CN113307996B - Preparation method of flexible composite membrane with hydrophobicity and low dielectric constant - Google Patents
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Abstract
The invention discloses a preparation method of a flexible composite membrane with hydrophobicity and low dielectric constant, which comprises the steps of dissolving P (VDF-TrFE) in a DMF (dimethyl formamide) organic solvent, dissolving a certain amount of PBDMS in isopropanol, uniformly mixing the two mixed solutions according to a certain proportion, and preparing the P (VDF-TrFE) -PBDMS flexible composite membrane by a solution casting method. The research shows that: the hydrophobic P (VDF-TrFE) -PBDMS flexible composite membrane still shows typical ferroelectricity, piezoelectricity and hydrophobicity along with the increase of the content of the PBDMS.
Description
Technical Field
The invention belongs to the technical field of preparation methods of dielectric composite materials, and particularly relates to a preparation method of a flexible composite membrane with hydrophobicity and low dielectric constant.
Background
In the field of information technology industry, the development of multifunctional, high-performance and light-weight microelectronic products greatly promotes the development of key technologies and materials with ultrahigh density and high performance. In order to solve the problems of signal delay and power consumption caused by high-density integration, the development of a new generation of high-performance low-dielectric and even ultra-low-dielectric material becomes one of the most important research directions in the field. The dielectric organic polymer material can effectively prevent the electrolytic action of the conductive liquid drops, can improve the change of voltage to the controllable range of contact angles, reduces the driving voltage and greatly promotes the practical application of the electrowetting device.
Polyvinylidene fluoride-trifluoroethylene P (VDF-TrFE) is a polar polymer material with piezoelectric effect, and can be used for preparing functional devices such as piezoelectric sensors, exciters, transducers and the like due to good piezoelectric, pyroelectric and ferroelectric properties. Polyborosiloxane (PBDMS) is a novel material in organic silicon resin modified by inorganic elements, has more excellent high-temperature resistance and bonding property compared with common organic polysiloxane resin, but has poorer adhesive force, so the patent combines the excellent characteristics of the two materials to invent a flexible film with hydrophobicity and low dielectric constant.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible composite film with both hydrophobicity and low dielectric constant, and the prepared film has the problems of simultaneously having hydrophobicity, ferroelectricity and piezoelectricity.
The technical scheme adopted by the invention is as follows: a preparation method of a flexible composite film with hydrophobicity and low dielectric constant is characterized in that low-dielectric-constant polyborosiloxane is added into polyvinylidene fluoride-trifluoroethylene to synthesize a hydrophobic low-dielectric-constant flexible film, and the preparation method is implemented according to the following steps:
step 1: preparation of strain rate sensitive substrates
Step 1.1: heating boric acid at 140-180 ℃ for 2-4 h to prepare pyroboric acid;
step 1.2: mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2-4 h in a vacuum kneader at 160-180 ℃, and cooling the final product to room temperature to obtain a polyborosiloxane polymer matrix;
step 2: preparation of hydrophobic P (VDF-TrFE) -PBDMS low dielectric constant flexible composite membrane
Step 2.1: weighing the following raw materials in percentage by mass: polyvinylidene fluoride-trifluoroethylene: polyborosiloxane polymer matrix = (65-95): 5-35);
step 2.2: dissolving polyvinylidene fluoride-trifluoroethylene in an organic solvent DMF, and continuously stirring for 6-12h to obtain a mixed solution A;
step 2.3: dissolving a polyborosiloxane polymer matrix in isopropanol, and continuously stirring to obtain a mixed solution B;
step 2.4: further mixing the mixed solutions A and B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solutions A and B are completely uniform to obtain a mixed solution C;
step 2.5: placing the cleaned glass slide into a vacuum oven, and sucking the mixed solution by using a rubber head dropper to drip on the glass slide placed in the vacuum oven;
step 2.6: vacuumizing, and drying at 60-80 ℃ for 6-8 h;
step 2.7: on the basis of the step 2.6, setting the temperature of the vacuum oven at 120-180 ℃ for annealing for 2-8 hours, and then cooling to room temperature to obtain a composite membrane;
step 2.8: soaking the composite membrane in deionized water for about 5-10 h, and stripping;
and step 3: and (3) stretching the stripped composite membrane to a certain multiplying power in a high molecular polymer stretching instrument at a stretching speed of 3-5 mm/min at room temperature to obtain the final low dielectric flexible composite membrane with hydrophobicity.
The present invention is also characterized in that,
in step 2.2, 5.395-7.885 g of polyvinylidene fluoride-trifluoroethylene are required per 100mL of DMF.
In step 2.3, 0.4165-2.9155 g of polyborosiloxane polymer matrix per 100mL of isopropanol is required.
The multiplying power in the step 3 is 0.5-2.
The stirring time in the step 2.3 is 6-12 h.
The beneficial effects of the invention are:
1) The invention relates to a preparation method of a flexible composite membrane with hydrophobicity and low dielectric constant, which can regulate and control the dielectric constant, mechanical property, waterproofness and corrosion resistance of the flexible composite membrane by selecting reactants with different mass fractions;
2) The prepared flexible composite film has typical ferroelectricity, and the saturation polarization value is reduced along with the increase of the content of PBDMS;
3) The prepared flexible composite membrane has small thickness (micron level), certain piezoelectricity and is suitable for being applied to piezoelectric functional devices.
4) The flexible composite membrane prepared by adopting a solution casting method has a low dielectric constant and good hydrophobicity.
5) The method adopts a method of adding a reactant with low dielectric constant to reduce the dielectric constant and simultaneously has good hydrophobicity, and the static contact angle of water on the surface of the water is large, so that the method is suitable for being applied to electronic devices.
Drawings
FIG. 1 is an XRD pattern of a flexible composite membrane with both hydrophobicity and low dielectric constant prepared in examples 3 and 4 of the invention;
FIG. 2 is a stress-strain curve diagram of the flexible composite film with hydrophobicity and low dielectric constant prepared in examples 3 and 4 of the present invention;
FIG. 3 is a graph showing the relationship between the dielectric constant and the frequency of the flexible composite film with both hydrophobicity and low dielectric constant prepared in examples 3 and 4 of the present invention;
FIG. 4 is a graph of hysteresis loop of a flexible composite film with both hydrophobicity and low dielectric constant prepared in example 3 of the present invention;
FIG. 5 is a graph of hysteresis loop of a flexible composite film with both hydrophobicity and low dielectric constant prepared in example 4 of the present invention;
FIG. 6 is a bar graph of piezoelectric constants of the flexible composite films with hydrophobic property and low dielectric constant prepared in examples 1, 2, 3 and 4 of the present invention;
FIG. 7 is a graph showing the wettability test of the flexible composite film with hydrophobicity and low dielectric constant prepared in example 3 of the present invention;
FIG. 8 is a wettability test chart of the flexible composite film with hydrophobicity and low dielectric constant prepared in example 4 of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
Example 1
Step 1, preparing a strain rate sensitive matrix:
step 1.1 boric acid (H) 3 BO 3 ) Heating at 180 ℃ for 2h to prepare pyroboric acid;
step 1.2, mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2 hours in a vacuum kneading machine at 180 ℃, and cooling a final product to room temperature to obtain a Polyborosiloxane (PBDMS) polymer matrix; wherein the mass ratio of the pyroboric acid to the dimethyl siloxane to the isopropanol is as follows: 1.5:8:0.5
And 2, preparing a hydrophobic P (VDF-TrFE) -PBDMS (PBDMS) low-dielectric-constant flexible composite membrane.
Step 2.1, weighing the following raw materials in percentage by mass: p (VDF-TrFE): PBDMS = 65;
step 2.2, dissolving P (VDF-TrFE) in an organic solvent DMF, and continuously stirring for 6 hours to obtain a mixed solution A; wherein, 5.4145g of P (VDF-TrFE) is required per 100mL of DMF;
step 2.3, dissolving PBDMS in isopropanol, and continuously stirring for 6-12h to obtain a mixed solution B; wherein, PBDMS is required for each 100mL of isopropanol, 2.9155g;
step 2.4, further mixing the mixed solution A and the mixed solution B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solution A and the mixed solution B are completely uniform to obtain a mixed solution C;
2.5, placing the cleaned glass slide into a vacuum oven, sucking a certain volume of mixed solution by using a rubber head dropper, and dripping the mixed solution on the glass slide placed in the vacuum oven;
step 2.6, vacuumizing, and drying for 6 hours at the temperature of 60 ℃;
step 2.7, setting the temperature of the vacuum oven on the basis of the step 2.6, and annealing for 8 hours at the temperature of 120 ℃;
step 2.8, cooling to room temperature, soaking the composite membrane in deionized water for about 5 hours, and stripping;
and 3, stretching the stripped composite membrane to a certain magnification in a high molecular polymer stretcher at a stretching rate of 3mm/min at room temperature to obtain the final hydrophobic low dielectric flexible composite membrane.
Example 2
Step 1, preparing a strain rate sensitive matrix:
step 1.1 boric acid (H) 3 BO 3 ) Heating at 180 ℃ for 2h to prepare pyroboric acid;
step 1.2, mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2 hours in a vacuum kneader at 180 ℃, and cooling the final product to room temperature to obtain a Polyborosiloxane (PBDMS) polymer matrix; wherein the mass ratio of the pyroboric acid to the dimethyl siloxane to the isopropanol is as follows: 1.5;
and 2, preparing a hydrophobic P (VDF-TrFE) -PBDMS (PBDMS) low-dielectric-constant flexible composite membrane.
Step 2.1, weighing the following raw materials in percentage by mass: p (VDF-TrFE): PBDMS = 80;
step 2.2, dissolving P (VDF-TrFE) in an organic solvent DMF, and continuously stirring for 6-12h to obtain a mixed solution A; wherein 6.664g of P (VDF-TrFE) is required per 100mL of DMF;
step 2.3, dissolving PBDMS in isopropanol, and continuously stirring for 6-12h to obtain a mixed solution B; wherein, each 100mL of isopropanol needs 1.666g of PBDMSs;
step 2.4, further mixing the mixed solution A and B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solution A and the mixed solution B are completely uniform to obtain a mixed solution C;
2.5, placing the cleaned glass slide into a vacuum oven, sucking a certain volume of mixed solution by using a rubber head dropper, and placing the mixed solution on the glass slide of the vacuum oven;
step 2.6, vacuumizing, and drying for 6 hours at the temperature of 60 ℃;
step 2.7, setting the temperature of the vacuum oven on the basis of the step 2.6, and annealing for 6 hours at the temperature of 140 ℃;
step 2.8, cooling to room temperature, soaking the composite membrane in deionized water for about 5 hours, and stripping;
and 3, stretching the stripped composite membrane to a certain magnification in a high molecular polymer stretcher at a stretching rate of 3mm/min at room temperature to obtain the final hydrophobic low dielectric flexible composite membrane.
Example 3
Step 1, preparing a strain rate sensitive matrix:
step 1.1 boric acid (H) 3 BO 3 ) Heating at 180 ℃ for 2h to prepare pyroboric acid;
step 1.2, mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2 hours in a vacuum kneader at 180 ℃, and cooling the final product to room temperature to obtain a Polyborosiloxane (PBDMS) polymer matrix; wherein the mass ratio of the pyroboric acid to the dimethyl siloxane to the isopropanol is as follows: 1.5;
and 2, preparing a hydrophobic P (VDF-TrFE) -PBDMS (PBDMS) low-dielectric-constant flexible composite membrane.
Step 2.1, weighing the following raw materials in percentage by mass: p (VDF-TrFE): PBDMS = 85;
step 2.2, dissolving P (VDF-TrFE) in an organic solvent DMF, and continuously stirring for 6-12h to obtain a mixed solution A; wherein, 7.0805g of P (VDF-TrFE) is needed for every 100mL of DMF;
step 2.3, dissolving PBDMS in isopropanol, and continuously stirring for 6-12h to obtain a mixed solution B; wherein, PBDMS1.2495g is needed for each 100mL of isopropanol;
step 2.4, further mixing the mixed solution A and the mixed solution B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solution A and the mixed solution B are completely uniform to obtain a mixed solution C;
step 2.5, placing the cleaned glass slide into a vacuum oven, sucking a certain volume of mixed solution by using a rubber head dropper, and then placing the mixed solution on the glass slide of the vacuum oven;
step 2.6, vacuumizing, and drying for 7 hours at the temperature of 60 ℃;
step 2.7, setting the temperature of the vacuum oven on the basis of the step 2.6, and annealing for 6 hours at the temperature of 140 ℃;
step 2.8, cooling to room temperature, soaking the composite membrane in deionized water for about 5 hours, and stripping;
and 3, stretching the stripped composite membrane to a certain magnification in a high molecular polymer stretcher at a stretching rate of 4mm/min at room temperature to obtain the final hydrophobic low dielectric flexible composite membrane.
Example 4
Step 1, preparing a strain rate sensitive matrix:
step 1.1 boric acid (H) 3 BO 3 ) Heating at 180 ℃ for 2h to prepare pyroboric acid;
step 1.2, mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2 hours in a vacuum kneader at 180 ℃, and cooling the final product to room temperature to obtain a Polyborosiloxane (PBDMS) polymer matrix; wherein the mass ratio of the pyroboric acid to the dimethyl siloxane to the isopropanol is as follows: 1.5;
and 2, preparing a hydrophobic P (VDF-TrFE) -PBDMS (PBDMS) low-dielectric-constant flexible composite membrane.
Step 2.1, weighing the following raw materials in percentage by mass: p (VDF-TrFE): PBDMS = 90;
step 2.2, dissolving P (VDF-TrFE) in an organic solvent DMF, and continuously stirring for 6-12h to obtain a mixed solution A; wherein, 7.497g of P (VDF-TrFE) is required per 100mL of DMF;
step 2.3, dissolving PBDMS in isopropanol, and continuously stirring for 6-12h to obtain a mixed solution B; wherein, PBDMS0.833g is needed for each 100mL of isopropanol;
step 2.4, further mixing the mixed solution A and B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solution A and the mixed solution B are completely uniform to obtain a mixed solution C;
2.5, placing the cleaned glass slide into a vacuum oven, sucking a certain volume of mixed solution by using a rubber head dropper, and placing the mixed solution on the glass slide of the vacuum oven;
step 2.6, vacuumizing, and drying for 7 hours at 70 ℃;
step 2.7, setting the temperature of the vacuum oven on the basis of the step 2.6, and annealing for 4 hours at the temperature of 160 ℃;
step 2.8, cooling to room temperature, soaking the composite membrane in deionized water for about 8 hours, and stripping;
and 3, stretching the stripped composite membrane to a certain magnification in a high molecular polymer stretcher at a stretching rate of 4mm/min at room temperature to obtain the final hydrophobic low dielectric flexible composite membrane.
Example 5
Step 1, preparing a strain rate sensitive matrix:
step 1.1 boric acid (H) 3 BO 3 ) Heating at 180 ℃ for 2h to prepare pyroboric acid;
step 1.2, mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2 hours in a vacuum kneader at 180 ℃, and cooling the final product to room temperature to obtain a Polyborosiloxane (PBDMS) polymer matrix; wherein the mass ratio of the pyroboric acid to the dimethyl siloxane to the isopropanol is as follows: 1.5;
and 2, preparing a hydrophobic P (VDF-TrFE) -PBDMS (PBDMS) low-dielectric-constant flexible composite membrane.
Step 2.1, weighing the following raw materials in percentage by mass: p (VDF-TrFE): PBDMS = 95;
step 2.2, dissolving P (VDF-TrFE) in an organic solvent DMF, and continuously stirring for 6-12h to obtain a mixed solution A; wherein, 7.885g of P (VDF-TrFE) is needed per 100mL of DMF;
step 2.3, dissolving PBDMS in isopropanol, and continuously stirring for 6-12h to obtain a mixed solution B; wherein PBDMS is required for each 100mL of isopropanol, 0.4165g;
step 2.4, further mixing the mixed solution A and B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solution A and the mixed solution B are completely uniform to obtain a mixed solution C;
step 2.5, placing the cleaned glass slide into a vacuum oven, sucking a certain volume of mixed solution by using a rubber head dropper, and then placing the mixed solution on the glass slide of the vacuum oven;
step 2.6, vacuumizing, and drying for 6 hours at 80 ℃;
step 2.7, setting the temperature of the vacuum oven on the basis of the step 2.6, and annealing for 2 hours at the temperature of 180 ℃;
step 2.8, cooling to room temperature, soaking the composite membrane in deionized water for about 10 hours, and stripping;
and 3, stretching the stripped composite membrane to a certain magnification in a high molecular polymer stretcher at a stretching rate of 5mm/min at room temperature to obtain the final hydrophobic low dielectric flexible composite membrane.
P (VDF-TrFE) in the present invention means polyvinylidene fluoride-trifluoroethylene;
as shown in FIG. 1, XRD patterns of the hydrophobic P (VDF-TrFE) -PBDMS low dielectric constant flexible composite films prepared in examples 3 and 4 are shown. The main diffraction peaks at 19.7 ° are respectively in the β phase; the peak at the position where 2 theta is 12.6 degrees indicates the existence of polyborosiloxane, and an XRD (X-ray diffraction) pattern indicates that the hydrophobic low-dielectric-constant flexible composite film prepared by the method meets the expectation;
as shown in fig. 2, as the amount of PBDMS increases, the strain of the P (VDF-TrFE) -PBDMS flexible composite film decreases, and the elastic modulus also decreases, which indicates that the mechanical properties of the PBDMS added composite film decrease;
as shown in fig. 3, the dielectric spectrograms of the hydrophobic P (VDF-TrFE) -PBDMS low-dielectric-constant flexible composite films prepared in examples 3 and 4 have a dielectric constant of only 3.9 at a PBDMS loading of 20 wt.%;
as shown in fig. 4 and 5, the hysteresis loops of the hydrophobic P (VDF-TrFE) -PBDMS low dielectric constant flexible composite films prepared in examples 3 and 4 are illustrated, and the results show that the composite films of the above examples all exhibit typical hysteresis loops and have ferroelectricity;
as shown in FIG. 6, the piezoelectric coefficients of the hydrophobic P (VDF-TrFE) -PBDMS low-k flexible composite films of examples 1, 2, 3 and 4 vary with the intensity of the electric field, and the flexible composite film d increases with the amount of PBDMS 33 Gradually decrease; when the PBDMS content reaches 5% with the increase of the electric field intensity, d 33 The temperature is increased to 4.3pC/N;
as shown in fig. 7-8, the wettability test of the hydrophobic P (VDF-TrFE) -PBDMS low dielectric constant flexible composite film prepared in examples 3 and 4 shows that when the content of PBDMS reaches 20%, the contact angle reaches 107.2, and the composite film is hydrophobic.
Claims (5)
1. A preparation method of a flexible composite film with hydrophobicity and low dielectric constant is characterized in that a low dielectric constant substance polyborosiloxane is added into polyvinylidene fluoride-trifluoroethylene to synthesize a flexible film with hydrophobicity and low dielectric constant, and the preparation method specifically comprises the following steps:
step 1: preparation of strain rate sensitive substrates
Step 1.1: heating boric acid at 140-180 ℃ for 2-4 h to prepare pyroboric acid;
step 1.2: mixing pyroboric acid, dimethyl siloxane and isopropanol, stirring for 2-4 h in a vacuum kneading machine at 160-180 ℃, and cooling a final product to room temperature to obtain a polyborosiloxane polymer matrix;
step 2: preparation of hydrophobic P (VDF-TrFE) -PBDMS low dielectric constant flexible composite membrane
Step 2.1: weighing the following raw materials in percentage by mass: polyvinylidene fluoride-trifluoroethylene: polyborosiloxane polymer matrix = (65-95): 5-35);
step 2.2: dissolving polyvinylidene fluoride-trifluoroethylene in an organic solvent DMF, and continuously stirring for 6-12h to obtain a mixed solution A;
step 2.3: dissolving a polyborosiloxane polymer matrix in isopropanol, and continuously stirring to obtain a mixed solution B;
step 2.4: further mixing the mixed solutions A and B prepared in the step 2.2 and the step 2.3 at room temperature, and stirring until the mixed solutions A and B are completely uniform to obtain a mixed solution C;
step 2.5: placing the cleaned glass slide into a vacuum oven, and sucking the mixed solution by using a rubber head dropper to drip on the glass slide placed in the vacuum oven;
step 2.6: vacuumizing, and drying at 60-80 ℃ for 6-8 h;
step 2.7: on the basis of the step 2.6, setting the temperature of the vacuum oven at 120-180 ℃ for annealing for 2-8 hours, and then cooling to room temperature to obtain a composite film;
step 2.8: soaking the composite membrane in deionized water for about 5-10 h, and stripping;
and 3, step 3: and (3) stretching the stripped composite film to a certain multiplying power in a high molecular polymer stretcher at a stretching speed of 3-5 mm/min at room temperature to obtain the final hydrophobic low dielectric flexible composite film.
2. The method as claimed in claim 1, wherein in step 2.2, 5.395-7.885 g of polyvinylidene fluoride-trifluoroethylene is required per 100mL of DMF.
3. The method as claimed in claim 1, wherein in step 2.3, 0.4165-2.9155 g of polyborosiloxane is required per 100mL of isopropanol.
4. The method for preparing the flexible composite membrane with hydrophobicity and low dielectric constant according to claim 1, wherein the multiplying power in the step 3 is 0.5-2.
5. The method as claimed in claim 1, wherein the stirring time in step 2.3 is 6-12 h.
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