CN102277128A - Conductive silicone rubber adhesive moulded on-site at room temperature and application method - Google Patents
Conductive silicone rubber adhesive moulded on-site at room temperature and application method Download PDFInfo
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Abstract
The invention provides a conductive silicone rubber adhesive moulded on-site at room temperature. The adhesive comprises component A and component B. The component A includes by weight: 400-1000 parts of metal base conductive filling material, 20-80 parts of vinyl terminiated polysiloxane, 20-80 parts of vinyl silicone resin, 0.01-1 part of Karstedt catalyst. The component B includes by weight: 400-1000 parts of metal base conductive filling material, 20-80 parts of vinyl terminiated polysiloxane, 20-80 parts of vinyl silicone resin, 10-35 parts of hydrogen containing silicone oil, and 0.01-1 part of inhibitor. The adhesive of the invention has the characteristics of high conductivity and low operation condition, and the conducting layer formed has the advantages of reliable adhesiveness, long service life, good sealing, vibration resistance and resistance to impacts of high and low temperatures. The invention also provides an application method of the above conductive silicone rubber adhesive moulded on-site at room temperature. The adhesive comprises component A and component B. In application, the component A and component B are fully mixed in a ratio of 1:1 at room temperature. With the method of the invention, the adhesive is convenient for use and can mould on-site and solidify at room temperature without being affected by the thickness of an adhesive layer.
Description
Technical field
The invention belongs to chemical material technical field, but specifically a kind of room temperature deep layer is solidified in-situ forming high-conductivity silicon rubber tackiness agent and preparation method thereof.
Background technology
Conductive silicon rubber is the very important conducing composite material of a class.It had both had the characteristic that can realize conductive adhesion after common conductive resin solidifies, and also had the silicon rubber good springiness, and the stopping property height is anti-aging, the characteristic that the life-span is long.Therefore at the electromagnetic shielding of various electronicss, anti-interference, aspects such as radioprotective have purposes widely.By the method for the conductive silicon rubber bar being installed or smearing the conductive silicon rubber tackiness agent, can effectively reduce electromagnetic radiation and the interference of minimizing external electromagnetic radiation that electronics externally produces to electronics at the shell seam crossing of electronics.Wherein can be divided into carbon black or graphite and be the low conductive silicon rubber (volume specific resistance〉10 ohmcms) of filler and be the high-conductivity silicon rubber (volume specific resistance＜0.1 ohmcm) of filler with metal-powder or metallizing powder according to its conductive capability.
Traditional high conductive resin rubber generally is the silicon rubber bar of making conduction in advance, then this conductive silicon rubber bar process screw location or fluting is installed in the position that needs electromagnetic sealing, is close to press to make that sealing is conducted electricity between two portions.A kind of conductive silicon rubber composition is disclosed such as Chinese patent: CN1605604, adopt the mode of mixing two-component silicone rubber and silver-plated conductive particle filler, technology (100 ~ 250 degrees centigrade of thermal treatment temps) by hot briquetting obtains the high-conductivity silicon rubber bar.Chinese patent: CN1649963 adopts metal matrix conductive filler material and spherical silicone rubber particles as the weighting material of addition-type silicon rubber, vulcanizes high-conductivity silicon rubber sheet or the India-rubber strip that has obtained soft and low permanent compression set under 150 degrees centigrade of conditions of two hours.
Adopt the electron device of traditional conductive silicon rubber bar sealing, need the accurate conductive rubber sealing-ring of customization size in advance and press fixing the use.To such an extent as to when the surface shape complexity of needs sealings or material is soft when can't pressurize, just be difficult to use.Therefore the new technology of in-place forming is suggested.A kind of heat curing in-situ forming high-conductivity silicon rubber composition is disclosed as Chinese patent: CN101624471.Said composition is mixed and is formed by vinyl polysiloxane, containing hydrogen silicone oil, metal matrix conductive filler material, catalyst made from platonic, functional stuffing.Take out from container during use, be coated in the joint face place that needs connection, under 150 celsius temperatures, be solidified into the target high-conductivity silicon rubber composition.But the high-conductivity silicon rubber that this patent is introduced needs at high temperature to solidify, and bonded parts are had higher requirement, is difficult to use in some occasions that can not heat.
Many times, the environment of in-place forming does not allow to be heating and curing, and can only adopt the mode of self-vulcanizing.Chinese patent CN1775862 discloses a kind of single-component room-temperature curable nigh conductive silicon rubber composition.Said composition is formed by absorbing the mixing of water in air steam solidified condensed type room curing silicon rubber (RTV-1) and metal matrix conductive filler material and functional stuffing.From the sealed vessel of isolated moisture, take out during use, be coated in the joint face place that needs connection, be solidified into the target conductive silicon rubber composition by being exposed to from airborne moisture.But this conductive silicon rubber is solidified by absorbing water in air gas, therefore has the common drawback of all RTV-1 silicon rubber, is exactly deep layer to solidify.When bondline thickness surpasses 3mm, inside will be solidified slowly even can not be solidified.But therefore develop a kind of room temperature deep layer curing in-situ forming high-conductivity silicon rubber and become a kind of urgent demand.
Reference:
CN 101260238 conductive silicon rubbers
CN 1605604 high electroconductive rubbers and manufacture method thereof
CN 1649963 conductive silicon rubber compositions
CN 1775862 single-component room-temperature curable nigh conductive silicon rubber compositions
101,624,471 1 kinds of heat curing in-situ forming high-conductivity silicon rubber compositions of CN and application thereof
Summary of the invention
The objective of the invention is in order to overcome the deficiencies in the prior art, but a kind of room temperature deep layer cure silicone rubber of design is a matrix, solidifies the in-situ forming high-conductivity silicon rubber tackiness agent but the metal matrix conductive powder is the room temperature deep layer of filler.
For this reason, the present invention is by the following technical solutions: this tackiness agent comprises component A and B component, and described component A comprises: the metal matrix conductive filler material of 400 ~ 1000 weight parts, the ethenyl blocking polysiloxane of 20 ~ 80 weight parts, the vinyl polysiloxane of 20 ~ 80 weight parts, 0.01 ~ 1 weight part
KarstedtCatalyzer; Described B component comprises: 400 ~ 1000 parts metal matrix conductive filler material, the ethenyl blocking polysiloxane of 20 ~ 80 weight parts, the vinyl polysiloxane of 20 ~ 80 weight parts, the containing hydrogen silicone oil of 10 ~ 35 weight parts, the inhibitor of 0.01 ~ 1 weight part.
The present invention can also adopt following further technical scheme: described metal matrix conductive filler material is the metallic particles of diameter at 100nm ~ 5000nm, described metallic particles is shaped as flakey or spherical, described metallic particles is silver powder or silver plated glass powder or silver plated copper powder, and copper powder, nickel powder.
Described ethenyl blocking polysiloxane, its contents of ethylene are 0.2% ~ 1%, and viscosity is 1000 ~ 10000cp.
The contents of ethylene of described vinyl polysiloxane is 1% ~ 4%, and viscosity is 1000 ~ 10000cp.
The reactive hydrogen content of described containing hydrogen silicone oil is 0.3%-1.5%, and viscosity is 50-250cp.
Described Karstedt catalyzer is the tetramethyl divinyl disiloxane solution of platinum containing amount 5000 ppm.
Described inhibitor comprises multi-vinyl silicone oil.
Described component A also comprises viscosity increaser, and described viscosity increaser is the triethoxyl silane that contains vinyl.
By above technical scheme, the present invention compares with the technology of existing conductive silicon rubber, has the electroconductibility height, the characteristics that operational condition is low, and the conductive layer bonding of formation is reliable, life-span length, good airproof performance, vibration resistance, high-low temperature resistant impact.Adopt the present invention can significantly improve the range of application of conductive silicon rubber, save material, simplify technology, shorten man-hour, reduce cost, have great using value.
The present invention also provides the using method of above-mentioned room temperature in-place forming conductive silicon rubber tackiness agent, and described tackiness agent comprises component A and component B, during use, with component A and component B at room temperature according to the ratio thorough mixing of 1:1.
By above using method, the present invention is easy to use, and the energy in-place forming solidifies under the room temperature, not influenced by bondline thickness, can deep layer solidify.
Embodiment
This tackiness agent comprises component A and B component, and described component A comprises: the metal matrix conductive filler material of 400 ~ 1000 weight parts, the ethenyl blocking polysiloxane of 20 ~ 80 weight parts, the vinyl polysiloxane of 20 ~ 80 weight parts, 0.01 ~ 1 weight part
KarstedtCatalyzer; Described B component comprises: 400 ~ 1000 parts metal matrix conductive filler material, the ethenyl blocking polysiloxane of 20 ~ 80 weight parts, the vinyl polysiloxane of 20 ~ 80 weight parts, the containing hydrogen silicone oil of 10 ~ 35 weight parts, the inhibitor of 0.01 ~ 1 weight part.
Described metal matrix conductive filler material is the metallic particles of diameter at 100nm ~ 5000nm, and described metallic particles is shaped as flakey or spherical, and described metallic particles is silver powder or silver plated glass powder or silver plated copper powder, and copper powder, nickel powder.
Described ethenyl blocking polysiloxane, its contents of ethylene are 0.2% ~ 1%, and viscosity is 1000 ~ 10000cp.
The contents of ethylene of described vinyl polysiloxane is 1% ~ 4%, and viscosity is 1000 ~ 10000cp.
The reactive hydrogen content of described containing hydrogen silicone oil is 0.3%-1.5%, and viscosity is 50-250cp.
Described Karstedt catalyzer is the tetramethyl divinyl disiloxane solution of platinum containing amount 5000 ppm.
Described inhibitor comprises multi-vinyl silicone oil.
Described component A also comprises viscosity increaser, and described viscosity increaser is the triethoxyl silane that contains vinyl.
The present invention also provides the using method of above-mentioned room temperature in-place forming conductive silicon rubber tackiness agent, and described tackiness agent comprises component A and component B, during use, with component A and component B at room temperature according to the ratio thorough mixing of 1:1.
Specifically, component A, component B are existed in respectively in the container of sealing, at room temperature long-term storage.During use, with component A, the component B ratio thorough mixing according to weight or volume ratio 1:1, being coated in needs on the conduction agglutinating joint face, and self-vulcanizing promptly formed the conductive silicon rubber elastomerics in 24 ~ 48 hours.Be used for matrix metal, semi-conductor, ITO conductive glass etc., form the integral body of conductive seal.To realizing the electromagnetic shielding sealing of electronic machine complex surface under the room temperature, has very significant effect.
Example 1:
Component A makes: in dry, clean container, the following component of uniform mixing: 1000 weight part diameters are the flakey silver powder of 1000nn, 80 weight part viscosity are the mixture of 0.3% ethenyl blocking polysiloxane for the 3000cp contents of ethylene, 20 weight part viscosity are 1% vinyl polysiloxane for the 6000cp contents of ethylene, the Karstedt catalyzer of 1 weight part, the triethoxyl silane viscosity increaser that contains vinyl of 5 weight parts.Obtain the thick liquid that viscosity is 10000cp ~ 20000cp after having mixed, be kept in the container of sealing.
Component B makes: in dry, clean container, the following component of uniform mixing: 900 weight part diameters are the flakey silver powder of 1000nn, 80 weight part viscosity are the mixture of 0.3% ethenyl blocking polysiloxane for the 3000cp contents of ethylene, 20 weight part viscosity are 1% vinyl polysiloxane for the 6000cp contents of ethylene, 20 weight part viscosity are that 120cp reactive hydrogen content is 0.3% containing hydrogen silicone oil, the multi-vinyl silicone oil inhibitor of 1 weight part.Obtain the thick liquid that viscosity is 10000cp ~ 20000cp after having mixed, be kept in the container of sealing.
During use,, be coated on the face that needs the conduction connection, at room temperature solidified 24 hours A, component B ratio thorough mixing according to weight or volume ratio 1:1.Obtaining hardness is Shao Shi A55, and extensibility 60%, electric conductivity do not ftracture to the variation of 100 degree celsius temperature at-20 degrees centigrade less than the conductive silicon rubber of 0.01 ohmcm, remain good electrical conductivity and stopping property.
The Karstedt catalyzer refers to a kind of silicon rubber catalyzer of naming according to the name of contriver Karstedt among the present invention, and composition is the reaction product of Platinic chloride and tetramethyl divinyl disiloxane.
Example 2:
Component A makes: in dry, clean container, the following component of uniform mixing: 400 weight part diameters are the spherical silver-plated copper powder of 100nn, 20 weight part viscosity are the mixture of 1% ethenyl blocking polysiloxane for the 1000cp contents of ethylene, 80 weight part viscosity are 4% vinyl polysiloxane for the 10000cp contents of ethylene, 0.1 the Karstedt catalyzer of weight part, the triethoxyl silane viscosity increaser that contains vinyl of 0.1 weight part.Obtain the thick liquid that viscosity is 15000cp ~ 25000cp after having mixed, be kept in the container of sealing.
Component B makes: in dry, clean container, the following component of uniform mixing: 400 weight part diameters are the spherical silver-plated copper powder of 100nn, 20 weight part viscosity are the mixture of 1% ethenyl blocking polysiloxane for the 1000cp contents of ethylene, 80 weight part viscosity are 4% vinyl polysiloxane for the 10000cp contents of ethylene, 35 weight part viscosity are that 50cp reactive hydrogen content is 0.8% containing hydrogen silicone oil, the multi-vinyl silicone oil inhibitor of 0.1 weight part.Obtain the thick liquid that viscosity is 15000cp ~ 25000cp after having mixed, be kept in the container of sealing.
During use,, be coated on the face that needs the conduction connection, at room temperature solidified 48 hours A, component B ratio thorough mixing according to weight or volume ratio 1:1.Obtaining hardness is Shao Shi A70, extensibility 40%, and electric conductivity is less than the conductive silicon rubber of 0.01 ohmcm.Do not ftracture to the variation of 100 degree celsius temperature at-20 degrees centigrade, remain good electrical conductivity and stopping property.
Example 3:
Component A makes: in dry, clean container, the following component of uniform mixing: 700 weight part diameters are the spherical silvered glass powder of 5000nn, 30 weight part viscosity are the mixture of 0.2% ethenyl blocking polysiloxane for the 10000cp contents of ethylene, 50 weight part viscosity are 2% vinyl polysiloxane for the 1000cp contents of ethylene, 0.01 the Karstedt catalyzer of weight part, the triethoxyl silane viscosity increaser that contains vinyl of 2 weight parts.Obtain the thick liquid that viscosity is 8000cp ~ 15000cp after having mixed, be kept in the container of sealing.
Component B makes: in dry, clean container, the following component of uniform mixing: 700 weight part diameters are the spherical silvered glass powder of 5000nn, 30 weight part viscosity are the mixture of 0.2% ethenyl blocking polysiloxane for the 10000cp contents of ethylene, 50 weight part viscosity are 2% vinyl polysiloxane for the 1000cp contents of ethylene, 10 weight part viscosity are that 250cp reactive hydrogen content is 1.5% containing hydrogen silicone oil, the multi-vinyl silicone oil inhibitor of 0.01 weight part.Obtain the thick liquid that viscosity is 8000cp ~ 15000cp after having mixed, be kept in the container of sealing.
During use,, be coated on the face that needs the conduction connection, at room temperature solidified 48 hours A, component B ratio thorough mixing according to weight or volume ratio 1:1.Obtaining hardness is Shao Shi A60, extensibility 100%, and electric conductivity is less than the conductive silicon rubber of 0.01 ohmcm.Do not ftracture to the variation of 100 degree celsius temperature at-20 degrees centigrade, remain good electrical conductivity and stopping property.
Example 4:
Component A makes: in dry, clean container, the following component of uniform mixing: 800 weight part diameters are the spherical copper powder of 2000nn, 50 weight part viscosity are the mixture of 0.25% ethenyl blocking polysiloxane for the 7000cp contents of ethylene, 30 weight part viscosity are 3% vinyl polysiloxane for the 3000cp contents of ethylene, 0.5 the Karstedt catalyzer of weight part, the triethoxyl silane viscosity increaser that contains vinyl of 1 weight part.Obtain the thick liquid that viscosity is 10000cp ~ 16000cp after having mixed, be kept in the container of sealing.
Component B makes: in dry, clean container, the following component of uniform mixing: 800 weight part diameters are the spherical copper powder of 2000nn, 50 weight part viscosity are the mixture of 0.25% ethenyl blocking polysiloxane for the 7000cp contents of ethylene, 30 weight part viscosity are 3% vinyl polysiloxane for the 3000cp contents of ethylene, 20 weight part viscosity are that 200cp reactive hydrogen content is 0.8% containing hydrogen silicone oil, the multi-vinyl silicone oil inhibitor of 0.5 weight part.Obtain the thick liquid that viscosity is 10000cp ~ 16000cp after having mixed, be kept in the container of sealing.
During use,, be coated on the face that needs the conduction connection, at room temperature solidified 48 hours A, component B ratio thorough mixing according to weight or volume ratio 1:1.Obtaining hardness is Shao Shi A65, extensibility 80%, and electric conductivity is less than the conductive silicon rubber of 0.05 ohmcm.Do not ftracture to the variation of 100 degree celsius temperature at-20 degrees centigrade, remain good electrical conductivity and stopping property.
Example 5:
Component A makes: in dry, clean container, the following component of uniform mixing: 900 weight part diameters are the flakey nickel powder of 800nn, 60 weight part viscosity are the mixture of 0.4% ethenyl blocking polysiloxane for the 5000cp contents of ethylene, 40 weight part viscosity are 2% vinyl polysiloxane for the 5000cp contents of ethylene, the Karstedt catalyzer of 1 weight part, the triethoxyl silane viscosity increaser that contains vinyl of 3 weight parts.Obtain the thick liquid that viscosity is 12000cp ~ 22000cp after having mixed, be kept in the container of sealing.
Component B makes: in dry, clean container, the following component of uniform mixing: 900 weight part diameters are the flakey nickel powder of 800nn, 60 weight part viscosity are the mixture of 0.4% ethenyl blocking polysiloxane for the 5000cp contents of ethylene, 40 weight part viscosity are 2% vinyl polysiloxane for the 5000cp contents of ethylene, 25 weight part viscosity are that 100cp reactive hydrogen content is 0.5% containing hydrogen silicone oil, the multi-vinyl silicone oil inhibitor of 1 weight part.Obtain the thick liquid that viscosity is 12000cp ~ 22000cp after having mixed, be kept in the container of sealing.
During use,, be coated on the face that needs the conduction connection, at room temperature solidified 24 hours A, component B ratio thorough mixing according to weight or volume ratio 1:1.Obtaining hardness is Shao Shi A60, extensibility 70%, and electric conductivity is less than the conductive silicon rubber of 0.05 ohmcm.Do not ftracture to the variation of 100 degree celsius temperature at-20 degrees centigrade, remain good electrical conductivity and stopping property.
The high-conductivity silicon rubber tackiness agent of the present invention preparation can at room temperature solidify to form the elastomeric material of good conductivity, is not subjected to humidity, the influence of thickness simultaneously.The electroconductibility height, cohesive force is strong, and long service life can be widely used in the various occasions that need electromagnetic shielding to be connected with conduction.
Claims (9)
1. room temperature in-place forming conductive silicon rubber tackiness agent, it is characterized in that: this tackiness agent comprises component A and B component, described component A comprises: the metal matrix conductive filler material of 400 ~ 1000 weight parts, the ethenyl blocking polysiloxane of 20 ~ 80 weight parts, the vinyl polysiloxane of 20 ~ 80 weight parts, 0.01 ~ 1 weight part
KarstedtCatalyzer; Described B component comprises: 400 ~ 1000 parts metal matrix conductive filler material, the ethenyl blocking polysiloxane of 20 ~ 80 weight parts, the vinyl polysiloxane of 20 ~ 80 weight parts, the containing hydrogen silicone oil of 10 ~ 35 weight parts, the inhibitor of 0.01 ~ 1 weight part.
2. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: described metal matrix conductive filler material is the metallic particles of diameter at 100nm ~ 5000nm, described metallic particles is shaped as flakey or spherical, described metallic particles is silver powder or silver plated glass powder or silver plated copper powder, and copper powder, nickel powder.
3. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: described ethenyl blocking polysiloxane, its contents of ethylene are 0.2% ~ 1%, viscosity is 1000 ~ 10000cp.
4. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: the contents of ethylene of described vinyl polysiloxane is 1% ~ 4%, viscosity is 1000 ~ 10000cp.
5. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: the reactive hydrogen content of described containing hydrogen silicone oil is 0.3%-1.5%, viscosity is 50-250cp.
6. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: described Karstedt catalyzer is the tetramethyl divinyl disiloxane solution of platinum containing amount 5000 ppm.
7. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: described inhibitor comprises multi-vinyl silicone oil.
8. a kind of room temperature in-place forming conductive silicon rubber tackiness agent according to claim 1, it is characterized in that: described component A also comprises viscosity increaser, described viscosity increaser is the triethoxyl silane that contains vinyl.
9. the using method of the described a kind of room temperature in-place forming conductive silicon rubber tackiness agent of claim 1 is characterized in that described tackiness agent comprises component A and B component, during use, with component A and B component at room temperature according to the ratio thorough mixing of 1:1.
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| JP2016519174A (en) * | 2013-03-14 | 2016-06-30 | ダウ コーニング コーポレーションＤｏｗ Ｃｏｒｎｉｎｇ Ｃｏｒｐｏｒａｔｉｏｎ | Curable silicone composition, conductive silicone adhesive, method for producing and using the same, and electrical device containing the same |
| CN105950105A (en) * | 2016-06-30 | 2016-09-21 | 杭州福斯特光伏材料股份有限公司 | Thixotrope for packaging LED (light emitting diode ) chip |
| WO2017114440A1 (en) | 2015-12-31 | 2017-07-06 | Bluestar Silicones Shanghai Co., Ltd. | Electrically-conductive curable organosilicon rubber |
| CN107325748A (en) * | 2017-06-02 | 2017-11-07 | 中国航发北京航空材料研究院 | It is capable of bi-component electrically conductive organosilicon sealant of doped graphene and preparation method thereof |
| CN109575610A (en) * | 2018-12-20 | 2019-04-05 | 海昌隐形眼镜有限公司 | Surface silicon hydrogen functionalized silicon rubber material and preparation, hydrophilic treated and methods for using them |
| CN109852336A (en) * | 2018-12-10 | 2019-06-07 | 上海卫星装备研究所 | The conductive adhesive and its application method pasted suitable for glass mould second surface mirror |
| CN110845851A (en) * | 2019-11-22 | 2020-02-28 | 新安天玉有机硅有限公司 | Liquid conductive adhesive for power cable accessories and preparation method thereof |
| CN115433541A (en) * | 2022-09-30 | 2022-12-06 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016519174A (en) * | 2013-03-14 | 2016-06-30 | ダウ コーニング コーポレーションＤｏｗ Ｃｏｒｎｉｎｇ Ｃｏｒｐｏｒａｔｉｏｎ | Curable silicone composition, conductive silicone adhesive, method for producing and using the same, and electrical device containing the same |
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| CN105950105A (en) * | 2016-06-30 | 2016-09-21 | 杭州福斯特光伏材料股份有限公司 | Thixotrope for packaging LED (light emitting diode ) chip |
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| CN109852336A (en) * | 2018-12-10 | 2019-06-07 | 上海卫星装备研究所 | The conductive adhesive and its application method pasted suitable for glass mould second surface mirror |
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| CN110845851A (en) * | 2019-11-22 | 2020-02-28 | 新安天玉有机硅有限公司 | Liquid conductive adhesive for power cable accessories and preparation method thereof |
| CN110845851B (en) * | 2019-11-22 | 2022-02-11 | 新安天玉有机硅有限公司 | Liquid conductive adhesive for power cable accessories and preparation method thereof |
| CN115433541A (en) * | 2022-09-30 | 2022-12-06 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
| CN115433541B (en) * | 2022-09-30 | 2023-11-07 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
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Application publication date: 20111214 |