CN112143239B - Broadband heat-conducting wave-absorbing gasket and preparation method thereof - Google Patents
Broadband heat-conducting wave-absorbing gasket and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of preparation of heat-conducting wave-absorbing materials, in particular to a broadband heat-conducting wave-absorbing gasket and a preparation method thereof, wherein the broadband heat-conducting wave-absorbing gasket comprises the following components in parts by mass: vinyl polysiloxane: 100-150 parts; polydimethylsiloxane: 5-50 parts; heat-conducting powder: 150-750 parts; modifying wave-absorbing powder: 150-450 parts; volatile solvent (c): 10-50 parts; 5-30 parts of hydrogen-containing silicone oil; 1-10 parts of an inhibitor; 0.5-5 parts of a catalyst. The filling of the wave-absorbing filler is improved, the wave-absorbing performance is improved, and meanwhile, the heat-conducting performance of the material is greatly improved.
Description
Technical Field
The invention relates to the technical field of preparation of heat-conducting wave-absorbing materials, in particular to a broadband heat-conducting wave-absorbing gasket and a preparation method thereof.
Background
The wave-absorbing material is widely applied to electronic products, and along with the functions of the electronic products are more and more powerful, the size is smaller and thinner, besides functional parts, the space reserved for other auxiliary parts is smaller and smaller, and other auxiliary functions are required to be integrated in the limited space as much as possible. The heat-conducting and electromagnetic wave absorption functional filler is integrated into a system to be made into a heat-conducting wave absorption material.
At present, the heat-conducting wave-absorbing material is mainly used in a gasket mode, and has certain heat-conducting and electromagnetic absorption performances, however, in the 5G era, higher requirements are provided for products in the aspects of heat management, EMI (electromagnetic interference) resistance and the like.
The existing method still has the problems that the heat conduction-wave absorption performance is difficult to be considered, and the like, if the filler is only filled with the wave absorption filler, the general heat conduction coefficient k value is only 0.5-1W/m.k, the wave absorption filler and the heat conduction filler are required to be matched and filled for realizing the high heat conduction wave absorption and heat conduction gasket, and excessive addition of the heat conduction filler has a certain attenuation effect on the wave absorption performance, so that the absorption effect of the heat conduction and wave absorption material under low-frequency electromagnetic waves, particularly under 3GHZ, is weak.
In the prior art, the filling of the wave-absorbing filler is improved, the wave-absorbing performance is improved, and meanwhile, the heat-conducting performance of the material is greatly reduced. In addition, excessive filling of the heat-conducting filler and the wave-absorbing filler can cause great influence on the hardness and the mechanical property of the gasket. At present, for a heat-conducting wave-absorbing material, the problem of the compatibility difference between the heat-conducting filler and the wave-absorbing filler in an organic silicon system is often ignored under the filling of the heat-conducting filler and the wave-absorbing filler, the heat-conducting wave-absorbing material is difficult to have good uniform dispersion and poor dispersion effect, so that the heat-conducting wave-absorbing material and the wave-absorbing material cannot achieve ideal effects, and the problem of the heat conductivity and the wave-absorbing property of the heat-conducting wave-absorbing material are difficult to solve.
Disclosure of Invention
Unless otherwise specified, "components" and "parts" in the present invention mean "parts by mass".
In view of the above problems, embodiments of the present invention are proposed to provide a broadband heat-conducting and wave-absorbing gasket and a preparation method thereof, which overcome the above problems or at least partially solve the above problems.
In order to solve the problems, the embodiment of the invention discloses a preparation method of a broadband heat-conducting wave-absorbing gasket, which comprises the following steps:
s1, preparing modified wave-absorbing powder by deionized water, a surfactant, an aluminum salt, a buffering agent, wave-absorbing powder, ammonia water and absolute ethyl alcohol according to a first preset procedure; specifically, S11, sequentially adding 0.1-2 parts of surfactant, 0.5-5 parts of aluminum salt and 0.5-2 parts of buffering agent into 100 parts of deionized water, adjusting the pH value to 6-7.5, and fully and uniformly stirring to obtain a uniform mixed solution; s12, adding 100-450 parts of wave absorbing powder and 100-600 parts of ammonia water with the concentration of 15% -30% into the uniform mixed solution, and performing ultrasonic dispersion for 0.5-1 h to obtain mixed slurry; s13, carrying out heat preservation and heating treatment on the mixed slurry for 3-5 hours to obtain wave-absorbing powder with a precursor coating on the surface; s141, carrying out suction filtration and washing on the wave-absorbing powder with the surface coated with the precursor for 2-3 times by using absolute ethyl alcohol to obtain filtered and washed wave-absorbing powder; s142, freeze-drying the filtered and washed wave-absorbing powder to obtain a freeze-dried wave-absorbing powder, and placing the cold-dried wave-absorbing powder in a tubular furnace; s143, placing the tube furnace in a magnetic field, and introducing nitrogen into the tube furnace, wherein the magnetic induction intensity of the magnetic field is 0.5-8T, and the nitrogen flow rate is 15-100 ml/min; s144, calcining the tube furnace at the high temperature of 800-1100 ℃ for 2-8 hours to obtain modified wave-absorbing powder;
s2, preparing a heat-conducting wave-absorbing gasket by using base glue, heat-conducting powder, a catalyst, a volatile solvent and the modified wave-absorbing powder according to a second preset program; specifically, S21, uniformly stirring 100-150 parts of vinyl polysiloxane, 5-50 parts of polydimethylsiloxane, 5-30 parts of hydrogen-containing silicone oil and 1-10 parts of inhibitor to obtain the base adhesive; s22, adding 150-750 parts of heat conduction powder and 150-450 parts of modified wave-absorbing powder into the base adhesive, and stirring and mixing for 0.5-2 hours in vacuum at a rotating speed of 300-2500 r/min to obtain a primary mixed material; wherein the heat conducting powder is aluminum oxide; s23, adding 0.5-5 parts of catalyst and 10-50 parts of volatile solvent into the preliminary mixed material, and stirring for 0.5h in vacuum at the rotating speed of 50-250 r/min to obtain a uniformly mixed material; s24, passing the uniformly mixed material through a curing conveying furnace with an additional directional magnetic field to obtain an oriented sheet type semi-finished product through a tape casting or calendering process; s25, drying and curing the sheet-shaped semi-finished product at 100-180 ℃ for 0.5-2 h to obtain the heat-conducting wave-absorbing gasket.
Further preferably, the mixed slurry is subjected to heat preservation and heating treatment for 3-5 hours to obtain the wave-absorbing powder with the surface coated with the precursor, and the method comprises the following steps:
s131, placing the mixed slurry into a reaction kettle;
s132, placing the reaction kettle into a baking oven at 50-100 ℃, and carrying out heat preservation and heating treatment for 3-5 hours;
s133, taking the reaction kettle out of the oven, and cooling to obtain the wave-absorbing powder with the precursor coating on the surface.
Further preferably, the step of passing the uniformly mixed material through a curing conveyer furnace with an additional directional magnetic field to obtain an oriented sheet type semi-finished product by a casting or calendering process comprises:
and (2) carrying out tape casting or calendaring process on the uniformly mixed material in a curing conveying furnace with an additional directional magnetic field to volatilize and cure the solvent in the uniformly mixed material for 0.25-2 h, and orderly arranging the easy magnetization axes of the modified wave-absorbing powder along the direction of the magnetic field to obtain an oriented sheet type semi-finished product, wherein the magnetic induction intensity of the magnetic field is 0.5-8T, and the temperature in the furnace chamber is set to be 50-80 ℃.
Further preferably, the surfactant is an amphiphilic polymer surfactant, specifically polyvinyl alcohol or polyvinylpyrrolidone or sodium polyvinylbenzene sulfonate.
Further preferably, the aluminum salt is aluminum sulfate and/or aluminum chloride and/or aluminum nitrate;
the aluminum content in the aluminum salt is 0.25-2.5% of the mass of the wave-absorbing filler.
Further preferably, the buffer comprises sodium acetate-acetic acid and/or phosphate.
The embodiment of the invention also discloses a broadband heat-conducting wave-absorbing gasket prepared by the preparation method based on any one of the above mentioned methods, which comprises the following components in parts by mass:
vinyl polysiloxane: 100-150 parts; polydimethylsiloxane: 5-50 parts; heat-conducting powder: 150-750 parts; modifying the wave-absorbing powder: 150-450 parts; volatile solvent (c): 10-50 parts; hydrogen-containing silicone oil: 5-30 parts of a solvent; inhibitor (B): 1-10 parts; catalyst: 0.5-5 parts.
More preferably, the vinyl polysiloxane is vinyl-terminated polydimethylsiloxane and/or methyl vinyl polysiloxane, wherein the viscosity of the vinyl polysiloxane is 200-600000 mPa.s.
Further preferably, the viscosity of the polydimethylsiloxane is 500-100000 mPa.s.
Further preferably, the particle size of the heat-conducting powder is 0.5-90 μm.
Preferably, the modified wave-absorbing powder is a wave-absorbing powder with the surface coated with alumina.
Preferably, the wave-absorbing powder comprises ferrosilicon powder and/or ferrosilicon-aluminum powder and/or ferronickel-molybdenum powder and/or permalloy powder and/or super permalloy powder; the particle size of the wave-absorbing powder is 0.5-60 mu m.
Further preferably, the volatile solvent comprises cyclomethicone and/or isoparaffin solvent oil and/or D40 environment-friendly solvent oil and/or D60 environment-friendly solvent oil and/or D80 environment-friendly solvent oil.
More preferably, the hydrogen-containing silicone oil is single-end hydrogen-containing silicone oil, wherein the active hydrogen content is 0.10-0.8%.
Further preferably, the inhibitor is 1-ethynyl-1-cyclohexanol, and the catalyst is a platinum complex.
The embodiment of the invention has the following advantages:
(1) according to the invention, the self-adhesive cured silicone oil is obtained by adjusting the curing ratio of the organosilicon polymer and the hydrogen-containing silicone oil, and after the heat-conducting and wave-absorbing filler is filled, the self-adhesive property of the heat-conducting wave-absorbing gasket is improved by adjusting the ratio of an organosilicon-based adhesive system and the matching of the particle size ratio of the filler types, and the cured silicone oil still has certain viscosity, so that the self-adhesive property can be effectively adhered to an electronic component without gum treatment, and the effects of reducing contact thermal resistance and keeping good heat-conducting wave-absorbing property can be realized only by curing the self-adhesive property of the cured silicone oil.
(2) According to the invention, through coating modification treatment on the wave-absorbing powder, the compatibility of the heat-conducting powder and the wave-absorbing powder in a silicone oil system can be obtained, the dispersibility is good, the mutual heat-conducting network formed by the wave-absorbing powder and the heat-conducting powder is ensured, and good filling and lapping of the heat-conducting filler and the wave-absorbing filler are realized through a directional orientation process, so that high absorption rate and good heat-conducting property on electromagnetic waves in a wide frequency band can be realized under low filling.
(3) According to the invention, by utilizing a directional orientation process, firstly, modified wave-absorbing powder with good directional effect is obtained by utilizing magnetic field heat treatment, meanwhile, a directional magnetic field is added in the calendaring and curing process, the viscosity of the semi-finished product is properly reduced by adding a volatile solvent, the magnetic powder can better overcome the constraint of a bonding system under the action of the magnetic field, certain rotation is generated under the action of magnetic field force, the semi-finished product is orderly arranged along the direction of an external magnetic field, and a sheet type semi-finished product with stable orientation is obtained through low-temperature semi-solidification treatment, so that the electromagnetic property of the prepared heat-conducting wave-absorbing gasket is greatly improved.
(4) The heat-conducting wave-absorbing gasket has higher shielding efficiency and long-term high and low temperature aging resistance, and the heat conductivity and the magnetic conductivity of the gasket are not obviously reduced after long-term high and low temperature aging. The broadband heat conduction and wave absorption gasket prepared by the invention has the advantages that the heat conduction coefficient and the magnetic conductivity are reduced less than 10% in a high-low temperature aging test for 500h, and the broadband heat conduction and wave absorption gasket has good aging resistance. The heat-conducting wave-absorbing gasket has low hardness (the hardness is less than or equal to 55shore 00) and excellent mechanical property, and can meet and adapt to the high requirements of the new generation of 5G electronic products.
Drawings
FIG. 1 is a flowchart illustrating steps of an embodiment of a method for manufacturing a broadband heat-conducting wave-absorbing gasket according to the present invention;
FIG. 2 is a flow chart of sub-steps of step S1 in FIG. 1;
fig. 3 is a flow chart of sub-steps of step S2 in fig. 1.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The hardness described herein is shore hardness, or also referred to as shore hardness, which may be designated shore O or shore OO or shore 00 or shore OO; the unit T of the magnetic induction of the magnetic field is (Tesla ), other known units, and the description in the scheme is not provided.
One of the core ideas of the embodiment of the invention is that self-adhesive cured silicone oil is obtained by adjusting the curing ratio of the organosilicon polymer and the hydrogen-containing silicone oil, and after the heat-conducting and wave-absorbing filler is filled, the self-adhesive property of the heat-conducting wave-absorbing gasket is improved by adjusting the ratio of an organosilicon-based adhesive system and the matching of the particle size ratio of the filler types, and the cured silicone oil still has certain viscosity, does not need gum treatment, can be effectively adhered to an electronic component only by curing the self viscosity of the cured silicone oil, realizes the reduction of contact thermal resistance, and keeps good heat-conducting and wave-absorbing properties. The compatibility of the heat-conducting powder and the wave-absorbing powder in a silicone oil system can be obtained through the coating modification treatment of the wave-absorbing powder, the dispersibility is good, the wave-absorbing powder and the heat-conducting powder are ensured to form an intercommunicated heat-conducting network, and the heat-conducting filler and the wave-absorbing filler are well filled and lapped through a directional orientation process, so that the high absorption rate and the good heat-conducting property to electromagnetic waves in a wide frequency band can be realized under the condition of low filling. By utilizing a directional orientation process, firstly, magnetic field heat treatment is utilized to obtain modified wave-absorbing powder with good directional effect, a directional magnetic field is added in the calendering and curing process, the viscosity of the semi-finished product is properly reduced by adding a volatile solvent, the magnetic powder can better overcome the constraint of a bonding system under the action of the magnetic field, certain rotation is carried out under the action of magnetic field force, the semi-finished product is orderly arranged along the direction of an external magnetic field, and a stably oriented sheet type semi-finished product is obtained through low-temperature semi-curing treatment, so that the electromagnetic performance of the prepared heat-conducting wave-absorbing gasket is greatly improved.
The embodiment discloses a broadband heat-conducting wave-absorbing gasket which comprises the following components in parts by mass:
vinyl polysiloxane: 100-150 parts; polydimethylsiloxane: 5-50 parts; heat-conducting powder: 150-750 parts; modifying the wave-absorbing powder: 150-450 parts; volatile solvent (c): 10-50 parts; hydrogen-containing silicone oil: 5-30 parts; inhibitor (B): 1-10 parts; catalyst: 0.5-5 parts.
More preferably, the vinyl polysiloxane is vinyl-terminated polydimethylsiloxane and/or methyl vinyl polysiloxane, wherein the viscosity of the vinyl polysiloxane is 200-600000 mPa.s.
More preferably, the viscosity of the vinyl polysiloxane is 200 to 100000 mpa.s.
Further preferably, the viscosity of the polydimethylsiloxane is 500-100000 mPa.s.
More preferably, the polydimethylsiloxane is preferably methyl-terminated dimethyl polysiloxane, and the viscosity is 1000-20000 mPa.s.
Further preferably, the heat conducting powder is a heat conducting filler composed of aluminum oxide and/or zinc oxide and/or boron nitride, or a heat conducting filler composed of aluminum oxide and/or zinc oxide and/or aluminum nitride; the particle size of the heat-conducting filler is 0.5-90 μm.
Preferably, the modified wave-absorbing powder is a wave-absorbing powder with the surface coated with alumina.
Further preferably, the wave-absorbing powder comprises ferrosilicon powder and/or ferrosilicon-aluminum powder and/or ferronickel-molybdenum powder and/or permalloy powder and/or ultra permalloy powder; the particle size of the wave-absorbing powder is 0.5-60 mu m.
Further preferably, the wave-absorbing powder preferably has a particle size of 5-45 μm.
Further preferably, the volatile solvent comprises cyclomethicone and/or isoparaffin solvent oil and/or D40 environment-friendly solvent oil and/or D60 environment-friendly solvent oil and/or D80 environment-friendly solvent oil. Further preferably, the cyclomethicone is a pentameric and/or a hexameric cyclomethicone.
More preferably, the hydrogen-containing silicone oil is single-end hydrogen-containing silicone oil, wherein the active hydrogen content is 0.10-0.8%.
Further preferably, the inhibitor is 1-ethynyl-1-cyclohexanol, and the catalyst is a platinum complex.
Referring to fig. 1, a flowchart illustrating steps of an embodiment of a method for manufacturing a broadband heat-conducting wave-absorbing gasket of the present invention is shown, which may specifically include the following steps:
s1, preparing modified wave-absorbing powder by deionized water, a surfactant, an aluminum salt, a buffering agent, wave-absorbing powder, ammonia water and absolute ethyl alcohol according to a first preset procedure;
and S2, preparing the heat-conducting wave-absorbing gasket according to a second preset program by using the base adhesive, the heat-conducting powder, the catalyst, the volatile solvent and the modified wave-absorbing powder.
Further preferably, as shown in fig. 2, the modified wave-absorbing powder is prepared by deionized water, a surfactant, an aluminum salt, a buffer, wave-absorbing powder, ammonia water and absolute ethyl alcohol according to a first preset procedure, and comprises the following steps:
s11, sequentially adding 0.1-2 parts of surfactant, 0.5-5 parts of aluminum salt and 0.5-2 parts of buffering agent into 100 parts of deionized water, adjusting the pH value to 6-7.5, and fully and uniformly stirring to obtain a uniform mixed solution;
s12, adding 100-450 parts of wave absorbing powder and 100-600 parts of ammonia water with the concentration of 15% -30% into the uniform mixed solution, and performing ultrasonic dispersion for 0.5-1 h to obtain mixed slurry;
s13, carrying out heat preservation and heating treatment on the mixed slurry for 3-5 h to obtain wave-absorbing powder with a precursor coating on the surface;
and S14, treating the wave-absorbing powder coated with the precursor on the surface by absolute ethyl alcohol and nitrogen according to a third preset program to obtain the modified wave-absorbing powder.
Preferably, as shown in fig. 3, the heat-conducting wave-absorbing gasket is prepared by base glue, heat-conducting powder, catalyst, volatile solvent and the modified wave-absorbing powder according to a second preset program, and includes the following steps:
s21, blending the base rubber: uniformly stirring 100-150 parts of vinyl polysiloxane, 5-50 parts of polydimethylsiloxane, 5-30 parts of hydrogen-containing silicone oil and 1-10 parts of inhibitor to obtain the base adhesive;
s22, mixing materials: adding 150-750 parts of heat conducting powder and 150-450 parts of modified wave absorbing powder into the base adhesive, and stirring and mixing for 0.5-2 hours in vacuum at the rotating speed of 300-2500 r/min to obtain a preliminary mixed material;
s23, adding 0.5-5 parts of catalyst and 10-50 parts of volatile solvent into the preliminary mixture, and stirring for 0.5h in vacuum at the rotating speed of 50-250 r/min to obtain a uniformly mixed material;
s24, orientation: the uniformly mixed materials pass through a curing conveying furnace with an additional directional magnetic field to obtain an oriented sheet type semi-finished product by a tape casting or calendering process;
s25, curing: and drying and curing the sheet-type semi-finished product at 100-180 ℃ for 0.5-2 h to obtain the heat-conducting wave-absorbing gasket.
Further preferably, the mixed slurry is subjected to heat preservation and heating treatment for 3-5 hours to obtain the wave-absorbing powder with the surface coated with the precursor, and the method comprises the following steps:
s131, placing the mixed slurry into a reaction kettle;
s132, placing the reaction kettle into an oven at the temperature of 50-100 ℃, and carrying out heat preservation and heating treatment for 3-5 hours;
s133, taking the reaction kettle out of the oven, and cooling to obtain the wave-absorbing powder with the precursor coating on the surface.
Preferably, the microwave absorbing powder coated with the precursor on the surface is processed by absolute ethyl alcohol and nitrogen according to a third preset program to obtain modified microwave absorbing powder, and the method comprises the following steps:
s141, carrying out suction filtration and washing on the wave-absorbing powder with the surface coated with the precursor for 2-3 times by using absolute ethyl alcohol to obtain filtered and washed wave-absorbing powder;
s142, freeze-drying the filtered and washed wave-absorbing powder to obtain dry wave-absorbing powder, and placing the dry wave-absorbing powder in a tubular furnace;
s143, placing the tube furnace in a magnetic field, and introducing nitrogen into the tube furnace, wherein the magnetic induction intensity of the magnetic field is 0.5-8T, and the nitrogen flow rate is 15-100 ml/min;
s144, calcining the tube furnace at the high temperature of 800-1100 ℃ for 2-8 hours to obtain the modified wave-absorbing powder.
Further preferably, the step of passing the uniformly mixed material through a curing conveyer furnace with an additional directional magnetic field to obtain an oriented sheet type semi-finished product by a casting or calendaring process comprises:
and (2) carrying out tape casting or calendaring process on the uniformly mixed material by a curing conveying furnace with an additional directional magnetic field to volatilize and cure the solvent in the uniformly mixed material for 0.25-2 h, and orderly arranging the easy magnetization axes of the modified wave-absorbing powder along the direction of the magnetic field to obtain an oriented sheet type semi-finished product, wherein the magnetic induction intensity of the magnetic field is 0.5-8T, and the temperature in the furnace chamber is set to be 50-80 ℃.
Further preferably, the surfactant is an amphiphilic polymer surfactant, preferably polyvinyl alcohol, polyvinylpyrrolidone, and sodium polyvinylbenzenesulfonate.
Further preferably, the aluminum salt is one or two or more of aluminum sulfate, aluminum chloride and aluminum nitrate; the content of aluminum in the aluminum salt is 0.25-2.5% of the mass of the wave-absorbing filler.
Further preferably, the buffer is one or two of sodium acetate-acetic acid and phosphate.
The materials used for the examples of the invention and the comparative examples are as follows:
a represents a vinyl polysiloxane, A-1 is a vinyl-terminated polydimethylsiloxane having a viscosity of 2000mPa.s, and A-2 is a methyl vinyl polysiloxane having a viscosity of 10000 mPa.s.
B represents polydimethylsiloxane, and B-1 is methyl-terminated dimethylpolysiloxane having a viscosity of 10000 mPa.s.
C represents heat-conducting powder, C-1 is alumina, and the particle size is 90 μm; c-2 is alumina with a particle size of 10 μm.
D represents wave-absorbing powder, D-1 is ferrum-silicon-aluminum powder, and the particle size is 35 mu m; d-2 is ferrum-silicon-aluminum powder with the grain diameter of 5 mu m.
E represents volatile silicone oil, and E-1 is cyclomethicone mainly composed of pentamer and hexamer.
F represents single-end hydrogen-containing silicone oil, and the active hydrogen content is 0.16 percent.
G represents 1-ethynyl-1-cyclohexanol.
H represents a platinum-gold complex catalyst.
I represents deionized water.
J represents a surfactant, and J-1 represents polyvinylpyrrolidone (PVP).
K represents an aluminum salt, and K-1 represents aluminum sulfate.
L represents a buffer, and L-1 represents sodium acetate-acetic acid.
M represents ammonia water, and M-1 represents 28% ammonia water.
Table 1: formula components for preparing modified wave-absorbing powder
As in table 1 above: w-1 and W-2 are modified wave-absorbing powder prepared from normal components, and W-3 is modified wave-absorbing powder prepared without aluminum salt coating.
In the example of W-1, the wave-absorbing powder consisting of 100 parts of sendust powder with the particle size of 35 microns and 20 parts of sendust powder with the particle size of 5 microns is used; 100 parts of deionized water; the surfactant is 0.25 part of polyvinylpyrrolidone; aluminum salt is 0.5 part of aluminum sulfate; the buffer is sodium acetate-acetic acid 0.6 part; 150 parts of 28% ammonia water; the conditions of the reaction kettle are as follows: the temperature is 80 ℃, and the reaction time is 3 hours; the high-temperature calcination conditions are as follows: the temperature is 1000 ℃, and the calcining time is 2 hours; setting the magnetic induction intensity of the external magnetic field as 2T; and nitrogen flow rate in the preparation equipment is 50ml/min, and the modified wave-absorbing powder is prepared.
In the W-2 example, the wave-absorbing powder consisting of 350 parts of sendust powder with the particle size of 35 microns and 100 parts of sendust powder with the particle size of 5 microns is used; 100 parts of deionized water; the surfactant is 0.5 part of polyvinylpyrrolidone; the aluminum salt is 2 parts of aluminum sulfate; the buffer is sodium acetate-acetic acid 1.2 parts; 250 parts of 28% ammonia water; the conditions of the reaction kettle are as follows: the temperature is 80 ℃, and the reaction time is 5 hours; the high-temperature calcination conditions are as follows: the temperature is 1000 ℃, and the calcining time is 5 hours; setting the magnetic induction intensity of the external magnetic field to be 8T; and nitrogen flow rate in the preparation equipment is 50ml/min, and the modified wave-absorbing powder is prepared.
In the example of W-3, the wave-absorbing powder consisting of 100 parts of sendust powder with the particle size of 35 microns and 20 parts of sendust powder with the particle size of 5 microns is used; 100 parts of deionized water; the surfactant is 0.25 part of polyvinylpyrrolidone; the buffer is sodium acetate-acetic acid 0.6 part; 150 parts of 28% ammonia water; the conditions of the reaction kettle are as follows: the temperature is 80 ℃, and the reaction time is 3 hours; the high-temperature calcination conditions are as follows: the temperature is 1000 ℃, and the calcining time is 2 hours; the modified wave-absorbing powder is prepared without aluminum salt coating, external magnetic field and nitrogen in the preparation equipment.
Table 2: formula component table for preparing heat-conducting wave-absorbing gasket
As shown in table 2 above: examples 1 and 2 are thermally conductive and wave absorbing gaskets prepared from normal components; the comparative example 1-1 is a heat-conducting wave-absorbing gasket prepared by the wave-absorbing powder without coating modification; the comparative example 1-2 is a heat conduction wave absorption gasket prepared without applying a magnetic field; comparative examples 1-3 are heat-conducting and wave-absorbing gaskets prepared without adding a volatile solvent.
In example 1, 100 parts of a vinyl-terminated polydimethylsiloxane having a viscosity of 2000mpa.s was selected as the vinyl polysiloxane; 50 parts of methyl-terminated dimethyl polysiloxane with the viscosity of 10000mPa.s is selected as the polydimethylsiloxane; 450 parts of alumina with the grain diameter of 90 mu m and 150 parts of alumina with the grain diameter of 10 mu m are selected as the heat-conducting powder; volatile silicone oil is selected from 20 parts of cyclomethicone mainly comprising pentamer and hexamer; 10 parts of single-end hydrogen-containing silicone oil with active hydrogen content of 0.16 percent is selected; selecting 2.5 parts of 1-ethynyl-1-cyclohexanol; 1.5 parts of platinum complex catalyst is selected; and selecting 250 parts of the modified wave-absorbing powder prepared in the W-1 example; and applying a directional magnetic field to prepare the heat-conducting wave-absorbing gasket.
In example 2, 150 parts of methylvinylpolysiloxane having a viscosity of 10000mpa.s was used as the vinylpolysiloxane; 50 parts of methyl terminated dimethyl polysiloxane with the viscosity of 10000mPa.s is selected as the polydimethylsiloxane; 350 parts of alumina with the grain diameter of 90 mu m and 200 parts of alumina with the grain diameter of 10 mu m are selected as the heat-conducting powder; volatile silicone oil is selected from 50 parts of cyclomethicone mainly comprising pentamer and hexamer; selecting 8 parts of single-end hydrogen-containing silicone oil with active hydrogen content of 0.16 percent; selecting 2.5 parts of 1-ethynyl-1-cyclohexanol; 1.5 parts of platinum complex catalyst is selected; 300 parts of modified wave-absorbing powder prepared in the W-2 example; and applying a directional magnetic field to prepare the heat-conducting wave-absorbing gasket.
In comparative example 1-1, 100 parts of a double-terminal vinyl polydimethylsiloxane having a viscosity of 2000mpa.s was selected as the vinyl polysiloxane; 50 parts of methyl terminated dimethyl polysiloxane with the viscosity of 10000mPa.s is selected as the polydimethylsiloxane; 450 parts of alumina with the grain diameter of 90 mu m and 150 parts of alumina with the grain diameter of 10 mu m are selected as the heat-conducting powder; volatile silicone oil is selected from 20 parts of cyclomethicone mainly comprising pentamer and hexamer; 10 parts of single-end hydrogen-containing silicone oil with active hydrogen content of 0.16 percent is selected; selecting 2.5 parts of 1-ethynyl-1-cyclohexanol; 1.5 parts of platinum complex catalyst is selected; and selecting 250 parts of the modified wave-absorbing powder prepared in the W-3 example; and applying a directional magnetic field to prepare the heat-conducting wave-absorbing gasket.
In comparative example 1-2, 150 parts of methyl vinyl silicone having a viscosity of 10000mPa.s was selected as the vinyl silicone; 50 parts of methyl-terminated dimethyl polysiloxane with the viscosity of 10000mPa.s is selected as the polydimethylsiloxane; 350 parts of alumina with the grain diameter of 90 mu m and 200 parts of alumina with the grain diameter of 10 mu m are selected as the heat-conducting powder; volatile silicone oil is selected from 5 parts of cyclomethicone mainly comprising pentamer and hexamer; 8 parts of single-end hydrogen-containing silicone oil with active hydrogen content of 0.16 percent is selected; selecting 2.5 parts of 1-ethynyl-1-cyclohexanol; 1.5 parts of platinum complex catalyst is selected; 300 parts of modified wave-absorbing powder prepared in the W-2 example; and (4) preparing the heat-conducting wave-absorbing gasket without applying a directional magnetic field.
In comparative examples 1 to 3, 100 parts of a vinyl-terminated polydimethylsiloxane having a viscosity of 2000mpa.s was selected as the vinyl-terminated polysiloxane; 50 parts of methyl-terminated dimethyl polysiloxane with the viscosity of 10000mPa.s is selected as the polydimethylsiloxane; 450 parts of alumina with the grain diameter of 90 mu m and 150 parts of alumina with the grain diameter of 10 mu m are selected as the heat-conducting powder; no volatile agent (volatile silicone oil in this example) is selected; 10 parts of single-end hydrogen-containing silicone oil with active hydrogen content of 0.16 percent is selected; selecting 2.5 parts of 1-ethynyl-1-cyclohexanol; 1.5 parts of platinum complex catalyst is selected; and selecting 250 parts of the modified wave-absorbing powder prepared in the W-1 example; and applying a directional magnetic field to prepare the heat-conducting wave-absorbing gasket.
The properties of the heat-conductive and wave-absorbing gasket manufactured by example 1, example 2, comparative example 1-1, comparative example 1-2, and comparative example 1-3 are shown in table 3.
Table 3: performance index of heat-conducting wave-absorbing gasket
In table 3 above: the aging test conditions were: high and low temperature tests (-40-140 ℃, 500h namely-40 ℃/15min, 140 ℃/15min, heating up to-15 min, cooling down to-15 min, 1h/cycle, 500 cycle).
According to the table 3, as shown by comparing various performance indexes of the heat-conducting wave-absorbing gasket prepared in the example 1 with those prepared in the comparative example 1-1, through the coating modification treatment of the wave-absorbing powder, the heat-conducting powder and the wave-absorbing powder have good compatibility and dispersibility in a silicone oil system, and the wave-absorbing powder and the heat-conducting powder form an intercommunicated heat-conducting network, and through the directional orientation process, the heat-conducting powder and the wave-absorbing powder are ensured to be well filled and lapped, and under the condition of low filling, the heat-conducting wave-absorbing gasket can realize high absorption rate and good heat-conducting performance to electromagnetic waves in a wider frequency band.
According to table 3, as can be seen from comparison of various performance indexes of the heat-conducting wave-absorbing gasket prepared in example 1 and comparative examples 1-3, the viscosity of the semi-finished product is properly reduced by adding the volatile solvent, so that the magnetic powder can better overcome the constraint of a bonding system under the action of a magnetic field, certain rotation is generated under the action of magnetic field force, the semi-finished product is orderly arranged along the direction of an external magnetic field, and the stable-oriented sheet-type semi-finished product is obtained through low-temperature semi-solidification treatment, so that the electromagnetic performance and the mechanical performance of the prepared heat-conducting wave-absorbing gasket are greatly improved.
According to the comparison of various performance indexes of the heat-conducting wave-absorbing gasket prepared in the middle example 2 and the comparative examples 1-2 shown in the table 3, the modified wave-absorbing powder with good orientation effect is obtained by utilizing the oriented orientation process, and meanwhile, the oriented magnetic field is added in the calendering and curing process to obtain the sheet-type semi-finished product with stable orientation, so that the electromagnetic performance of the prepared heat-conducting wave-absorbing gasket is greatly improved. The heat-conducting wave-absorbing gasket has higher shielding efficiency and long-term high and low temperature aging resistance, and the heat conductivity and the magnetic conductivity have unobvious changes after long-term high and low temperature aging.
It should be noted that, for simplicity of description, the method embodiments are described as a series of acts or combination of acts, but those skilled in the art will recognize that the present invention is not limited by the illustrated order of acts, as some steps may occur in other orders or concurrently in accordance with the embodiments of the present invention. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the invention.
The embodiments in the present specification are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or terminal that comprises the element.
The broadband heat-conducting wave-absorbing gasket and the preparation method thereof provided by the invention are introduced in detail, the principle and the implementation mode of the invention are explained by applying specific examples, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (13)
1. A preparation method of a broadband heat-conducting wave-absorbing gasket is characterized by comprising the following steps:
s1, preparing modified wave-absorbing powder by deionized water, a surfactant, an aluminum salt, a buffering agent, wave-absorbing powder, ammonia water and absolute ethyl alcohol according to a first preset procedure; specifically, S11, sequentially adding 0.1-2 parts of surfactant, 0.5-5 parts of aluminum salt and 0.5-2 parts of buffering agent into 100 parts of deionized water, adjusting the pH value to 6-7.5, and fully and uniformly stirring to obtain a uniform mixed solution; wherein the aluminum salt is one or more of aluminum sulfate, aluminum chloride and aluminum nitrate; the aluminum content in the aluminum salt is 0.25 to 2.5 percent of the mass of the wave-absorbing filler; s12, adding 100-450 parts of wave absorbing powder and 100-600 parts of ammonia water with the concentration of 15% -30% into the uniform mixed solution, and performing ultrasonic dispersion for 0.5-1 h to obtain mixed slurry; s13, carrying out heat preservation and heating treatment on the mixed slurry for 3-5 h to obtain wave-absorbing powder with a precursor coating on the surface; s141, carrying out suction filtration and washing on the wave-absorbing powder with the surface coated with the precursor for 2-3 times by using absolute ethyl alcohol to obtain filtered and washed wave-absorbing powder; s142, freeze-drying the filtered and washed wave-absorbing powder to obtain a freeze-dried wave-absorbing powder, and placing the cold-dried wave-absorbing powder in a tubular furnace; s143, placing the tube furnace in a magnetic field, and introducing nitrogen into the tube furnace, wherein the magnetic induction intensity of the magnetic field is 0.5-8T, and the flow rate of the nitrogen is 15-100 ml/min; s144, calcining the tube furnace at the high temperature of 800-1100 ℃ for 2-8 hours to obtain modified wave-absorbing powder;
s2, preparing a heat-conducting wave-absorbing gasket by using base glue, heat-conducting powder, a catalyst, a volatile solvent and the modified wave-absorbing powder according to a second preset program; specifically, S21, uniformly stirring 100-150 parts of vinyl polysiloxane, 5-50 parts of polydimethylsiloxane, 5-30 parts of hydrogen-containing silicone oil and 1-10 parts of an inhibitor to obtain the base adhesive; s22, adding 150-750 parts of heat conducting powder and 150-450 parts of modified wave absorbing powder into the base adhesive, and stirring and mixing for 0.5-2 hours in vacuum at the rotating speed of 300-2500 r/min to obtain a primary mixed material; wherein the heat conducting powder is aluminum oxide; s23, adding 0.5-5 parts of catalyst and 10-50 parts of volatile solvent into the preliminary mixed material, and stirring for 0.5h in vacuum at the rotating speed of 50-250 r/min to obtain a uniformly mixed material; wherein the volatile solvent is cyclomethicone; s24, passing the uniformly mixed material through a curing conveying furnace with an additional directional magnetic field to obtain an oriented sheet type semi-finished product through a tape casting or calendering process; s25, drying and curing the sheet-shaped semi-finished product at 100-180 ℃ for 0.5-2 h to obtain the heat-conducting wave-absorbing gasket.
2. The preparation method of the broadband heat-conducting wave-absorbing gasket according to claim 1, wherein the mixed slurry is subjected to heat preservation and heating treatment for 3-5 hours to obtain the wave-absorbing powder with the surface coated with the precursor, and the method comprises the following steps:
s131, placing the mixed slurry into a reaction kettle;
s132, placing the reaction kettle into a baking oven at 50-100 ℃, and carrying out heat preservation and heating treatment for 3-5 hours;
s133, taking the reaction kettle out of the oven, and cooling to obtain the wave-absorbing powder with the precursor coating on the surface.
3. The method for preparing the broadband heat-conducting wave-absorbing gasket according to claim 1, wherein the step of obtaining the oriented sheet-type semi-finished product by casting or calendaring the uniformly mixed material through a curing and conveying furnace with an additional directional magnetic field comprises the following steps:
and (2) carrying out tape casting or calendaring process on the uniformly mixed material in a curing conveying furnace with an additional directional magnetic field to volatilize and cure the solvent in the uniformly mixed material for 0.25-2 h, and orderly arranging the easy magnetization axes of the modified wave-absorbing powder along the direction of the magnetic field to obtain an oriented sheet type semi-finished product, wherein the magnetic induction intensity of the magnetic field is 0.5-8T, and the temperature in the furnace chamber is set to be 50-80 ℃.
4. The method for preparing a broadband heat-conducting wave-absorbing gasket according to claim 1, wherein the surfactant is an amphiphilic polymer surfactant, specifically polyvinyl alcohol or polyvinylpyrrolidone or sodium polyvinylbenzene sulfonate.
5. The method for preparing a broadband heat-conducting and wave-absorbing gasket according to claim 1, wherein the buffer comprises one or both of sodium acetate-acetic acid and phosphate.
6. A broadband heat-conducting wave-absorbing gasket prepared by the preparation method of the broadband heat-conducting wave-absorbing gasket according to any one of claims 1 to 5 is characterized by comprising the following components in parts by mass:
vinyl polysiloxane: 100-150 parts; polydimethylsiloxane: 5-50 parts; heat-conducting powder: 150-750 parts; modifying the wave-absorbing powder: 150-450 parts; volatile solvent (c): 10-50 parts; hydrogen-containing silicone oil: 5-30 parts of a solvent; inhibitor (B): 1-10 parts; catalyst: 0.5-5 parts.
7. The broadband heat-conducting wave-absorbing gasket according to claim 6, wherein the vinyl polysiloxane is one or two of vinyl-terminated polydimethylsiloxane and methyl vinyl polysiloxane, and the viscosity of the vinyl polysiloxane is 200-600000 mPa.s.
8. The broadband heat-conducting wave-absorbing gasket as claimed in claim 6, wherein the viscosity of the polydimethylsiloxane is 500-100000 mPa.s.
9. The broadband heat-conducting wave-absorbing gasket as claimed in claim 6, wherein the particle size of the heat-conducting powder is 0.5-90 μm.
10. The broadband heat-conducting wave-absorbing gasket of claim 6, wherein the modified wave-absorbing powder is a wave-absorbing powder with a surface coated with alumina.
11. The broadband heat-conducting wave-absorbing gasket of claim 10, wherein the wave-absorbing powder comprises one or more of ferrosilicon powder, ferrosilicon aluminum powder, ferronickel molybdenum powder, permalloy powder and super permalloy powder; the particle size of the wave-absorbing powder is 0.5-60 mu m.
12. The broadband heat-conducting wave-absorbing gasket of claim 6, wherein the hydrogen-containing silicone oil is single-ended hydrogen-containing silicone oil, and active hydrogen content is 0.10-0.8%.
13. The broadband thermally conductive and microwave absorbing gasket of claim 6, wherein the inhibitor is 1-ethynyl-1-cyclohexanol, and the catalyst is platinum complex.
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| CN112980398A (en) * | 2021-02-24 | 2021-06-18 | 天津泽希新材料有限公司 | High-thermal-conductivity wave-absorbing silica gel gasket and preparation method thereof |
| CN113214638B (en) * | 2021-05-27 | 2022-04-22 | 湖南飞鸿达新材料有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
| CN113249031B (en) * | 2021-06-07 | 2022-06-28 | 宁波晶飞新材料有限公司 | High-thermal-conductivity silica gel wave absorbing plate and preparation method thereof |
| CN114105529B (en) * | 2021-11-17 | 2023-08-29 | 深圳市鸿富诚新材料股份有限公司 | High-heat-conductivity wave-absorbing composite material, preparation method thereof and wave-absorbing heat-conducting gasket |
| CN114231039A (en) * | 2021-12-27 | 2022-03-25 | 东莞市博恩复合材料有限公司 | Heat-conducting wave-absorbing gasket and preparation method thereof |
| CN114479476A (en) * | 2022-02-23 | 2022-05-13 | 深圳先进电子材料国际创新研究院 | Wide-frequency-band wide-temperature-range high-damping heat-conducting gel and preparation method and application thereof |
| CN114539778B (en) * | 2022-02-23 | 2022-10-28 | 深圳市锐扬创科技术股份有限公司 | Heat-conducting wave-absorbing nanoscale functional composite material applied to high-wide frequency spectrum and preparation method thereof |
| CN114940827B (en) * | 2022-06-15 | 2023-07-25 | 深圳市德弘电子材料有限公司 | Heat-conducting wave-absorbing cement and preparation method thereof |
| CN117264420A (en) * | 2022-07-23 | 2023-12-22 | 苏州汇美包装制品有限公司 | Heat-conducting wave-absorbing gasket material |
| CN115746362B (en) * | 2022-09-09 | 2023-07-14 | 东莞市零度导热材料有限公司 | Wave-absorbing heat-conducting sheet and preparation method thereof |
| CN116333498B (en) * | 2022-11-23 | 2024-07-16 | 四川天邑康和通信股份有限公司 | High-heat-conductivity wave-absorbing gasket and preparation method thereof |
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