CN104592926A - Adhesive and preparation method thereof - Google Patents
Adhesive and preparation method thereof Download PDFInfo
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- CN104592926A CN104592926A CN201510017212.5A CN201510017212A CN104592926A CN 104592926 A CN104592926 A CN 104592926A CN 201510017212 A CN201510017212 A CN 201510017212A CN 104592926 A CN104592926 A CN 104592926A
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Abstract
The invention provides an adhesive which comprises the following components in parts by weight: 100 parts of matrix resin, 5-350 parts of high-dielectric-constant filler, 0.01-5 parts of dispersing agent, 0.1-5 parts of coupling agent and 8-25 parts of toner. The adhesive has the characteristics of high relative dielectric constant (greater than 6), favorable light proofness, adjustable color, high bonding power and the like, and can be used for bonding in capacitive fingerprint identification chip module packaging; and the packaged capacitive fingerprint identification chip module can transmit capacitance signals without shielding or reflecting the capacitance signals. The electronic packaging adhesive provided by the invention is easy to assemble; the assembly mode can be adhesive dotting, scratch coating, roller coating or screen printing, and the bonding is performed by automatic curing; and thus, the adhesive is especially suitable for mass production. The invention also provides a preparation method of the adhesive, which simplifies the packaging technique.
Description
Technical field
The present invention relates to a kind of caking agent and preparation method thereof, particularly relate to a kind of caking agent with high-k and preparation method thereof.
Background technology
In recent years, along with the development of Electronic Encapsulating Technology, the caking agent used for electronic packaging with property is more and more subject to people's attention, such as, play the conductive glue of electric action, heat conduction glue having also had conductive force etc.And in some application scenario, need to use the special electronics packaging plastic water (or being called Electronic Packaging caking agent) with high relative dielectric constant, such as in the encapsulation process of semicoductor capacitor formula signals collecting chip, bonding packaging plastic glassware for drinking water is needed to have high dielectric characteristics, to prevent capacitance signal conductively-closed or to be reflected, affect signals collecting precision.And traditional Electronic Packaging caking agent relative permittivity general lower (being generally less than 6), thus need to develop the Electronic Packaging glue with high relative dielectric properties.Simultaneously; such chip needs to use the dielectric materials of hard as protective layer; such as sapphire, glass, pottery etc.; in use all there is printing opacity problem in various degree in these materials; for solving printing opacity problem; traditional way is, to material back side silk-screen light shield layers in advance such as sapphire, glass, potteries, to prevent printing opacity.The specific inductivity of this silk-screen layer itself is lower, can have certain detrimentally affect to capacitance signal transmission.In capacitance type fingerprint identification chip module, for preventing capacitance signal conductively-closed or being reflected, encapsulation glue used needs higher relative permittivity, general requirement relative permittivity ε r >=6, and guarantee capacitance signal can be transferred on chip smoothly.And the specific inductivity of most of organic resin is very low, in apple patent US8618910B2, mention a kind of polymkeric substance, poly(vinylidene fluoride) (PVDF), its relative permittivity is approximately about 7, but it is poor to the adhesive power of pottery, be difficult to use as ceramic bonding agent; The relative permittivity of general caking agent organic resin used is lower, is generally about 2 ~ 4, and such as the caking agent of 3M house journal CN200880114990.4, obviously can not meet the requirement of relative permittivity ε r >=6.Although partial monopoly refer to add inorganic powder to improve the method for relative permittivity, often can not use as caking agent; Although Sumitomo patent CN200410071084.4 refer to a kind of method of high dielectric resin composition, the resin combination obtained can not be applied in bonding glue.The caking agent that prior art makes all is difficult to obtain corresponding high relative dielectric properties, and its major cause is, organic resin is because himself structure is difficult to polarized, and its specific inductivity is difficult to improve.Then there is the easy agglomeration of powder in the method for usually adding powder in organism, can cause severe jamming to Signal transmissions.
Summary of the invention
The object of the invention is to overcome weak point that prior art exists and provide a kind of caking agent, caking agent provided by the invention solves the problem that Electronic Packaging caking agent relative permittivity is on the low side in the past, and maintain the characteristic of Electronic Packaging caking agent high adhesive force, its adhering object can be sapphire, glass, pottery, plastic cement, silicon etc., present invention also offers the preparation method of described caking agent, described preparation method is by having carried out disperse modified process to the ceramic powder added in described caking agent, the caking agent obtained also has good dispersing characteristic, its fineness can reach less than 2 μm, this caking agent also has shading and toning effect concurrently simultaneously, simplify packaging process.
For achieving the above object, the technical scheme taked: a kind of caking agent, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 5 ~ 350 parts, dispersion agent 0.01 ~ 5 part, coupling agent 0.1 ~ 5 part, toning agent 8 ~ 25 parts.The filler that the present invention adds high-k in described caking agent is the specific inductivity in order to improve caking agent, and adding toning agent in caking agent of the present invention is play toning and interception.
Preferably, described matrix resin is moisture-cure polyurethane resin performed polymer.The synthesis material of moisture-cure polyurethane resin performed polymer of the present invention can select aromatic isocyanate, such as TDI, MDI, NDI, PPDI, XDI or PAPI, also aliphatic isocyanates can be selected, such as HDI, HMDI, HTDI, HXDI, or two or more mixture of above isocyanic ester; And its synthesis material polyvalent alcohol can select polyester polyol, polyether glycol or their mixture; Have the base polyurethane prepolymer for use as of moisture cure characteristics, can not add solidifying agent, it can moisture in absorbing environmental and chain extension-crosslinking, thus plays solidification.
Preferably, described matrix resin is the moisture-cure polyurethane resin performed polymer of 2.5% ~ 15%-NCO containing massfraction.
Preferably, described dispersion agent is anionic dispersing agents or non-ionic dispersing agent, and described coupling agent is silane coupling agent or titanate coupling agent, and described toning agent is the one in carbon black, titanium dioxide and gas-phase silica.More preferably, described coupling agent be silane resin acceptor kh-550, silane coupling agent KH-560, Silane coupling reagent KH-570, titanate coupling agent TM-58 or other contain the coupling agent of the corresponding functional group of resin.Preferably, described dispersion agent is polyacrylic acid sodium salt or phosphoric acid ester; More preferably, described dispersion agent is the one in Yelkin TTS, dispersion agent KD-4, dispersion agent KD-1 and dispersion agent 9400.
Preferably, the filler of described high-k is the ceramic powder with high dielectric characteristics.
Preferably, the ceramic powder described in high dielectric characteristics is TiO
2, ZrO
2, BaTiO
3, CaTiO
3, ZnO, CaZrO
3, MgZrO
3, Ba
xsr
1-xti
yzr
1-yo
3, Ca
yba
1-yzr
xti
1-xo
3, K
xna
1-xnbO
3in at least one; Described Ba
xsr
1-xti
yzr
1-yo
3middle x is 0 ~ 1, y is 0 ~ 1; Described Ca
yba
1-yzr
xti
1-xo
3middle x is 0 ~ 1, y is 0 ~ 1; Described K
xna
1-xnbO
3middle x is 0 ~ 1, y is 0 ~ 1.
Preferably, the particle diameter of the filler of described high-k is 0.1 μm ~ 20 μm.
Preferably, described caking agent also comprises at least one in anti-sedimentation agent and thinner, and its addition is 0.6 ~ 20 part.Add anti-sedimentation agent or thinner, if desired more low viscous caking agent as required, can suitably add non-volatile inert diluent; If desired the caking agent of viscosity higher, can select polyacrylate or aerosil to make anti-sedimentation agent.
Preferably, described anti-sedimentation agent is selected from that polymeric amide is cured, one in polyacrylate and aerosil, and described thinner is non-volatility thinner.More preferably, described thinner is one or more in white oil, phthalic ester, polyisobutene and polyester plasticizer.The currently available products of described phthalic ester is as thinner DOP, thinner DBP, diluent B BP or thinner DINP etc.
The invention provides a kind of preparation method of caking agent described above, described preparation method comprises the following steps:
(1a) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2a), after adding matrix resin and toning agent in the filler of the high-k after step (1a) process, redispersion is carried out to it, stirs, obtain described caking agent;
Or described preparation method comprises the following steps:
(1b) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring;
(2b) proceed to sand mill or milling train carries out redispersion after dispersion, obtain described caking agent.
Preferably, vacuum condition described above is the condition of vacuum without moisture.
The invention provides a kind of preparation method of caking agent described above, described preparation method comprises the following steps:
(1c) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2c), after adding matrix resin, thinner and toning agent in the filler of the high-k after step (1c) process, redispersion is carried out to it;
(3c) then add anti-sedimentation agent, stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1d) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, thinner, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring,
(2d) proceed to sand mill or milling train carries out redispersion after dispersion, add anti-sedimentation agent after discharging and stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1e) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2e), after adding matrix resin, thinner and toning agent in the filler of the high-k after step (1e) process, redispersion is carried out to it, stirs, obtain described caking agent;
Or described preparation method comprises the following steps:
(1f) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring;
(2f) proceed to sand mill or milling train carries out redispersion after dispersion, add anti-sedimentation agent after discharging and stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1g) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2g), after adding matrix resin, toning agent in the filler of the high-k after step (1g) process, redispersion is carried out to it;
(3g) then add anti-sedimentation agent, stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1h) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, thinner, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring,
(2h) proceed to sand mill or milling train carries out redispersion after dispersion, obtain described caking agent.
Preferably, vacuum condition described above is the condition of vacuum without moisture.
Preferably, described in described step (1a), (1c), (1e) and (1g), surface modification treatment mode is the one in ball milling, planetary mills, sand milling and planet stirring, and described in described step (2a), (2c), (2e) and (2g), dispersing mode is the one in ball milling, sand milling, planet stirring and milling train.
The assembling mode of caking agent of the present invention can be a glue formula, and can be also blade coating, roller coat or silk screen printing etc., then described caking agent can solidify voluntarily, when air is drier, can use humidifier humidifies.
Caking agent of the present invention needs sealing to preserve, and does not contact with air as far as possible, prevents solidification.
Beneficial effect of the present invention is: the caking agent used for electronic packaging that the invention provides a kind of high relative dielectric constant, it is high that this caking agent has relative permittivity simultaneously, under the test frequency of 1KHz ~ 10MHz, its relative permittivity is more than 6, the features such as opacifying property is good, Color tunable, bonding force are strong, can be used for the bonding of capacitance type fingerprint identification chip module packaging, can capacitance signal be transmitted and capacitance signal conductively-closed can not be caused or reflected after encapsulation.Caking agent used for electronic packaging provided by the invention is except having high relative dielectric constant, have shaded effect concurrently simultaneously, the silk-screen light shield layer to materials such as sapphire, glass, potteries can be cancelled, be conducive to simplifying assembly process, improve effectiveness, reduce production cost simultaneously.Electronic Packaging caking agent provided by the invention also has the advantages such as assembling is easy, and its assembling mode can be a glue formula, also can be blade coating, roller coat or silk screen printing etc., then bonding by automatic curing mode, is particularly suitable for mass production.Present invention also offers the preparation method of a kind of high relative dielectric constant caking agent used for electronic packaging, the method is by adding the inorganic ceramic powder of high-k, and disperse modified process has been carried out to ceramic powder, improve the consistency of ceramic powder, can be dispersed in organic bonding resin, do not affect solidification and the adhesion properties of resin, and interference can not be caused to Signal transmissions, simultaneously by adding the process of the mode such as toning agent and opalizer, make it also have shading and toning effect, simplify packaging process.
Embodiment
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 350 parts, dispersion agent 5 parts, coupling agent 5 parts, toning agent 15 parts; Described caking agent also comprises anti-sedimentation agent and thinner, and its addition is 9.9 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 2.5% containing massfraction), described thinner is thinner DOP, described dispersion agent is Yelkin TTS, described coupling agent is Silane coupling agent KH550, the filler of described high-k is potassium-sodium niobate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 350 weight parts, 5 weight parts and the coupling agent of 5 weight parts are added ball milling 6h in ball mill, add the matrix resin of 100 weight parts, the thinner of 9 weight parts, the toning agent of 15 weight parts, continue ball milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 0.9 weight part, dispersed with stirring is good, obtains described caking agent.
Embodiment 2
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 350 parts, dispersion agent 5 parts, coupling agent 5 parts, toning agent 15 parts; Described caking agent also comprises anti-sedimentation agent and thinner, and its addition is 8 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 2.5% containing massfraction), described thinner is thinner DOP, described dispersion agent is Yelkin TTS, described coupling agent is Silane coupling agent KH550, the filler of described high-k is sodium columbate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under the condition of vacuum without moisture, the thinner of the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 5 weight parts, 5 weight parts, 7 weight parts, the filler of the high-k of 350 weight parts, the toning agent of 15 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, after proceed in homogenizer, the anti-sedimentation agent adding 1 weight part stirs 15min, obtains described caking agent.
Embodiment 3
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 140 parts, dispersion agent 1.5 parts, coupling agent 1.2 parts, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent and thinner, and its addition is 11 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 3% containing massfraction), described thinner is thinner DOP, described dispersion agent is dispersion agent 9400, described coupling agent is silane resin acceptor kh-550, the filler of described high-k is barium titanate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 140 weight parts, 1.5 weight parts and the coupling agent of 1.2 weight parts are added planetary mills 6h in planet mill, add the matrix resin of 100 weight parts, the thinner of 10 weight parts, the toning agent of 10 weight parts, continue planetary mills 2h, discharging is in stirrer, add the anti-sedimentation agent of 1 weight part, dispersed with stirring is good, obtains described caking agent.
Embodiment 4
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 80 parts, dispersion agent 1.5 parts, coupling agent 1.2 parts, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent and thinner, and its addition is 11 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 3% containing massfraction), described thinner is thinner DOP, described dispersion agent is dispersion agent 9400, described coupling agent is silane resin acceptor kh-550, the filler of described high-k is barium titanate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 80 weight parts, 1.5 weight parts and the coupling agent of 1.2 weight parts are added planetary mills 6h in planet mill, add the matrix resin of 100 weight parts, the thinner of 10 weight parts, the toning agent of 10 weight parts, continue planetary mills 2h, discharging is in stirrer, add the anti-sedimentation agent of 1 weight part, dispersed with stirring is good, obtains described caking agent.
Embodiment 5
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 5 parts, dispersion agent 5 parts, coupling agent 5 parts, toning agent 8 parts; Described caking agent also comprises anti-sedimentation agent, and its addition is 0.6 part.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 6% containing massfraction), and described dispersion agent is dispersion agent 9400, and described coupling agent is silane coupling agent KH-560, and the filler of described high-k is SrTiO
3, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of filler 5 weight part of the high-k of 5 weight parts and the coupling agent of 5 weight parts are added sand milling 6h in sand mill, add the toning agent of the matrix resin of 100 weight parts, 8 weight parts, continue sand milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 0.6 weight part, dispersed with stirring is good, obtains described caking agent.
Embodiment 6
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 5 parts, dispersion agent 5 parts, coupling agent 5 parts, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent, and its addition is 0.8 part.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 6% containing massfraction), and described dispersion agent is dispersion agent 9400, and described coupling agent is silane coupling agent KH-560, and the filler of described high-k is Ca
0.5ba
0.5zr
0.5ti
0.5o
3, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under the condition of vacuum without moisture, the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 5 weight parts, 5 weight parts, the filler of the high-k of 5 weight parts, the toning agent of 10 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, after proceed in homogenizer, the anti-sedimentation agent adding 0.8 weight part stirs 15min, obtains described caking agent.
Embodiment 7
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 300 parts, dispersion agent 0.01 part, coupling agent 0.1 part, toning agent 25 parts; Described caking agent also comprises anti-sedimentation agent, and its addition is 2 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 8% containing massfraction), described dispersion agent is Yelkin TTS, and described coupling agent is silane resin acceptor kh-550, and the filler of described high-k is CaTiO
3, described anti-sedimentation agent is polyacrylate, and described toning agent is titanium dioxide.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under the condition of vacuum without moisture, the dispersion agent of the filler of the high-k of 300 weight parts, 0.01 weight part and the coupling agent of 0.1 weight part are added planetary mills 6h in planet mill, add the toning agent of the matrix resin of 100 weight parts, 25 weight parts, continue planetary mills 2h, discharging is in stirrer, add the anti-sedimentation agent of 2 weight parts, dispersed with stirring is good, obtains described caking agent.
Embodiment 8
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 300 parts, dispersion agent 0.01 part, coupling agent 0.1 part, toning agent 25 parts; Described caking agent also comprises anti-sedimentation agent, and its addition is 2 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 8% containing massfraction), and described dispersion agent is Yelkin TTS, and described coupling agent is silane resin acceptor kh-550, and the filler of described high-k is Ba
0.5sr
0.5ti
0.5zr
0.5o
3, described anti-sedimentation agent is polyacrylate, and described toning agent is titanium dioxide.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 0.01 weight part, 0.1 weight part, the filler of the high-k of 300 weight parts, the toning agent of 25 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, after proceed in homogenizer, the anti-sedimentation agent adding 2 weight parts stirs 15min, obtains described caking agent.
Embodiment 9
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 50 parts, dispersion agent 0.5 part, coupling agent 1 part, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent, and its addition is 5 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 10% containing massfraction), described dispersion agent is KD-4, described coupling agent is acid esters coupling agent TM-58, the filler of described high-k is ZnO, described anti-sedimentation agent is aerosil, and described toning agent is gas-phase silica.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under the condition of vacuum without moisture, the dispersion agent of the filler of the high-k of 50 weight parts, 0.5 weight part and the coupling agent of 1 weight part are added ball milling 6h in ball mill, add the toning agent of the matrix resin of 100 weight parts, 10 weight parts, continue row ball milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 5 weight parts, dispersed with stirring is good, obtains described caking agent.
Embodiment 10
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 50 parts, dispersion agent 0.5 part, coupling agent 1 part, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent, and its addition is 5 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 10% containing massfraction), and described dispersion agent is KD-4, and described coupling agent is acid esters coupling agent TM-58, and the filler of described high-k is SrTi
0.5zr
0.5o
3, described anti-sedimentation agent is aerosil, and described toning agent is gas-phase silica.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 0.5 weight part, 1 weight part, the filler of the high-k of 50 weight parts, the toning agent of 10 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, after proceed in homogenizer, the anti-sedimentation agent adding 5 weight parts stirs 15min, obtains described caking agent.
Embodiment 11
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 100 parts, dispersion agent 1 part, coupling agent 2 parts, toning agent 8 parts.Described caking agent also comprises thinner, and its addition is 10 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 12% containing massfraction), and described dispersion agent is dispersion agent KD-1, and described coupling agent is silane resin acceptor kh-550, and the filler of described high-k is CaZrO
3, described thinner is white oil, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 100 weight parts, 1 weight part and the coupling agent of 2 weight parts are added sand milling 6h in sand mill, add the matrix resin of 100 weight parts, the thinner of 10 weight parts, the toning agent of 8 weight parts, continue sand milling 2h, obtain described caking agent.
Embodiment 12
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 100 parts, dispersion agent 1 part, coupling agent 2 parts, toning agent 8 parts.Described caking agent also comprises thinner, and its addition is 10 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 12% containing massfraction), and described dispersion agent is dispersion agent KD-1, and described coupling agent is silane resin acceptor kh-550, and the filler of described high-k is SrZrO
3, described thinner is white oil, and described toning agent is carbon black
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the thinner of the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 1 weight part, 2 weight parts, 10 weight parts, the filler of the high-k of 100 weight parts, the toning agent of 8 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, obtain described caking agent.
Embodiment 13
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 200 parts, dispersion agent 0.05 part, coupling agent 0.05 part, toning agent 25 parts; Described caking agent also comprises thinner, and its addition is 15 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 15% containing massfraction), described thinner is diluent B BP, described dispersion agent is dispersion agent 9400, and described coupling agent is Silane coupling agent KH550, and the filler of described high-k is MgZrO
3, described toning agent is titanium dioxide.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under the condition of vacuum without moisture, the dispersion agent of the filler of the high-k of 200 weight parts, 0.05 weight part and the coupling agent of 0.05 weight part are added planet stirring 6h in planetary mixer, add the matrix resin of 100 weight parts, the thinner of 15 weight parts, the toning agent of 25 weight parts, continue planet stirring 2h, obtain described caking agent.
Embodiment 14
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 200 parts, dispersion agent 0.05 part, coupling agent 0.05 part, toning agent 25 parts; Described caking agent also comprises thinner, and its addition is 15 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 15% containing massfraction), described thinner is diluent B BP, described dispersion agent is dispersion agent 9400, and described coupling agent is Silane coupling agent KH550, and the filler of described high-k is SrTiO
3, described toning agent is titanium dioxide.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the thinner of the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 0.05 weight part, 0.05 weight part, 15 weight parts, the filler of the high-k of 200 weight parts, the toning agent of 25 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, obtain described caking agent.
Embodiment 15
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 300 parts, dispersion agent 2 parts, coupling agent 4 parts, toning agent 15 parts; Described caking agent also comprises thinner, and its addition is 20 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 12% containing massfraction), described thinner is thinner DBP, described dispersion agent is Yelkin TTS, and described coupling agent is silane coupling agent KH-560, and the filler of described high-k is K
0.5na
0.5nbO
3, described toning agent is gas-phase silica.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 300 weight parts, 2 weight parts and the coupling agent of 4 weight parts are added sand milling 6h in sand mill, add the matrix resin of 100 weight parts, the thinner of 20 weight parts, the toning agent of 15 weight parts, continue sand milling 2h, obtain described caking agent.
Embodiment 16
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 300 parts, dispersion agent 2 parts, coupling agent 4 parts, toning agent 12 parts; Described caking agent also comprises thinner, and its addition is 20 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 12% containing massfraction), described thinner is thinner DBP, described dispersion agent is Yelkin TTS, and described coupling agent is Silane coupling reagent KH-570, and the filler of described high-k is K
0.5na
0.5nbO
3, described toning agent is gas-phase silica.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the thinner of the coupling agent of the dispersion agent of the matrix resin of 100 weight parts, 2 weight parts, 4 weight parts, 20 weight parts, the filler of the high-k of 300 weight parts, the toning agent of 12 weight parts are joined in planetary mixer and disperse 30min, proceed in vertical grinding machine and grind 4 times, obtain described caking agent.
Embodiment 17
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, 20 parts, solidifying agent, the filler of high-k 140 parts, dispersion agent 1.5 parts, coupling agent 1.2 parts, toning agent 10 parts; Described caking agent also comprises thinner and anti-sedimentation agent, and its addition is 11.2 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 8% containing massfraction), described thinner is polyester plasticizer PPA-1500, described dispersion agent is dispersion agent 9400, described coupling agent is silane coupling agent KH-560, the filler of described high-k is barium titanate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 140 weight parts, 1.5 weight parts and the coupling agent of 1.2 weight parts are added sand milling 6h in sand mill, add the matrix resin of 100 weight parts, the thinner of 10 weight parts, the toning agent of 10 weight parts, continue sand milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 1.2 weight parts, dispersed with stirring is good, obtains described caking agent.
Embodiment 18
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 80 parts, dispersion agent 1.5 parts, coupling agent 1.2 parts, toning agent 8 parts; Described caking agent also comprises thinner and anti-sedimentation agent, and its addition is 11.2 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 8% containing massfraction), described thinner is polyester plasticizer PPA-1500, described dispersion agent is dispersion agent 9400, described coupling agent is silane coupling agent KH-560, the filler of described high-k is barium titanate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 80 weight parts, 1.5 weight parts and the coupling agent of 1.2 weight parts are added sand milling 6h in sand mill, add the matrix resin of 100 weight parts, the thinner of 10 weight parts, the toning agent of 8 weight parts, continue sand milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 1.2 weight parts, dispersed with stirring is good, obtains described caking agent.
Embodiment 19
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 90 parts, dispersion agent 0.5 part, coupling agent 2 parts, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent and thinner, and its addition is 10 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 6% containing massfraction), described thinner is thinner DINP, described dispersion agent is Dyhard RU 100, described coupling agent is silane coupling agent KH570, the filler of described high-k is strontium-barium titanate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 90 weight parts, 0.5 weight part and the coupling agent of 2 weight parts are added ball milling 6h in sand mill, add the matrix resin of 100 weight parts, the thinner of 9 weight parts, the toning agent of 10 weight parts, continue sand milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 1 weight part, dispersed with stirring is good, obtains described caking agent.
Embodiment 20
A kind of embodiment of caking agent of the present invention, described caking agent comprises the component of following weight part:: matrix resin 100 parts, the filler of high-k 140 parts, dispersion agent 0.5 part, coupling agent 2 parts, toning agent 10 parts; Described caking agent also comprises anti-sedimentation agent and thinner, and its addition is 10 parts.
Described matrix resin is moisture-cure polyurethane resin performed polymer (being-NCO of 6% containing massfraction), described thinner is thinner DINP, described dispersion agent is Dyhard RU 100, described coupling agent is silane coupling agent KH570, the filler of described high-k is strontium-barium titanate, described anti-sedimentation agent is that polymeric amide is cured, and described toning agent is carbon black.
A kind of embodiment of the preparation method of caking agent described above, described preparation method comprises the following steps:
Under vacuum, the dispersion agent of the filler of the high-k of 140 weight parts, 0.5 weight part and the coupling agent of 2 weight parts are added ball milling 6h in sand mill, add the matrix resin of 100 weight parts, the thinner of 9 weight parts, the toning agent of 10 weight parts, continue sand milling 2h, discharging is in stirrer, add the anti-sedimentation agent of 1 weight part, dispersed with stirring is good, obtains described caking agent.
Embodiment 21
Relative permittivity measures:
The cylindrical, hollow mould made with tetrafluoroethylene, the caking agent prepared by embodiment 1-20 injects wherein, solidify at a proper temperature, take out cured article after solidification, cylindrical cured article top and bottom are polished smooth, measure cylindrical cured article thickness (each position is measured difference and is no more than 0.05mm), top and bottom are gold-plated, at frequency 1MHz, under voltage 1V condition, measure electric capacity, drawn the relative permittivity of caking agent prepared by embodiment 1-20 by formulae discovery.
Cohesive strength measures:
Cohesive strength measures required equipment: ZrO pottery Eight characters mould (contact area 15*15mm), tensilon.
Cohesive strength measuring method: the tackiness agent prepared by embodiment 1-20 is coated in the contact area on Eight characters mould, gauge control, at 1 ± 0.1mm, leaves standstill 24h after solidification, tests cohesive strength with tensilon.
The relative permittivity of caking agent prepared by embodiment 1-20 and the measurement result of cohesive strength as shown in table 1, from the test result of table 1, the relative permittivity of caking agent prepared by the present invention meets relative permittivity ε r >=6 completely, can ensure that capacitance signal can be transferred on chip smoothly, and maintain high cohesive strength.
The relative permittivity of caking agent prepared by table 1 embodiment 1-20 measures
Finally to should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (12)
1. a caking agent, is characterized in that, described caking agent comprises the component of following weight part: matrix resin 100 parts, the filler of high-k 5 ~ 350 parts, dispersion agent 0.01 ~ 5 part, coupling agent 0.1 ~ 5 part, toning agent 8 ~ 25 parts.
2. caking agent according to claim 1, is characterized in that, described matrix resin is moisture-cure polyurethane resin performed polymer.
3. caking agent according to claim 2, is characterized in that, described matrix resin is the moisture-cure polyurethane resin performed polymer of 2.5% ~ 15%-NCO containing massfraction.
4. caking agent according to claim 1, it is characterized in that, described dispersion agent is anionic dispersing agents or non-ionic dispersing agent, and described coupling agent is silane coupling agent or titanate coupling agent, and described toning agent is the one in carbon black, titanium dioxide and gas-phase silica.
5. caking agent according to claim 1, is characterized in that, the filler of described high-k is the ceramic powder with high dielectric characteristics.
6. caking agent according to claim 5, is characterized in that, described in there is high dielectric characteristics ceramic powder be TiO
2, ZrO
2, BaTiO
3, CaTiO
3, ZnO, CaZrO
3, MgZrO
3, Ba
xsr
1-xti
yzr
1-yo
3, Ca
yba
1-yzr
xti
1-xo
3, K
xna
1-xnbO
3in at least one; Described Ba
xsr
1-xti
yzr
1-yo
3middle x is 0 ~ 1, y is 0 ~ 1; Described Ca
yba
1-yzr
xti
1-xo
3middle x is 0 ~ 1, y is 0 ~ 1; Described K
xna
1-xnbO
3middle x is 0 ~ 1, y is 0 ~ 1.
7. caking agent according to claim 5, is characterized in that, the particle diameter of the filler of described high-k is 0.1 μm ~ 20 μm.
8. caking agent according to claim 1, is characterized in that, described caking agent also comprises at least one in anti-sedimentation agent and thinner, and its addition is 0.6 ~ 20 part.
9. caking agent according to claim 8, is characterized in that, described anti-sedimentation agent is selected from that polymeric amide is cured, one in polyacrylate and aerosil, and described thinner is non-volatility thinner.
10. a preparation method for caking agent as claimed in claim 1, is characterized in that, described preparation method comprises the following steps:
(1a) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2a), after adding matrix resin and toning agent in the filler of the high-k after step (1a) process, redispersion is carried out to it, stirs, obtain described caking agent;
Or described preparation method comprises the following steps:
(1b) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring;
(2b) proceed to sand mill or milling train carries out redispersion after dispersion, obtain described caking agent.
The preparation method of 11. 1 kinds of caking agents as claimed in claim 8, is characterized in that, described preparation method comprises the following steps:
(1c) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2c), after adding matrix resin, thinner and toning agent in the filler of the high-k after step (1c) process, redispersion is carried out to it;
(3c) then add anti-sedimentation agent, stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1d) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, thinner, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring,
(2d) proceed to sand mill or milling train carries out redispersion after dispersion, add anti-sedimentation agent after discharging and stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1e) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2e), after adding matrix resin, thinner and toning agent in the filler of the high-k after step (1e) process, redispersion is carried out to it, stirs, obtain described caking agent;
Or described preparation method comprises the following steps:
(1f) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring;
(2f) proceed to sand mill or milling train carries out redispersion after dispersion, add anti-sedimentation agent after discharging and stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1g) under vacuum, carry out pre-dispersed to the filler of high-k, by interpolation dispersion agent and coupling agent, surface modification treatment is carried out to the filler of described high-k;
(2g), after adding matrix resin, toning agent in the filler of the high-k after step (1g) process, redispersion is carried out to it;
(3g) then add anti-sedimentation agent, stir, obtain described caking agent;
Or described preparation method comprises the following steps:
(1h) under vacuum, by the filler of matrix resin, dispersion agent, coupling agent, thinner, high-k and toning agent mixing after in stirrer or planetary mixer dispersed with stirring,
(2h) proceed to sand mill or milling train carries out redispersion after dispersion, obtain described caking agent.
The preparation method of 12. caking agents according to claim 10 or 11, it is characterized in that, described in described step (1a), (1c), (1e) and (1g), surface modification treatment mode is the one in ball milling, planetary mills, sand milling and planet stirring, and described in described step (2a), (2c), (2e) and (2g), dispersing mode is the one in ball milling, sand milling, planet stirring and milling train.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105952749A (en) * | 2016-06-21 | 2016-09-21 | 深圳爱易瑞科技有限公司 | Adhesive dispensing method for fingerprint recognition module |
| CN105972017A (en) * | 2016-06-21 | 2016-09-28 | 深圳爱易瑞科技有限公司 | Automatic dispensing control method |
| CN106024945A (en) * | 2016-06-15 | 2016-10-12 | 李孟平 | High-durability solar panel back film |
| CN106995313A (en) * | 2017-05-06 | 2017-08-01 | 信阳师范学院 | A kind of potassium-sodium niobate-based ceramic powder and preparation method thereof |
| CN109485822A (en) * | 2018-11-28 | 2019-03-19 | 四川九洲电器集团有限责任公司 | The preparation method of encapsulating polyurethane foam |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106024945A (en) * | 2016-06-15 | 2016-10-12 | 李孟平 | High-durability solar panel back film |
| CN105952749A (en) * | 2016-06-21 | 2016-09-21 | 深圳爱易瑞科技有限公司 | Adhesive dispensing method for fingerprint recognition module |
| CN105972017A (en) * | 2016-06-21 | 2016-09-28 | 深圳爱易瑞科技有限公司 | Automatic dispensing control method |
| CN105972017B (en) * | 2016-06-21 | 2019-01-18 | 黄伟 | A kind of automatic control dispensing method |
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| CN106995313A (en) * | 2017-05-06 | 2017-08-01 | 信阳师范学院 | A kind of potassium-sodium niobate-based ceramic powder and preparation method thereof |
| CN106995313B (en) * | 2017-05-06 | 2020-05-08 | 信阳师范学院 | Potassium sodium niobate-based ceramic powder and preparation method thereof |
| CN109485822A (en) * | 2018-11-28 | 2019-03-19 | 四川九洲电器集团有限责任公司 | The preparation method of encapsulating polyurethane foam |
| CN113956818A (en) * | 2021-10-28 | 2022-01-21 | 东莞市骏青电子科技有限公司 | High-insulativity acrylic adhesive tape and preparation method thereof |
| CN113956818B (en) * | 2021-10-28 | 2023-01-24 | 东莞市骏青电子科技有限公司 | High-insulativity acrylic adhesive tape and preparation method thereof |
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Application publication date: 20150506 |