CN110668735A - Thermosetting high-temperature-resistant microwave dielectric composite material and preparation method thereof - Google Patents
Thermosetting high-temperature-resistant microwave dielectric composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of organic/inorganic composite materials, and particularly relates to a thermosetting high-temperature-resistant microwave dielectric composite material and a preparation method thereof. The thermosetting high-temperature-resistant microwave medium composite material comprises the material components of ceramic powder and thermosetting silylene resin with low viscosity; the ceramic powder is as follows: the mass percentage ratio of the silylene resin is 80:20, the general formula of the ceramic powder is as follows: 0.5MgTiO3‑0.5(Ca0.5Nd0.3)TiO3Or SrTiO3. The thermosetting resin adopts linear silylyne resin, branched silylyne resin and star silylyne resin, and a body casting technology is adopted to prepare the composite material substrate. The composite material substrate has the advantages of high dielectric constant, low dielectric loss, adjustable heat resistance and dielectric constant, simple preparation process and the like.
Description
Technical Field
The invention belongs to the field of organic/inorganic composite materials, in particular to a thermosetting high-temperature-resistant microwave dielectric composite material and a preparation method thereof,
background
In recent years, as the ceramic-filled polymer-based composite material has excellent comprehensive performance, combines the mechanical flexibility and the processability of a polymer matrix and has outstanding dielectric properties of ceramic, the ceramic-filled polymer-based composite material has attracted great attention of researchers in the fields of electronic packaging, 5G mobile communication, high-capacity satellites, wearable electronic products and the like as a most important functional material. These fields require devices having fast and stable information processing capabilities, and thus require miniaturization of electronic components and high integrity of circuit signal transmission. The high dielectric constant is beneficial to reducing the size of the embedded device so as to reduce the size of a chip, the low dielectric loss is beneficial to improving the signal transmission integrity of the device, and the heat dissipation design is simplified. The resins used in the microwave dielectric composite materials at present are mostly thermoplastic resins, such as: polytetrafluoroethylene, polyphenylene oxide, polyphenylene sulfide, and the like. The use temperature of composite substrates prepared with thermoplastic resins is typically below 400 ℃. Therefore, the development of a microwave dielectric composite material with high dielectric constant, low dielectric loss and high temperature resistance is of great significance in reducing the volume of electronic components, improving the integrity of signal transmission and improving the service temperature of a substrate.
The silicon-eneyne resin (PSAE) is very suitable as a substrate for a substrate material in a high-frequency and high-speed field due to its excellent properties such as high temperature resistance, low loss, low viscosity, and stable broadband dielectric properties. In particular, the resin has low viscosity, and the viscosity can be adjusted by the temperature and the prepolymerization time, so that the preparation of the composite material is very favorable. When the resin viscosity is low, the resin and the ceramic powder are fully mixed, the viscosity of the mixture is increased to a certain degree by a pre-polymerization mode after the mixture is uniformly mixed, and then the body casting is carried out, so that the ceramic powder is uniformly dispersed in a resin matrix. However, the resin also has some disadvantages such as a low dielectric constant of the resin. Therefore, in order to increase the dielectric constant, we use the recombination effect to increase the dielectric constant by compounding a ceramic material having a high dielectric constant, a low dielectric loss, and a low thermal expansion coefficient in the PSEA resin, and further decrease the thermal expansion coefficient, fusing the excellent characteristics of the polymer and the conventional microwave ceramic. In the eighties of the last century, the united states rogers first proposed a substrate technology of composite glass fiber cloth or ceramic with polytetrafluoroethylene as a matrix, and has already achieved many applications in the field of high-frequency microwave circuits.
The chinese patent with application number 201510136815.7 provides a method for preparing a microwave dielectric ceramic/resin bicontinuous composite material for a PCB substrate. The preparation method comprises the steps of adding a dispersing agent and a binder into ceramic powder to prepare a porous ceramic green body, preserving the heat of the porous ceramic green body at high temperature to prepare a microwave ceramic dielectric prefabricated body, pouring bisphenol A type cyanate ester resin into a mold, placing the prefabricated body on the resin, performing post-curing, cooling along with a furnace, and demolding to obtain the microwave dielectric ceramic/resin bicontinuous composite material for the PCB substrate. The dielectric constant of the microwave dielectric ceramic/resin bicontinuous composite material for the PCB substrate provided by the technology is 17.5, but the preparation process provided by the technology is complicated, and more additional components (dispersing agent, binder and the like) are required to be added.
The Chinese patent with the application number of 201710700372.9 provides a polytetrafluoroethylene-ceramic composite material and a preparation method thereof. The raw materials are mixed, ball-milled, dried, calcined and screened to obtain a ceramic material, and the ceramic powder is treated by a coupling agent to obtain modified ceramic powder. And performing ball milling and mixing on the modified ceramic powder and polytetrafluoroethylene, performing emulsion breaking to obtain dough, and molding, hot-pressing and sintering the dough to obtain the polytetrafluoroethylene-ceramic composite medium substrate. The dielectric constant of the polytetrafluoroethylene-ceramic composite material prepared by the method provided by the technology is (12.5), the dielectric loss is (2.05E-03), the thermal expansion coefficient is 19.8 ppm/DEG C, the thermal expansion coefficient is larger, the preparation method adopted by the patent needs the working procedures of ball milling, rotary calendering and the like, the subsequent curing temperature is higher, the curing time is longer (250-300 ℃ and 20 hours), the preparation working procedure is more complicated, and the industrial production is not facilitated.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-temperature-resistant microwave dielectric silylyne resin-ceramic composite material substrate with high dielectric constant, low dielectric loss and low expansion and a preparation method thereof, so that a thermosetting microwave composite material substrate with adjustable heat resistance and adjustable dielectric constant is obtained while high dielectric constant, low dielectric loss, low thermal expansion coefficient and high heat resistance are obtained, a body pouring technology is adopted, the process is simple, raw materials only need to be compounded by resin and ceramic powder, solvents and other diluents or binders do not need to be added, and the method is easy for industrial production.
The technical scheme of the invention is as follows:
a thermosetting high temperature resistant microwave medium composite material comprises ceramic powder and thermosetting silylene alkyne resin with low viscosity; the ceramic powder is as follows: the mass percentage ratio of the silylene resin is 80:20, the general formula of the ceramic powder is as follows: 0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3Or SrTiO3。
Further, the low-viscosity thermosetting silylene resin is linear silylene resin, branched silylene resin or star silylene resin.
Still further, the low viscosity thermosetting silylene resin has the formula:
the invention also provides a preparation method of the thermosetting high-temperature-resistant microwave dielectric composite material, which comprises the following steps:
(b) ceramic powder and silylene resin are mixed according to the proportion of the ceramic powder: the mass percentage ratio of the silylene resin is 80:20, mechanically stirring and mixing;
(g) ultrasonically dispersing a mixture of resin and ceramic powder;
(h) pre-polymerizing the mixture uniformly mixed by ultrasound at high temperature;
(i) then, carrying out body casting on the mould, and then carrying out bubble pumping under the vacuum condition;
(j) finally, putting the powder into a blast drying oven for post-curing;
(k) and (5) after the mold is cooled, demolding to obtain the product.
Further, in the step (b), the ultrasonic dispersion time is 1-2h, and the ultrasonic frequency is 40-53 KHz.
Further, in the step (c), the prepolymerization temperature is 140-150 ℃, and the prepolymerization time is 2-3 h.
Further, in the step (d), the bubble pumping temperature in the vacuum environment is 80-100 ℃, and the bubble pumping time is 2-3 h.
Further, in step (e), the post-curing procedure is 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h.
The invention provides two microwave dielectric ceramics with high dielectric constant and low dielectric loss, and the ceramic materials have the following general formula:
0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3
SrTiO3
the invention also provides three kinds of low-viscosity, high-temperature-resistant and low-dielectric-loss silylyne resins;
the silylene alkyne resin is characterized in that the structural formula is
The value of n is 2-3.
The invention also provides a silylyne resin-ceramic composite material substrate, which comprises the following material components: according to the silylene resin: the mass percentage of the ceramic powder is 80: 20.
the invention also provides a preparation method of the silylene resin-ceramic composite material substrate, which is characterized by comprising the following steps of:
(a) ceramic powder and silylene resin are mixed according to the proportion of the ceramic powder: the mass percent of the silicon eneyne resin is 80:20 mechanically stirring and mixing to obtain a mixture;
(b) ultrasonically dispersing a mixture of resin and ceramic powder;
(c) pre-polymerizing the mixture uniformly mixed by ultrasound at high temperature;
(d) then, carrying out body pouring in a mould, and then carrying out bubble pumping under the vacuum condition;
(e) finally, the powder is placed into a blast drying oven for post-curing.
(f) And (5) after the mold is cooled, demolding to obtain the product.
Further, in the step (b), the ultrasonic dispersion time is 1h, and the ultrasonic frequency is 53 KHz. In the step (c), the prepolymerization temperature is 150 ℃, and the prepolymerization time is 2-3 h. In the step (d), the temperature for vacuum foam pumping is 80-100 ℃, and the time for foam pumping is 2-3 h. In the step (e), the post-curing procedure is 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h.
The beneficial technical effects of the invention are as follows:
(1) the invention adopts a one-step synthesis process to prepare the silicon eneyne resin-ceramic composite material substrate, and the composite material substrate has the advantages of high dielectric constant, low dielectric loss, low thermal expansion coefficient, high temperature resistance, adjustable dielectric constant and heat resistance, and the like.
(2) The resin adopted by the invention has low viscosity, the viscosity can be adjusted according to the temperature and the prepolymerization time, the preparation method is very favorable for preparing the composite material, the resin can be fully mixed with the ceramic powder when the viscosity of the resin is low, the mixture is uniformly mixed, and then the body casting is carried out in a prepolymerization mode when the viscosity of the mixture is high, so that the ceramic filler is uniformly distributed in a resin matrix, and the preparation method is very favorable for the performance of a product. The preparation process of the composite material is simple, only the resin and the ceramic powder are required to be compounded, and no solvent is required to be used.
(3) The three structural resins adopted by the invention have good thermal stability and Td5The temperature is respectively as high as 530 ℃, 570 ℃ and 650 ℃, and the microwave dielectric material is prepared by compounding the ceramic powder with the microwave dielectric material, so that the heat resistance of the prepared composite material substrate can be adjusted according to the required use temperature.
(4) The resin adopted by the invention has small dielectric loss which is 0.001-0.004 under 1MHz, and is very beneficial to reducing the dielectric loss of the composite material substrate.
Drawings
FIG. 1 is a TGA profile of a silylyne resin.
Detailed Description
The invention will now be described more fully hereinafter:
the invention provides two high-temperature-resistant microwave dielectric ceramic materials with high dielectric constant and low dielectric loss, which have the following general formula:
0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3
SrTiO3
the invention provides a preparation method of a silylene resin-ceramic composite material substrate, which comprises the following steps:
(1) mixing ceramic powder and resin: heating the resin in an oven until the resin is in a flowing state, adding the ceramic powder into the resin, and mechanically stirring and mixing the ceramic powder uniformly.
(2) Ultrasonic dispersion: and placing the mixture into an ultrasonic machine for ultrasonic dispersion for 1h, so that the ceramic powder can be uniformly dispersed in the resin matrix.
(3) Preparation of a prepolymer: and (3) placing the uniformly dispersed mixture into a drying oven at 150 ℃ for prepolymerization, wherein the prepolymerization time is 2-3 h.
(4) And (3) foam pumping of the prepolymer: pouring the pre-polymerized mixture into a specific mould through a body casting technology, and putting the mould into a vacuum oven at 80-100 ℃ for soaking for 2-3 h.
(5) Curing the prepolymer: and (3) placing the mould into a forced air drying oven for curing, wherein the curing procedure is 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4h, and obtaining the product after the mould is cooled and demoulded.
According to the invention, the silylyne resin is taken as a base material, and different structural resins can be selected for compounding according to the use temperature of the composite material substrate, so that the heat resistance of the composite material substrate can be adjusted;
according to the invention, ceramic powder is used as a filler, and ceramic powder with different dielectric constants and dielectric losses can be selected for compounding according to the dielectric properties required by the composite material substrate, so that the dielectric constant can be adjusted.
According to the invention, the viscosity of the mixture is improved by a pre-polymerization method for the ceramic powder and resin mixture, and the body casting is carried out when the viscosity of the mixture is higher, so that the ceramic powder is uniformly dispersed in the resin matrix, and various performances of the silylyne-ceramic microwave composite material substrate are greatly improved.
In the invention, the ceramic powder and the resin prepolymer are foamed in a vacuum oven for 2-3h, so that the adverse effect on the performance of the product caused by gaps or air holes in the product is avoided.
In the invention, the body casting technology with simple process, safety and environmental protection is adopted, the use of organic solvent in the traditional solution casting is avoided, and the method is very environmental-friendly and economic and is beneficial to actual production. And the body pouring technology is adopted, so that the adverse effects of solvent volatilization in the solution pouring technology on the quality and appearance of the product can be avoided. The following examples, which are included to provide a further understanding of the invention and are not to be construed as limiting the invention in any way, will illustrate embodiments of the invention by specific examples. It should be noted that several variations and modifications can be made by one skilled in the art without departing from the inventive concept. All falling within the scope of the present invention.
In the invention, the structures of the linear silylyne resin, the branched silylyne resin and the star silylyne resin all contain olefinic bonds and acetylene bonds, wherein the olefinic bonds in the structures are as follows: acetylenic linkage 1:2
Example 1 was carried out: preparation method of silicon eneyne resin-ceramic composite material substrate
(1) According to the ceramic powder 0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3: mixing linear silylene resin (olefinic bond: acetylene bond ═ 1: 2) ═ 80:20(W t%), mechanically stirring at 80 deg.C, and mixing;
(2) ultrasonically dispersing the obtained mixture for 1 h;
(3) pre-polymerizing the mixed solution uniformly mixed by ultrasonic in a drying oven at 150 ℃ for 2-3 h;
(4) after prepolymerization is finished, a prepolymer with higher viscosity is obtained, and the prepolymer is poured into a specific mould by adopting a body pouring technology;
(5) putting the mould into a vacuum oven at 100 ℃ and carrying out soaking for 2 h;
(6) after the foam pumping is finished, transferring the mould into a forced air drying oven for post-curing according to a curing procedure of 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h;
(7) and (3) after the solidification is finished, cooling the mold, demolding to obtain a product, and processing the obtained sample into a test standard sample to perform microwave dielectric test (10GHz) and thermal performance test. The properties are shown in Table 1.
Example 2: preparation method of silicon eneyne resin-ceramic composite material substrate
(1) Ceramic powder (SrTiO)3): mixing linear silylene resin (olefinic bond: acetylene bond ═ 1: 2) ═ 80:20 (Wt%), mechanically stirring at 80 deg.C, and mixing well;
(2) ultrasonically dispersing the obtained mixture for 1 h;
(3) pre-polymerizing the mixed solution uniformly mixed by ultrasonic in a drying oven at 150 ℃ for 2-3 h;
(4) after the prepolymerization is finished, obtaining a prepolymer with higher viscosity, and pouring the prepolymer into a specific mould by adopting a body pouring technology;
(5) putting the mould into a vacuum oven at 100 ℃ and carrying out soaking for 2 h;
(6) after the foam pumping is finished, transferring the mould into a forced air drying oven for post-curing according to a curing procedure of 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h;
(7) and (3) after the solidification is finished, cooling the mold, demolding to obtain a product, and processing the obtained sample into a test standard sample to perform microwave dielectric test (10GHz) and thermal performance test. The properties are shown in Table 1.
Example 3:
(1) according to the ceramic powder 0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3: mixing branched silylene resin (olefinic bond: acetylene bond ═ 1: 2) ═ 80:20 (Wt%), mechanically stirring at 80 deg.C, and mixing;
(2) ultrasonically dispersing the obtained mixture for 1 h;
(3) placing the mixture which is uniformly mixed by ultrasonic into a drying oven with the temperature of 150 ℃ for prepolymerization for 2-3 h;
(4) after the prepolymerization is finished, obtaining a prepolymer with higher viscosity, and pouring the prepolymer into a specific mould by adopting a body pouring technology;
(5) putting the mould into a vacuum oven at 100 ℃ and carrying out soaking for 2 h;
(6) after the foam pumping is finished, the mould is transferred into a forced air drying oven for post-curing according to the curing procedure of 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h.
(7) And (3) after the solidification is finished, cooling the mold, demolding to obtain a product, and processing the obtained sample into a test standard sample to perform microwave dielectric test (10GHz) and thermal performance test. The properties are shown in Table 1.
Example 4:
(1) according to the ceramic powder 0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3: star-shaped silylene resin (olefinic bond: acetylene bond ═ 1: 2) ═ 80:20(W t%), mixing the two, mechanically stirring at 80 ℃, and mixing uniformly;
(2) ultrasonically dispersing the obtained mixture for 1 h;
(3) pre-polymerizing the mixed solution uniformly mixed by ultrasonic in a drying oven at 150 ℃ for 2-3 h;
(4) after prepolymerization is finished, obtaining a prepolymerization liquid with higher viscosity, and pouring the prepolymerization liquid into a specific mould by adopting a body pouring technology;
(5) putting the mould into a vacuum oven at 100 ℃ and carrying out soaking for 2 h;
(6) after the foam pumping is finished, transferring the mould into a forced air drying oven for post-curing according to a curing procedure of 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h;
(7) and (3) after the solidification is finished, cooling the mold, demolding to obtain a product, and processing the obtained sample into a test standard sample for microwave dielectric test (10GHz) and thermal performance test. The properties are shown in Table 1.
TABLE 1 Properties of the samples prepared in the examples
TABLE 1 Properties of the samples
In summary, the present invention is only a preferred embodiment, and not intended to limit the scope of the invention, and all equivalent changes and modifications in the shape, structure, characteristics and spirit of the present invention described in the claims should be included in the scope of the present invention.
Claims (10)
1. A thermosetting high-temperature-resistant microwave dielectric composite material is characterized in that: the material components comprise ceramic powder and thermosetting silylene alkyne resin with low viscosity; the ceramic powder is as follows: the mass percentage ratio of the silylene resin is 80:20, the general formula of the ceramic powder is as follows: 0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3Or SrTiO3。
2. The thermosetting high-temperature-resistant microwave dielectric composite material as claimed in claim 1, wherein: the low-viscosity thermosetting silylyne resin is linear silylyne resin, branched silylyne resin or star silylyne resin.
3. The thermosetting high-temperature-resistant microwave dielectric composite material as claimed in claim 1, wherein: the low-viscosity thermosetting silicon eneyne resin has a structural formula as follows:
or the like, or, alternatively,
4. a method for preparing the thermosetting high-temperature-resistant microwave dielectric composite material as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
(a) ceramic powder and silylene resin are mixed according to the proportion of the ceramic powder: the mass percentage ratio of the silylene resin is 80:20, mechanically stirring and mixing;
(b) ultrasonically dispersing a mixture of resin and ceramic powder;
(c) pre-polymerizing the mixture uniformly mixed by ultrasound at high temperature;
(d) then, carrying out body casting on the mould, and then carrying out bubble pumping under the vacuum condition;
(e) finally, putting the powder into a blast drying oven for post-curing;
(f) and (5) after the mold is cooled, demolding to obtain the product.
5. The preparation method of the thermosetting high-temperature microwave dielectric composite material as claimed in claim 4, wherein the preparation method comprises the following steps: in the step (b), the ultrasonic dispersion time is 1-2h, and the ultrasonic frequency is 40-53 KHz.
6. The preparation method of the thermosetting high-temperature microwave dielectric composite material as claimed in claim 4, wherein the preparation method comprises the following steps: in the step (c), the prepolymerization temperature is 140-150 ℃, and the prepolymerization time is 2-3 h.
7. The preparation method of the thermosetting high-temperature microwave dielectric composite material as claimed in claim 4, wherein the preparation method comprises the following steps: in the step (d), the bubble pumping temperature in the vacuum environment is 80-100 ℃, and the bubble pumping time is 2-3 h.
8. The preparation method of the thermosetting high-temperature microwave dielectric composite material as claimed in claim 4, wherein the preparation method comprises the following steps: in step (e), the post-curing procedure is 150 ℃/2h +170 ℃/2h +210 ℃/2h +250 ℃/4 h.
9. A microwave dielectric ceramic is characterized by having a general formula: 0.5MgTiO3-0.5(Ca0.5Nd0.3)TiO3。
10. A microwave dielectric ceramic is characterized by having a general formula: SrTiO3。
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Application publication date: 20200110 |