CN105086855A - Bonding method of silicone rubber and article and flexible wave-absorbing material - Google Patents
Bonding method of silicone rubber and article and flexible wave-absorbing material Download PDFInfo
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Abstract
The invention discloses a bonding method of silicone rubber and an article, a method of adding a microstructure interlayer between silicone rubber bases and a flexible wave-absorbing material. According to the bonding method of the silicone rubber and the article, the article is made from a material different from the silicone rubber, and the bonding method comprises the following steps: (1) uniformly coating an epoxy bonding agent on a bonding surface of the article, and baking the article to enable the epoxy bonding agent to be in a half-cured state; (2) uniformly coating a layer of the silicone bonding agent on the bonding surface of the silicone rubber; (3) pressing and bonding the bonding surface coated with the epoxy bonding agent of the article in the step(1) and the bonding surface coated with the silicone bonding agent of the silicone rubber in the step(2); and and (4) enabling the epoxy bonding agent and the silicone bonding agent to be completely cured. The bonding method of the silicone rubber and the article provided by the invention is simple and feasible and is large in bond strength.
Description
Technical field
The present invention relates to absorbing material, particularly relate to the adhesive method of a kind of silicon rubber and object and flexible absorbing material.
Background technology
Water insoluble and any solvent of silicon rubber, nonpoisonous and tasteless, stable chemical nature, does not react with any material except highly basic, hydrofluoric acid.The chemical composition of silicon rubber and physical structure, determine it have other same type of material many be difficult to replace feature.Silicon rubber has acidproof, alkaline-resisting, resistant to elevated temperatures feature as the matrix of absorbing material, but also makes absorbing material have flexibility.
Existing flexible absorbing material uses rubber and wave absorbing agent filler by a certain percentage through mixing, electromagnetic-wave absorbing rubber paster is made in calendering, but the complex process of this mode, labour intensity is large, and the absorption frequency scope (hereinafter referred to as Absorber Bandwidth) of this absorbing material is less.
Simultaneously, prior art generally uses curable adhesive the method for silicon rubber and plastic bonding, and this method first prepares curable adhesive, then by filling in point gum machine for the curable adhesive prepared, by point gum machine point glue in silicon rubber bonding plane, then fit with plastic component.Laminating posterior photocuring.The shortcoming of this method needs the plurality of devices such as ultra-violet apparatus, point gum machine exactly, adds cost, adds Making programme.
Summary of the invention
In order to make up above-mentioned the deficiencies in the prior art, the invention provides the adhesive method of a kind of silicon rubber and object, between silicone rubber matrix, adding the method for microstructure interlayer and flexible absorbing material.
Technical problem of the present invention is solved by following technical scheme:
An adhesive method for silicon rubber and object, described object adopts the material different from described silicon rubber, comprises the steps:
(1) on the adhesive surface of described object, evenly apply epoxy adhesive, and be baked to and make described epoxy adhesive be semi-cured state;
(2) evenly coating one deck silicone adhesive agent on the adhesive surface of described silicon rubber;
(3) the bonding rear pressing of adhesive surface being coated with the described silicon rubber of described silicone adhesive agent in the adhesive surface of the described object of described epoxy adhesive and step (2) will be coated with in step (1);
(4) described epoxy adhesive and described silicone adhesive agent is made to solidify completely.
Preferably, described object adopts plastics or electro-conductive material.
Above technical scheme is simple, and cohesive strength is large, can use the occasion of silicon rubber and plastic bonding, also may be used for the bonding of silicone rubber matrix and microstructure.
Preferably, before step (1), also comprise the steps: film silicon rubber salivation or the mode of scraper being made 0.5-1mm thickness.
Preferably, described epoxy adhesive is epoxy AB glue, and wherein, described epoxy AB glue comprises component A and B component and is that 100:43 mixes by the mass ratio of described component A and B component.
Preferably, vacuum bag pressure method is adopted to carry out described pressing in step (3).
Adopt vacuum bag pressure method to carry out layer that pressing can ensure that epoxy adhesive and silicone adhesive agent formed further evenly and bubble-free.
A kind of flexible absorbing material, comprise the first silicon rubber and polyimide film, the one side of described polyimide film is provided with at least one microstructure, described microstructure is made up of electro-conductive material, the one side being provided with microstructure of polyimide film is evenly coated with epoxy bonds oxidant layer, the one side of described first silicon rubber is evenly coated with silicone adhesive oxidant layer, the one side being provided with microstructure of polyimide film is fitted in the one side of the first silicon rubber being coated with silicon rubber binding agent, described silicone adhesive oxidant layer and the bonding rear pressing of described epoxy bonds oxidant layer.
In silicone rubber matrix, add microstructure, the Absorber Bandwidth of flexible absorbing material can be expanded, and by the position of the size adjusting absorption peak of microstructure, good absorption can be had in the frequency range needed.
Preferably, described flexible absorbing material also comprises the second silicon rubber, the one side not being provided with microstructure of described polyimide film is also coated with epoxy bonds oxidant layer, the one side of described second silicon rubber is coated with silicone adhesive oxidant layer, the bonding rear pressing of epoxy bonds oxidant layer be not provided with in the one side of microstructure of the silicone adhesive oxidant layer in the one side of described second silicon rubber and described polyimide film.
Microstructure can expand the Absorber Bandwidth of flexible absorbing material as interlayer, and by the position of microstructure interlayer, and the position adjusting absorption peak realizes the absorption to special frequency channel.
Preferably, described flexible absorbing material also comprises wave absorbing agent, and described wave absorbing agent is magneticsubstance, and described wave absorbing agent and described first silicon rubber are mixed into one, and wherein, the mass ratio of described wave absorbing agent and described first silicon rubber is between 13:7 ~ 4:1.
Preferably, described flexible absorbing material also comprises wave absorbing agent, and described wave absorbing agent is magneticsubstance, and described wave absorbing agent and described second silicon rubber are mixed into one, and wherein, the mass ratio of described wave absorbing agent and described second silicon rubber is between 13:7 ~ 4:1.
Preferably, the thickness of described microstructure is 10-20 μm, and the thickness of described polyimide film is 65-85 μm, and described microstructure is in the first-class gap periods arrangement of polyimide film.
Preferably, the total thickness of described silicon rubber and the second silicon rubber is 1.2 ± 0.1mm.
A kind of method adding microstructure interlayer between silicone rubber matrix, described silicone rubber matrix comprises the first silicone rubber matrix and the second silicone rubber matrix, described microstructure makes also load in the one side of polyimide film by electro-conductive material, described microstructure is in the first-class gap periods arrangement of polyimide film, wherein, described method comprises the steps:
(1) beat through hole at the interval of every two adjacent described microstructures, this through hole is through to another side from the one side of polyimide film;
(2) by the mode of curtain coating or scraper, silicon rubber is done film forming, and be cured in semi-cured state to obtain described first silicone rubber matrix;
(3) one side of the polyimide film of step (1) is layered on described first silicone rubber matrix under semi-cured state;
(4) on the another side of the polyimide film of step (1), by the mode of curtain coating or scraper, silicon rubber is made the second silicone rubber matrix, obtain matrix material;
(5) described matrix material is solidified completely, obtain flexible absorbing material.
Adopt above method, utilize through hole, co-curing after upper and lower two-layer uncured silicon rubber filling is contacted in through hole, microstructure can be bonded on silicon rubber without binding agent, cohesive strength can also be made to reach bulk strength, and interiors of products does not have bubble yet.
Preferably, in step (2), the detailed step of described first silicone rubber matrix of preparation comprises:
A, silicon rubber and magneticsubstance powder are made into slurry, in described slurry, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1;
B, by the mode of curtain coating or scraper, described slurry is made the film of 0.5-1mm thickness, and be cured in semi-cured state to obtain described first silicone rubber matrix.
Further preferably, in described step B, by the mode of curtain coating, described slurry is made the film of 0.5-1mm thickness, and is cured to and specifically comprises with the step obtaining described first silicone rubber matrix in semi-cured state:
Described slurry is added feed chute, and wherein, the width of described hopper is 27-30cm, and the gap of casting knife and travelling belt is the thickness of described first silicone rubber matrix that need prepare, and the speed of described travelling belt is 0.1-0.5m/min;
After described slurry has salivated, open heating container to make described slurry semicure, wherein, the Heating temperature of described heating container is 80 ~ 120 DEG C, and the time is 10-30min.
Preferably, in step (4), the detailed step of described second silicone rubber matrix of preparation comprises:
A, silicon rubber and magneticsubstance powder are made into slurry, in described slurry, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1;
B, by the mode of curtain coating or scraper, described slurry is made the film of 0.5-1mm thickness, and solidification obtains described second silicone rubber matrix.
Further preferably, in described step B, by the mode of curtain coating, described slurry is made the film of 0.5-1mm thickness, and the step that solidification obtains described second silicone rubber matrix specifically comprises:
Described slurry is added feed chute, and wherein, the width of described hopper is 27-30cm, and the gap of casting knife and travelling belt is the thickness of described second silicone rubber matrix that need prepare, and the speed of described travelling belt is 0.1-0.5m/min;
After described slurry has salivated, open heating container to make described slurry curing, wherein, the Heating temperature of described heating container is 80 ~ 120 DEG C, and the time is 1.5-2h.
A kind of flexible absorbing material prepared by above-mentioned method, comprise the first silicone rubber matrix, second silicone rubber matrix, be folded in the microstructured layers between described first silicone rubber matrix and the second silicone rubber matrix, described microstructured layers comprises polyimide film and the microstructure of load in described polyimide film one side, described microstructure is made up of electro-conductive material, described microstructure is in the first-class gap periods arrangement of polyimide film, all there is through hole at the interval of every two adjacent described microstructures, this through hole is through to another side from the one side of polyimide film, the raw material of preparation first silicone rubber matrix and/or the second silicone rubber matrix is filled with in described through hole, described raw material comprises silicon rubber.
Preferably, also comprise magneticsubstance powder in described raw material, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1.
Preferably, the thickness of described first silicone rubber matrix is 0.5-1mm; And/or the thickness of described second silicon rubber is 0.5-1mm.
Flexible absorbing material of the present invention can change shape arbitrarily, can be pasted onto complex-shaped stealthy device and need on radiation-resistant device.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the microstructure in flexible absorbing material of the present invention is arranged at polyimide film;
Fig. 2 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention three;
Fig. 3 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention four;
Fig. 4 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention five;
Fig. 5 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention six;
Fig. 6 is the reflectance test result schematic diagram of the flexible absorbing material of comparative example one of the present invention;
Fig. 7 is the reflectance test result schematic diagram of the flexible absorbing material of comparative example two of the present invention;
Fig. 8 is the reflectance test result schematic diagram of the flexible absorbing material of comparative example three of the present invention;
Fig. 9 is the Rotating fields schematic diagram of the flexible absorbing material of the embodiment of the present invention seven ~ 12;
Figure 10 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention seven and eight;
Figure 11 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention nine and ten;
Figure 12 is the reflectance test result schematic diagram of the flexible absorbing material of the embodiment of the present invention 11 and 12;
Figure 13 is that in comparative example four of the present invention, thickness is the reflectance test result schematic diagram of the flexible absorbing material of 1.2mm;
Figure 14 is that in comparative example four of the present invention, thickness is the reflectance test result schematic diagram of the flexible absorbing material of 1.4mm;
The Rotating fields schematic diagram of the flexible absorbing material in Figure 15 embodiment of the present invention 13 and 14;
Figure 16 is the schematic diagram that microstructure that in the embodiment of the present invention 13 and 14, step (1) obtains is arranged at polyimide film.
Embodiment
Below contrast accompanying drawing and combine preferred embodiment the invention will be further described.
The invention provides the adhesive method of a kind of silicon rubber and object, described object adopts the material different from described silicon rubber, in one embodiment, comprises the steps:
(1) on the adhesive surface of described object, evenly apply epoxy adhesive, and be baked to and make epoxy adhesive be semi-cured state;
(2) evenly coating one deck silicone adhesive agent on the adhesive surface of silicon rubber;
(3) the bonding rear pressing of adhesive surface being coated with the silicon rubber of silicone adhesive agent in the adhesive surface of the object of epoxy adhesive and step (2) will be coated with in step (1); Silicone adhesive agent is easily solidified in atmosphere, not easily smoothen in the process be coated with, pressing can make silicone adhesive agent evenly and not stay bubble under pressure again, because if having bubble in sample, the electromagnetic performance of material can be affected, adopt vacuum bag pressure method to carry out pressing in a preferred embodiment.
(4) epoxy adhesive and silicone adhesive agent is made to solidify completely.
Wherein, preferred described silicone adhesive agent is at least one in single-component room-temperature vulcanized type silicon rubber, single component heating cure silicon rubber and bi-component addition type silica gel.Before step (1), also comprise the steps: film silicon rubber salivation or the mode of scraper being made 0.5-1mm thickness.
Described epoxy adhesive is epoxy AB glue, and epoxy AB glue comprises component A and B component and is that 100:43 mixes by the mass ratio of described component A and B component.Object adopts plastics or electro-conductive material, electro-conductive material may be used for making the microstructure (also referred to as electric circuit analogy structure) having and inhale ripple effect, by microstructure load on polyimide film, the pattern of microstructure can be two dimension or three-dimensional, as box-shaped, I-shaped, snowflake shape, hollow circular etc., as long as microstructure mainly has reflection and transmission effect to hertzian wave, no matter what shape and pattern, can as microstructure of the present invention.
Microstructure below in all embodiments is described for square block, and silicon rubber is the silicon rubber of the two component of AB, adopts Dow corning DC184 silicon rubber.Epoxy AB glue is produced by Shanghai Kangda Chemical New Material Co., Ltd..Single-component silicon glue caking agent is the E41 type silicone adhesive agent of being produced by German Wa Ke company.Bi-component addition type silica gel is the 707 silicon rubber binding agents produced by German Wa Ke company, and normal temperature refers to temperature 20-25 DEG C.
Be described in detail below by way of the adhesive method of specific embodiment to silicon rubber and object.
Embodiment one
(1) mode of silicon rubber curtain coating or scraper is made the film of 0.5-1mm thickness, stand-by after solidification, in this example, thickness is 0.8mm; Electrically conductive ink is made microstructure on polyimide film.
(2) component A of epoxy AB glue and B component are 100:43 mixing in mass ratio, are evenly coated in the one side of the polyimide film being provided with microstructure.
(3) microstructure is toasted 10-15min in 80 degree of baking boxs, be semi-cured state (namely not completely crued state, is as the criterion with tack-free) with epoxy AB glue, then take out.
(4) agent of E41 type silicone adhesive is evenly coated in the one side of silicon rubber.
(5) will the one side of E41 type silicone adhesive agent be scribbled and have the one side bonding rear employing vacuum bag pressure method pressing scribbling epoxy AB glue.
(6) the product normal temperature after bonding places 48 hours, after the silicone adhesive agent of E41 type and epoxy AB solidify completely.
Embodiment two
Step (1) ~ (3) and embodiment are together;
(4) 707 type silicone adhesive agent are evenly coated in the one side of silicon rubber.
(5) will the one side of 707 type silicone adhesive agent be scribbled and have the one side bonding rear employing vacuum bag pressure method pressing scribbling epoxy AB glue.
(6) the product normal temperature after bonding places 48 hours, after 707 type silicone adhesive agent and epoxy AB solidify completely.
Peel strength test is carried out to the product in embodiment one and two, because microstructure during test stripping strength is not torn, but silicon rubber is torn to shreds, therefore can think that the stripping strength of silicon rubber is greater than its tensile strength, the stripping strength that the tensile strength provided in the specification sheets according to DOW CORNING DC184 silicon rubber is released is about 7.1*10
6n/m.
As known from the above, adopt above technical scheme silicon rubber and plastics or electro-conductive material can be bondd, the method is simple, without complex apparatus, has saved cost, can also effectively solve silicon rubber and be combined with microstructure.
The present invention also discloses a kind of flexible absorbing material, in one embodiment, comprise the first silicon rubber and polyimide film, the one side of described polyimide film is provided with at least one microstructure, described microstructure is made up of electro-conductive material, the one side being provided with microstructure of polyimide film is evenly coated with epoxy bonds oxidant layer, the one side of described first silicon rubber is evenly coated with silicone adhesive oxidant layer, the one side being provided with microstructure of polyimide film is fitted in the one side of the first silicon rubber being coated with silicon rubber binding agent, described silicone adhesive oxidant layer and the bonding rear pressing of described epoxy bonds oxidant layer.
Wherein, vacuum bag pressure method can be preferably adopted to carry out pressing, first silicon rubber is the matrix as flexible absorbing material, polyimide film is the carrier as microstructure, have microstructure at the one side of polyimide film, as previously mentioned, microstructure can be the microstructure with different shape formed with electro-conductive material, as microstructure can be made of Copper Foil, also can make of electrically conductive ink.Preferably, the thickness of described first silicon rubber is 0.5-1mm.
In a preferred embodiment, described flexible absorbing material also comprises the second silicon rubber, the one side not being provided with microstructure of described polyimide film is also coated with epoxy bonds oxidant layer, the one side of described second silicon rubber is coated with silicone adhesive oxidant layer, the bonding rear pressing of epoxy bonds oxidant layer be not provided with in the one side of microstructure of the silicone adhesive oxidant layer in the one side of described second silicon rubber and polyimide film, and further preferably, the total thickness of described silicon rubber and the second silicon rubber is 1.2 ± 0.1mm.
In above embodiment, preferably can also comprise wave absorbing agent at described flexible absorbing material, described wave absorbing agent is magneticsubstance, described wave absorbing agent can be mixed into one respectively with described first silicon rubber and/or the second silicon rubber, the mass ratio of described wave absorbing agent and the first silicon rubber is between 13:7 ~ 4:1, and the mass ratio of described wave absorbing agent and the second silicon rubber is between 13:7 ~ 4:1.Wherein, magneticsubstance can be magneticmetal powder, as carbonyl iron dust.Preferably, the thickness of described microstructure is 10-20 μm, and the thickness of described polyimide film is 65-85 μm, and described microstructure is in the first-class gap periods arrangement of polyimide film.
Be described in detail to flexible absorbing material below by way of embodiment more specifically, the microstructure in following examples is made by Copper Foil, and the shape of microstructure is square block shape.Microstructure 21 is arranged on polyimide film 2 by identical gap period as shown in Figure 1, be covered with required area, wherein horizontal or longitudinal upper microstructure length of side is 1.1 ~ 1.8mm, namely as shown in fig. 1, the scope of a is 2-2.7mm, and the interval b of two the adjacent microstructures on horizontal or longitudinal is constant is 0.9mm.
Embodiment three
(1) the ratio mechanical stirring being 4:1 in mass ratio by carbonyl iron dust and silicon rubber mixes, and stirring velocity 300-500r/min, the time is 0.5-1h, and in this example, stirring velocity is 400r/min, and the time is 1h.Wherein, used is the digital display stirrer that Shanghai Suo Ying plant and instrument company limited produces, and silicon rubber adopts A, B two-part liquid silicon rubber, mass ratio A:B=10:1.
(2) the slurry curtain coating on casting machine mixed in step (1), making thickness 1.2 ± 0.1mm, is the flexible absorbing material matrix of 1.2mm in this example.Casting step concrete on casting machine is as follows:
The slurry mixed in step (1) is added feed chute, the width of hopper is 27-30cm, the gap of casting knife and travelling belt is the thickness of flexible absorbing material matrix, and in this example, the gap of casting knife and travelling belt is 1.2mm, and the speed of travelling belt is 0.1-0.5m/min.Open heating container after slurry has salivated, Heating temperature is 80 ~ 120 DEG C, time 1.5-2h, and slurry curing completes, and makes the flexible absorbing material matrix of thickness 1.2mm.
(3) surface uniform of flexible absorbing material matrix is coated with last layer single-component silicon glue caking agent.
(4) on polyimide film, microstructure is made with Copper Foil, microstructure 21 is evenly arranged at equal intervals on polyimide film 2, as shown in Figure 1, wherein the scope of a is 2-2.7mm, interval b is constant is 0.9mm, a=2mm in this example, is evenly coated with last layer epoxy adhesive in the side being provided with microstructure.
(5) will scribble after epoxy adhesive and single-component silicon glue caking agent bond and adopt vacuum bag pressure method pressing, place after 48 hours, caking agent curing molding obtains flexible absorbing material.
The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in Figure 2.
Embodiment four
Be with the difference of embodiment three: the microstructure adopting a=2.7mm in step (4).Other steps are identical with embodiment three.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in Figure 3.
Embodiment five
Be with the difference of embodiment three: in step (1), carbonyl iron dust and silicon rubber are 13:7 in mass ratio.Other steps are identical with embodiment three.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in Figure 4.
Embodiment six
Be with the difference of embodiment five: the microstructure adopting a=2.7mm in step (4).Other steps are identical with embodiment five.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in Figure 5.
Comparative example one
Embodiment three also can as flexible absorbing material by the flexible absorbing material matrix that step (1) and (2) obtain, and directly carry out reflectance test when not pasting microstructure, result as shown in Figure 6.
Comparative example two
Embodiment five also can as flexible absorbing material by the flexible absorbing material matrix that step (1) and (2) obtain, and directly carry out reflectance test when not pasting microstructure, result as shown in Figure 7.
Comparative example three
(1) the ratio mechanical stirring being 4:1 in mass ratio by carbonyl iron dust and silicon rubber mixes, and machine used is the digital display stirrer that Shanghai Suo Ying plant and instrument company limited produces, and stirring velocity 400r/min, the time is 1h.
(2) the slurry curtain coating on casting machine mixed in step (1), the flexible absorbing material of thickness 1.5mm is made.
(3) size that sample is cut into 300mm*300mm is carried out reflectance test, test result as shown in Figure 8.
When more than carrying out reflectance test, needs (also can be coat silicone adhesive agent on silicon rubber at the bonding one piece of smooth metal backing of the another side of the silicon rubber bonding with microstructure, the one side of metal backing coats epoxy adhesive, then silicone adhesive agent and epoxy adhesive are bonded), metal backing can adopt the FR4 plate covering copper, also can adopt Copper Foil.Above reflectance test is all be as the criterion with GJB2038-94 standard.The test result of each embodiment and comparative example illustrates above:
1, from Fig. 2,3,6 as seen when the thickness of flexible absorbing material matrix identical with the ratio of absorption agent (80%), the Absorber Bandwidth of flexible absorbing material more than-10dB not having microstructure (Fig. 6) is 12-18GHz.Be provided with (Fig. 2,3) of microstructure, when a is 2mm, the above Absorber Bandwidth of-10dB is 10-16.5GHz, when a is 2.7mm, the above Absorber Bandwidth of-10dB is 8.5-12.5GHz, so Absorber Bandwidth is wider when a is 2mm.Contrasted from Fig. 2 and Fig. 3, the size of adjustment a can make the position reaching adjustment absorption peak.Existing when not using microstructure, the position of absorption peak can only be adjusted by the ratio increasing thickness or increase filler, so just make sample increase weight more.
2, in the present invention, the total thickness being provided with the polyimide film of microstructure is 75-105 μm, and wherein copper thickness 10-20 μm, the microstructure of a 300mm*300mm only has about 10g.As seen from Figure 8, when thickness is 1.5mm under identical absorption agent ratio, just can reach the assimilation effect close with Fig. 2, and at this moment absorbing material presses size weightening finish about the 92g of 300mm*300mm.
3, from Fig. 4,5,7 as seen when the thickness of flexible absorbing material identical with the ratio of absorption agent (65%), do not have the flexible absorbing material of microstructure (Fig. 7) to be absorbed within the scope of 1-18GHz and almost there is no below-10dB.Be provided with (Fig. 4,5) of microstructure, when a is 2mm, the Absorber Bandwidth of more than-10dB is 14-18GHz, when a is 2.7mm, the Absorber Bandwidth of more than-10dB is 11-17GHz.When not having microstructure, bandwidth is obviously smaller, and when a is 2.7mm, Absorber Bandwidth is wider, and the size also showing a becomes the position that can adjust greatly absorption peak.
Therefore, in silicon rubber, introduce microstructure, wave absorbing agent can coordinate with microstructure with the proper ratio of silicon rubber, obtains good flexible absorbing material.
Embodiment seven ~ embodiment 12, microstructure is folded between flexible absorbing material matrix, the laminated layer sequence of flexible absorbing material as shown in Figure 9, wherein, 1 is the first flexible absorbing material matrix, 2 is polyimide films that load has microstructure, and 3 is second flexible absorbing material matrixes, and 4 is the metal backings of stickup when carrying out reflectance test.Utilize the thickness of flexible absorbing material matrix to adjust the position of microstructure interlayer in integral material, and keep the total thickness of absorbing material matrix to be all 1.2 ± 0.1mm.
Embodiment seven
(1) the ratio mechanical stirring being 4:1 in mass ratio by carbonyl iron dust and silicon rubber mixes, and stirring velocity 300-500r/min, the time is 0.5-1h, and in this example, stirring velocity is 400r/min, and the time is 1h.Wherein, used is the digital display stirrer that Shanghai Suo Ying plant and instrument company limited produces, and silicon rubber adopts A, B two-part liquid silicon rubber, mass ratio A:B=10:1.
(2) the slurry curtain coating on casting machine mixed in step (1), the first and second flexible absorbing material matrixes of thickness 0.9 ± 0.05mm (being 0.9mm in this example) and 0.3 ± 0.05mm (being 0.3mm in this example) are obtained respectively.Casting step concrete on casting machine is as follows:
The slurry mixed in step (1) is added feed chute, the width of hopper is 27-30cm, the gap of casting knife and travelling belt is the thickness of flexible absorbing material matrix, and in this example, the gap of casting knife and travelling belt is respectively 0.9mm and 0.3mm, and the speed of travelling belt is 0.1-0.5m/min.Open heating container after slurry has salivated, Heating temperature is 80 ~ 120 DEG C, time 1.5-2h, and slurry curing completes, and obtains the flexible absorbing material matrix of thickness 0.9mm and 0.3mm respectively.
(3) respectively a surface uniform of a surface of the first flexible absorbing material matrix and the second flexible absorbing material matrix is coated with last layer single-component silicon glue caking agent.
(4) on polyimide film, microstructure is made with Copper Foil, microstructure is evenly arranged at equal intervals on polyimide film, as shown in Figure 1, wherein the scope of a is 2-2.7mm, interval b is constant is 0.9mm, a=2mm in this example, is evenly coated with last layer epoxy adhesive on the two sides of polyimide, and epoxy adhesive can adopt epoxy AB glue.
(5) one side of the polyimide being provided with microstructure is pasted onto in the one side of the second flexible absorbing material matrix, the one side of the polyimide not being provided with microstructure is pasted onto in the one side of the first flexible absorbing material matrix, after normal temperature places 48 hours, caking agent curing molding obtains flexible absorbing material.
The flexible absorbing material obtained is cut into the square of 300mm*300mm, the one side of the metal backing 4 scribbling epoxy adhesive be pasted onto on the another side of the second flexible absorbing material matrix, for reflectance test after curing molding, test result as shown in Figure 10.
Embodiment eight
Be with the difference of embodiment seven: a=2.7mm in microstructure.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in Figure 10.
Embodiment nine
Be with the difference of embodiment seven: the thickness of the first and second flexible absorbing material matrixes is 0.6mm.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in figure 11.
Embodiment ten
Be with the difference of embodiment eight: the thickness of the first and second flexible absorbing material matrixes is 0.6mm.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in figure 11.
Embodiment 11
Be with the difference of embodiment seven: the thickness of the first and second flexible absorbing material matrixes is respectively 0.3mm and 0.9mm.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in figure 12.
Embodiment 12
Be with the difference of embodiment eight: the thickness of the first and second flexible absorbing material matrixes is respectively 0.3mm and 0.9mm.The flexible absorbing material obtained is cut into the square of 300mm*300mm, for reflectance test, test result as shown in figure 12.
Comparative example four
(1) the ratio mechanical stirring being 4:1 in mass ratio by carbonyl iron dust and silicon rubber mixes, and machine used is the digital display stirrer that Shanghai Suo Ying plant and instrument company limited produces, and stirring velocity 400r/min, the time is 1h.
(2) the slurry curtain coating on casting machine mixed in step (1), specific as follows:
The slurry mixed in step (1) is added feed chute, and the width of hopper is 27-30cm, and salivation cutter and the gap of travelling belt are 1.4 and 1.2mm respectively, and the speed of travelling belt is 0.1-0.5m/min.Open heating container after slurry has salivated, Heating temperature is 80 ~ 120 DEG C, time 1.5-2h, and slurry curing completes, and obtains the first and second flexible absorbing materials of thickness 1.4 ± 0.1mm and 1.2 ± 0.1mm respectively.
(3) respectively the size that the flexible absorbing material of 1.4mm and 1.2mm is cut into 300mm*300mm is carried out reflectance test.As shown in figure 13, the test result of 1.4mm as shown in figure 14 for 1.2mm test result.
Above reflectance test is all be as the criterion with GJB2038-94 standard.The test result of each embodiment and comparative example illustrates above: from Figure 10,11,12 as seen when microstructure is more away from metal backing, the absorption peak of flexible absorbing material more moves to low frequency.Figure 10,11, the Absorber Bandwidth of-10dB in 12 all curves, have wide also have narrow, when the distance of microstructure and metal backing is 0.3mm, and during a=2.7mm, Absorber Bandwidth is the widest, reach about 11-18GHz, compared with the curve of Figure 13, obviously visible microstructure interlayer adds the Absorber Bandwidth of flexible absorbing material, and suitable microstructure size and suitable interlayer position are described, not only can adjust the position of absorption peak, can also Absorber Bandwidth be increased.
Prior art realizes with the ratio of the thickness and absorption agent that increase absorbing material the position adjusting absorption peak.Figure 14 is the absorbing material not having microstructure interlayer of 1.4mm, its performance with have microstructure interlayer to absorb the similar nature of best absorbing material, at this moment increase weight absorbing material (300mm*300mm size) about 60g, and the weight of microstructure (300mm*300mm size) only has about 10g.
In sum, microstructure interlayer can increase the bandwidth of absorbing material, by adjusting the position of interlayer, can also adjust the position of absorbing material absorption peak, and the overall weight of flexible absorbing material increases few.
The present invention also provides a kind of method adding microstructure interlayer between silicone rubber matrix, in one embodiment, described silicone rubber matrix comprises the first silicone rubber matrix and the second silicone rubber matrix, described microstructure makes also load in the one side of polyimide film by electro-conductive material, described microstructure is in the first-class gap periods arrangement of polyimide film, and described method comprises the steps:
(1) beat through hole 5 at the interval of every two adjacent microstructures 21, this through hole 5 is through to another side from the one side of polyimide film 2, as shown in figure 16;
(2) by the mode of curtain coating or scraper, silicon rubber is done film forming, and be cured in semi-cured state to obtain the first silicone rubber matrix;
(3) one side of the polyimide film of step (1) is layered on the first silicone rubber matrix under semi-cured state;
(4) on the another side of the polyimide film of step (1), by the mode of curtain coating or scraper, silicon rubber is made the second silicone rubber matrix, obtain matrix material;
(5) described matrix material is solidified completely, obtain flexible absorbing material.
Wherein, the detailed step preparing the first silicone rubber matrix and the second silicone rubber matrix preferably includes:
A, silicon rubber and magneticsubstance powder are made into slurry, in described slurry, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1;
B, the slurry mixed in steps A is added feed chute, the width of hopper is 27-30cm, and the gap of salivation cutter and travelling belt is 0.5-1mm, and the speed of travelling belt is 0.1-0.5m/min.Open heating container after slurry has salivated, Heating temperature is 80 ~ 120 DEG C, time 10-30 minute, makes slurry semicure obtain the first silicone rubber matrix.
C, on the polyimide film completed, salivate the second silicone rubber matrix, specifically: the slurry mixed in steps A is added the second hopper, the width of the second hopper is 27-30cm, and the gap of the second salivation cutter and travelling belt is 1-2mm, and the speed of travelling belt is 0.1-0.5m/min.Open heating container after slurry has salivated, Heating temperature is 80 ~ 120 DEG C, time 1.5-2h, and slurry solidifies obtain the second silicone rubber matrix completely.
Accordingly, the present invention also provides a kind of flexible absorbing material prepared by above-mentioned method, in one embodiment, as shown in figs, comprise the first silicone rubber matrix 1, second silicone rubber matrix 3, be folded in the microstructured layers between described first silicone rubber matrix 1 and the second silicone rubber matrix 3, described microstructured layers comprises polyimide film 2 and the microstructure 21 of load in described polyimide film one side, described microstructure is made up of electro-conductive material, described microstructure is in the first-class gap periods arrangement of polyimide film, all there is through hole 5 at the interval of every two adjacent microstructures, this through hole 5 is through to another side from the one side of polyimide film 2, the raw material of preparation first silicone rubber matrix and/or the second silicone rubber matrix is filled with in described through hole, described raw material comprises silicon rubber.
In a preferred embodiment, also comprise magneticsubstance powder in described raw material, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1.
Be described below by way of embodiment more specifically, in following examples, silicon rubber adopts Dow corning DC184 silicon rubber, and polyimide membrane carrier is covered with the microstructure of Copper Foil etching.Iron powder is the carbonyl iron dust (ew iron powder) that BASF is produced.
Embodiment 13
(1) punching at the position, space of adjacent microstructure, punching when not destroying microstructure, as shown in figure 16.
(2) by the mode of curtain coating, silicon rubber is made the film of 0.5-1mm thickness, in this example, thickness is 0.6mm, and makes film hardening in semi-cured state, can be as the criterion, obtain the first silicone rubber matrix with tack-free;
(3) on the first silicone rubber matrix not establishing the one side of microstructure to be layered under semi-cured state the polyimide film of step (1);
(4) silicon rubber is made by the one side being provided with microstructure in the polyimide film of step (1) the second silicone rubber matrix of 0.5-1mm thickness by the mode of curtain coating or scraper, in this example, thickness is 0.6mm, obtains matrix material;
(5) described matrix material normal temperature shelf is solidified after 48 hours completely, obtain flexible absorbing material.
Embodiment 14
(1) punching at the position, space of adjacent microstructure, punching when not destroying microstructure, as shown in figure 15.
(2) silicon rubber and ew iron powder are made into slurry, the weight content of ew iron powder is 65% ~ 80% in the slurry, be 80% in this example, then by the mode of curtain coating or scraper, slurry is made the film of 0.5-1mm thickness, in this example, thickness is 0.6mm, and makes film hardening to being semi-cured state, can be as the criterion with tack-free, obtain the first silicone rubber matrix;
(3) one side of the polyimide film of step (1) is layered on the first silicone rubber matrix under semi-cured state;
(4) silicon rubber and ew iron powder are made into slurry, the weight content of ew iron powder is 65% ~ 80% in the slurry, be 80% in this example, then on the another side of the polyimide film of step (1), by the mode of curtain coating, slurry is made the second silicone rubber matrix of 0.5-1mm thickness, in this example, thickness is 0.6mm, obtains matrix material;
(5) described matrix material normal temperature shelf is solidified after 48 hours completely, obtain flexible absorbing material.
Peel strength test is carried out to the product in embodiment 13 and 14, because microstructure during test stripping strength is not torn, but silicon rubber is torn to shreds, therefore can think that the stripping strength of silicon rubber is greater than its tensile strength, be about 7.1*106N/m by the stripping strength released according to the tensile strength provided in the specification sheets of DOW CORNING 184 silicon rubber.
Adopt ultraviolet light polymerization in prior art, the equipment of adding turn increases cost, and caking agent changes the thickness of product, interiors of products also easily produces bubble, adopts above method, can without binding agent, cohesive strength can also be made to reach bulk strength, and interiors of products does not have bubble yet.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For those skilled in the art, without departing from the inventive concept of the premise, some equivalent to substitute or obvious modification can also be made, and performance or purposes identical, all should be considered as belonging to protection scope of the present invention.
Claims (20)
1. an adhesive method for silicon rubber and object, is characterized in that, described object adopts the material different from described silicon rubber, comprises the steps:
(1) on the adhesive surface of described object, evenly apply epoxy adhesive, and be baked to and make described epoxy adhesive be semi-cured state;
(2) evenly coating one deck silicone adhesive agent on the adhesive surface of described silicon rubber;
(3) the bonding rear pressing of adhesive surface being coated with the described silicon rubber of described silicone adhesive agent in the adhesive surface of the described object of described epoxy adhesive and step (2) will be coated with in step (1);
(4) described epoxy adhesive and described silicone adhesive agent is made to solidify completely.
2. adhesive method as claimed in claim 1, is characterized in that: described object adopts plastics or electro-conductive material.
3. adhesive method as claimed in claim 1 or 2, is characterized in that: before step (1), also comprises the steps: silicon rubber to salivate or the mode of scraper makes the film of 0.5-1mm thickness.
4. adhesive method as claimed in claim 1 or 2, is characterized in that: described epoxy adhesive is epoxy AB glue, and wherein, described epoxy AB glue comprises component A and B component and is that 100:43 mixes by the mass ratio of described component A and B component.
5. adhesive method as claimed in claim 1 or 2, is characterized in that: adopt vacuum bag pressure method to carry out described pressing in step (3).
6. a flexible absorbing material, it is characterized in that: comprise the first silicon rubber and polyimide film, the one side of described polyimide film is provided with at least one microstructure, described microstructure is made up of electro-conductive material, the one side being provided with microstructure of polyimide film is evenly coated with epoxy bonds oxidant layer, the one side of described first silicon rubber is evenly coated with silicone adhesive oxidant layer, the one side being provided with microstructure of polyimide film is fitted in the one side of the first silicon rubber being coated with silicon rubber binding agent, described silicone adhesive oxidant layer and the bonding rear pressing of described epoxy bonds oxidant layer.
7. flexible absorbing material as claimed in claim 6, it is characterized in that: described flexible absorbing material also comprises the second silicon rubber, the one side not being provided with microstructure of described polyimide film is also coated with epoxy bonds oxidant layer, the one side of described second silicon rubber is coated with silicone adhesive oxidant layer, the bonding rear pressing of epoxy bonds oxidant layer be not provided with in the one side of microstructure of the silicone adhesive oxidant layer in the one side of described second silicon rubber and described polyimide film.
8. flexible absorbing material as claimed in claims 6 or 7, it is characterized in that: described flexible absorbing material also comprises wave absorbing agent, described wave absorbing agent is magneticsubstance, described wave absorbing agent and described first silicon rubber are mixed into one, wherein, the mass ratio of described wave absorbing agent and described first silicon rubber is between 13:7 ~ 4:1.
9. flexible absorbing material as claimed in claim 7, it is characterized in that: described flexible absorbing material also comprises wave absorbing agent, described wave absorbing agent is magneticsubstance, described wave absorbing agent and described second silicon rubber are mixed into one, wherein, the mass ratio of described wave absorbing agent and described second silicon rubber is between 13:7 ~ 4:1.
10. the flexible absorbing material as described in claim 6,7 or 9, is characterized in that: the thickness of described microstructure is 10-20 μm, and the thickness of described polyimide film is 65-85 μm, and described microstructure is in the first-class gap periods arrangement of polyimide film.
11. flexible absorbing materials as claimed in claim 8, is characterized in that: the thickness of described microstructure is 10-20 μm, and the thickness of described polyimide film is 65-85 μm, and described microstructure is in the first-class gap periods arrangement of polyimide film.
12. flexible absorbing materials as claimed in claim 7, is characterized in that: the total thickness of described first silicon rubber and the second silicon rubber is 1.2 ± 0.1mm.
13. 1 kinds of methods adding microstructure interlayer between silicone rubber matrix, it is characterized in that, described silicone rubber matrix comprises the first silicone rubber matrix and the second silicone rubber matrix, described microstructure makes also load in the one side of polyimide film by electro-conductive material, described microstructure is in the first-class gap periods arrangement of polyimide film, wherein, described method comprises the steps:
(1) beat through hole at the interval of every two adjacent described microstructures, this through hole is through to another side from the one side of polyimide film;
(2) by the mode of curtain coating or scraper, silicon rubber is done film forming, and be cured in semi-cured state to obtain described first silicone rubber matrix;
(3) one side of the polyimide film of step (1) is layered on described first silicone rubber matrix under semi-cured state;
(4) on the another side of the polyimide film of step (1), by the mode of curtain coating or scraper, silicon rubber is made the second silicone rubber matrix, obtain matrix material;
(5) described matrix material is solidified completely, obtain flexible absorbing material.
14. methods as claimed in claim 13, is characterized in that: in step (2), the detailed step of described first silicone rubber matrix of preparation comprises:
A, silicon rubber and magneticsubstance powder are made into slurry, in described slurry, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1;
B, by the mode of curtain coating or scraper, described slurry is made the film of 0.5-1mm thickness, and be cured in semi-cured state to obtain described first silicone rubber matrix.
15. methods as claimed in claim 14, is characterized in that: the film by the mode of curtain coating, described slurry being made 0.5-1mm thickness in described step B, and are cured to and specifically comprise with the step obtaining described first silicone rubber matrix in semi-cured state:
Described slurry is added feed chute, and wherein, the width of described hopper is 27-30cm, and the gap of casting knife and travelling belt is the thickness of described first silicone rubber matrix that need prepare, and the speed of described travelling belt is 0.1-0.5m/min;
After described slurry has salivated, open heating container to make described slurry semicure, wherein, the Heating temperature of described heating container is 80 ~ 120 DEG C, and the time is 10-30min.
16. methods as claimed in claim 13, is characterized in that: in step (4), the detailed step of described second silicone rubber matrix of preparation comprises:
A, silicon rubber and magneticsubstance powder are made into slurry, in described slurry, the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1;
B, by the mode of curtain coating or scraper, described slurry is made the film of 0.5-1mm thickness, and solidification obtains described second silicone rubber matrix.
17. methods as claimed in claim 16, is characterized in that: the film by the mode of curtain coating, described slurry being made 0.5-1mm thickness in described step B, and the step that solidification obtains described second silicone rubber matrix specifically comprises:
Described slurry is added feed chute, and wherein, the width of described hopper is 27-30cm, and the gap of casting knife and travelling belt is the thickness of described second silicone rubber matrix that need prepare, and the speed of described travelling belt is 0.1-0.5m/min;
After described slurry has salivated, open heating container to make described slurry curing, wherein, the Heating temperature of described heating container is 80 ~ 120 DEG C, and the time is 1.5-2h.
18. 1 kinds of flexible absorbing materials prepared by the method described in claim 13-17 any one, it is characterized in that: comprise the first silicone rubber matrix, second silicone rubber matrix, be folded in the microstructured layers between described first silicone rubber matrix and the second silicone rubber matrix, described microstructured layers comprises polyimide film and the microstructure of load in described polyimide film one side, described microstructure is made up of electro-conductive material, described microstructure is in the first-class gap periods arrangement of polyimide film, all there is through hole at the interval of every two adjacent described microstructures, this through hole is through to another side from the one side of polyimide film, the raw material of preparation first silicone rubber matrix and/or the second silicone rubber matrix is filled with in described through hole, described raw material comprises silicon rubber.
19. flexible absorbing materials as claimed in claim 18, is characterized in that: also comprise magneticsubstance powder in described raw material, and the weight ratio of described magneticsubstance powder and silicon rubber is 13:7 ~ 4:1.
20. flexible absorbing materials as claimed in claim 18, is characterized in that: the thickness of described first silicone rubber matrix is 0.5-1mm; And/or the thickness of described second silicon rubber is 0.5-1mm.
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| CN111641044A (en) * | 2020-06-12 | 2020-09-08 | 中国科学院宁波材料技术与工程研究所 | Flexible electromagnetic metamaterial and preparation method thereof |
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| CN111300917B (en) * | 2020-03-10 | 2023-11-14 | 东莞市高酷纳米科技有限公司 | Anisotropic composite profile and preparation method thereof |
| CN112962328B (en) * | 2021-02-04 | 2022-04-01 | 东莞市瑞翔新型材料科技有限公司 | Special interlayer process for thin film material |
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Effective date of registration: 20210622 Address after: 2 / F, software building, No.9, Gaoxin Zhongyi Road, Nanshan District, Shenzhen City, Guangdong Province Patentee after: KUANG-CHI INSTITUTE OF ADVANCED TECHNOLOGY Address before: 18B, building a, CIC international business center, 1061 Xiangmei Road, Futian District, Shenzhen, Guangdong 518034 Patentee before: KUANG-CHI INNOVATIVE TECHNOLOGY Ltd. |