4. ultra-clean antistatic resin composition according to claim 1, wherein said dispersion agent are selected from paraffin oil, polyethylene wax, oxidized polyethlene wax, fatty acid soaps class, fatty acid ester, fatty acyl amide and ester class.
5. ultra-clean antistatic resin composition according to claim 1, wherein said antioxidant is selected from organophosphite and hindered phenol.
6. the preparation method of a ultra-clean antistatic resin material may further comprise the steps:
1) mixes following component: plastic basis material 63～98%, CNT (carbon nano-tube)/carbon black 1～30%, coupling agent 0.1～0.5%, dispersion agent 0.1～5%, antioxidant 0.5～1.5%;
2) utilize dual-screw pelletizer with the mixture pelleting that obtains in the previous step, obtain the ultra-clean antistatic resin material.
7. ultra-clean antistatic product that is used for semiconductor applications, it is by forming according to each described ultra-clean antistatic resin composition among the claim 1-5.
8. product according to claim 7, wherein said product are the pallet that is used for splendid attire and transmission electronic element.
9. according to each described ultra-clean antistatic resin composition application in shield electromagnetic among the claim 1-5.
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2007
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