Polysulfone polymer, resin composition, and process for producing the same
阅读说明：本技术 聚砜高分子、树脂组合物及其制造方法 (Polysulfone polymer, resin composition, and process for producing the same ) 是由 林典庆 高敏慈 于 2019-01-31 设计创作，主要内容包括：本发明公开一种聚砜高分子,其具有以下式(I)结构通式：<Image he="169" wi="700" file="DDA0001964599700000011.GIF" imgContent="drawing" imgFormat="GIF" orientation="portrait" inline="no"></Image>其中,R<Sub>2</Sub>为各自独立的取代或未经取代的芳香环；X为一同时具有酯基及羟基取代的连结基；R<Sub>3</Sub>为碳数3以上的脂肪族连结基或含有至少2个芳香环的芳香族连结基,且其芳香环中至少两个芳香环以氧原子、硫原子、异亚丙基或六氟异亚丙基连接；且R’为含有环氧官能基的末端基团。(The invention discloses a polysulfone macromolecule, which has the following structural general formula (I): wherein R is 2 Are each independently substituted or unsubstituted aromatic rings; x is a linking group having both an ester group and a hydroxyl group; r 3 Is an aliphatic linking group having 3 or more carbon atoms or an aromatic linking group having at least 2 aromatic rings, wherein at least two of the aromatic rings are selected from the group consisting of an oxygen atom, a sulfur atom, an isopropylidene group and a hexafluoro groupAn isopropylidene linkage; and R' is an end group containing an epoxy functional group.)
1. A polysulfone polymer having the general structural formula of formula (I):
R2are each independently substituted or unsubstituted aromatic rings;
x is a linking group having both an ester group and a hydroxyl group;
R3is an aliphatic linking group having 3 or more carbon atoms or an aromatic linking group having at least 2 aromatic rings, wherein at least two aromatic rings in the aromatic rings are connected by an oxygen atom, a sulfur atom, an isopropylidene group or a hexafluoroisopropylidene group;
n is 30 to 200; and is
R' is an end group containing an epoxy functional group.
2. The polysulfone polymer of claim 1, having the structure of formula (I):
wherein R is4、R5、R12、R13Hydrogen, chlorine, bromine or a group containing an aromatic ring structure, which are the same or different, wherein a, b, c and d are respectively 0-4;
R3r', n are as defined in claim 1.
3. The polysulfone polymer of claim 1, wherein R is3Is a C3 to C10 linear or branched alkylene group, a C3 to C10 linear or branched alkenyl group, a linkage group comprising a C3 to C20 alicyclic group, and wherein the C3 to C10 linear or branched alkylene group is unsubstituted, one or more methylene groups (-CH2-) are substituted with a carbonyl group (-C ═ O-) or an oxy group (-O-) and wherein the carbonyl group (-C ═ O-) or oxy group (-O-) substituents are not directly linked to each other; or a linking group comprising the general structural formula of the following formula (II):
y is oxygen atom, sulfur atom, isopropylidene or hexafluoroisopropylidene.
4. The polysulfone macromolecule of claim 1, wherein R' is a structure comprising formula (IV):
5. the polysulfone polymer according to any of claims 1, 3, or 4, wherein the linking group having both an ester group and a hydroxyl group is formed by reacting an acid group of a dicarboxylic acid compound with an epoxy group of a diepoxide containing a sulfonyl group.
6. The polysulfone polymer of claim 5, wherein the sulfonyl group-containing diepoxide has the general structural formula of formula (V):
wherein R is6～R9Is hydrogen, chlorine, bromine or a group containing an aromatic ring structure, R10、R11Is a chain structure containing a carbon chain having 1 or more carbon atoms or an ether or aromatic ring structure.
7. The polysulfone polymer of claim 5, wherein the dicarboxylic acid is selected from the group consisting of cis-butenedioic acid, trans-butenedioic acid, oxaloacetic acid, adipic acid derivatives, glutaric acid derivatives, succinic acid, malonic acid derivatives, pimelic acid, 1, 8-suberic acid, azelaic acid, sebacic acid, ketopimelic acid, 4' -diphenyletherdicarboxylic acid, cis-4-cyclohexene-1, 2-dicarboxylic acid, trans-4-cyclohexene-1, 2-dicarboxylic acid.
8. A process for producing the polysulfone polymer of claim 5, comprising the steps of:
providing a reaction mixture comprising a dicarboxylic acid and a sulfonyl-containing diepoxide, and the equivalent ratio of the sulfonyl-containing diepoxide to the dicarboxylic acid is greater than 1;
adding the reaction mixture into a solvent, and heating to enable the dicarboxylic acid in the reaction mixture and the diepoxide containing the sulfonyl to carry out polymerization reaction in the presence of a catalyst; and
after confirming that the dicarboxylic acid in the reaction mixture has completely reacted, the heating and polymerization reaction are stopped.
9. A resin composition comprising:
the polysulfone polymer of any of claims 1-4;
having sulfonyl groups in the main chain
an organic solvent.
10. The resin composition of claim 9, wherein the organic solvent comprises at least one of N-Methyl pyrrolidone (N-Methyl-2-pyrrolidone), N-ethyl pyrrolidone (N-ethyl-2-pyrrolidone), propylene glycol Methyl ether acetate (propylene glycol Methyl ether acetate), dimethylacetamide (N, N-dimethylacetamide), dimethylformamide (N, N-dimethylformamide), dimethylsulfoxide (dimethyl sulfoxide), propylene glycol monomethyl ether (propylene glycol monomethyl ether), Tetrahydrofuran (Tetrahydrofuran), and gamma-butyrolactone (gamma-butyrolactone), or a combination thereof.
11. The resin composition according to any one of claims 9 to 10, further comprising at least one of a leveling agent, a co-solvent, a surfactant, a silane coupling agent.
12. A substrate attaching method comprises the following steps:
providing a first substrate;
providing a resin composition according to any one of claims 9 to 10 and applying the resin composition to the surface of the first substrate;
performing a heat treatment to remove the organic solvent in the resin composition; and
and providing a second substrate, attaching the second substrate to the first substrate, and clamping the resin between the first substrate and the second substrate.
13. The method of claim 12, wherein the temperature of the heating step is 80-180 ℃.
14. The method of claim 12, wherein the step of bonding the second substrate to the first substrate is performed at a temperature of 180-220 ℃.
15. The method of claim 12, further comprising a step of forming a surface treatment layer on the first substrate surface before the step of applying the resin composition to the first substrate surface.
16. The method according to claim 15, wherein the surface treatment layer is a delamination profile comprising one or a combination of acrylic resin, polyimide, polyamide, polyamic acid, and polybenzoxazole.
17. The method of claim 16, wherein the release profile further comprises a plurality of inorganic particles.
[ technical field ] A method for producing a semiconductor device
The present invention relates to a polymer and a method for producing the same, a resin composition containing the polymer and a method for producing the same, and a method for bonding substrates using the resin composition, and more particularly, to a polysulfone polymer and a method for producing the same, a resin composition containing the polysulfone polymer and a method for producing the same, and a method for bonding substrates using the resin composition.
[ background of the invention ]
In the semiconductor packaging process, in order to facilitate the operation of the production line, the silicon wafer is temporarily attached to the carrier substrate by the adhesive material, and then the subsequent manufacturing process of the device is performed; the bonding temperature of the adhesive material is 220 ℃ as the upper limit, and if the temperature required by bonding exceeds 220 ℃, the problems of serious warping, interface damage or gas overflow of the silicon wafer and the like are easily caused. In addition, a short high temperature process is performed in the semiconductor packaging process, the high temperature can reach over 260 ℃, and if the heat resistance of the adhesive material is poor, the material can deform and even flow seriously.
The conventional polysulfone polymer (polysulfonene) commercial product is required to have high glass transition temperature (Tg), high heat resistance, acid resistance and alkali resistance, such as BASF companyPolysulfone polymers of E (Polyethylsulfone; PES), S (Polysulfon; PSU), P (Polyphenylsulfone; PPSU) series, SolveyWhen these commercially available polysulfone polymer (polysufone) series adhesives are used in semiconductor bonding processes, the glass transition temperature (Tg) of the polysulfone polymer (polysufone) in the adhesives is higher than 220 ℃ or the material structure is rigid, so the temperature required for bonding must be higher than 220 ℃, which causes problems such as severe warpage of the silicon wafer, interface destruction, or outgassing. Therefore, these commercially available polysulfone polymer (polysulfonone) series adhesives are not suitable for semiconductor packaging process.
Accordingly, a glue material that provides good bonding efficiency at a low bonding temperature (80-220 ℃) and does not overflow during other high temperature processes of semiconductor packaging is desired in the industry.
[ summary of the invention ]
The invention aims to provide a polysulfone polymer, which has the following structural general formula (I):
R2are each independently substituted or unsubstituted aromatic rings; x is a linking group having both an ester group and a hydroxyl group; r3Is an aliphatic linking group having 3 or more carbon atoms or an aromatic linking group having at least 2 aromatic rings, wherein at least two aromatic rings in the aromatic linking group are linked by an oxygen atom, a sulfur atom, an isopropylidene group or a hexafluoroisopropylidene group, and R is3A molecular structure having a soft segment; and R' is a terminal group containing an epoxy functional group; n is 30 to 200. Accordingly, by containing both sulfonyl and R3The soft segment molecular structure can be matched to adjust the softening temperature of the material, and the soft segment molecular structure can be suitable for lower operation temperature in the temporary bonding process of semiconductor packaging, wherein R3If a hard segment molecular structure, such as a benzene ring or biphenyl structure, is used, the bonding rate at a lower operating temperature is poor; the polysulfone polymer end of the invention has an epoxy functional group, which can improve the high temperature resistance of the whole material, so that the material can not deform or even flow seriously even in a high temperature environment in the packaging process of the rubber material.
Another object of the present invention is to provide a resin composition comprising: the polysulfone polymer described above; having sulfonyl groups in the main chain
Another object of the present invention is to provide a method for bonding a substrate, comprising the steps of: providing a first substrate; providing the resin composition described in the previous paragraph, applying the resin composition to the surface of the first substrate, and performing a heat treatment to remove the organic solvent in the resin composition; and providing a second substrate, bonding the second substrate to the first substrate, and sandwiching the resin between the first substrate and the second substrate, thereby temporarily bonding the second substrate to the first substrate.
[ description of the drawings ]
Fig. 1A to 1D illustrate a cross-sectional process of one embodiment of a substrate bonding method according to the present invention.
Fig. 2A to 2D illustrate cross-sectional processes of another embodiment of a substrate bonding method according to the present invention.
[ description of reference ]
100 first substrate
200 second substrate
201 back side
202 processed surface
300 resin composition
400 delamination profile
[ detailed description ] embodiments
The polysulfone polymer has the following structural general formula (I):
R2are each independently substituted or unsubstituted aromatic rings; x is a linking group having both an ester group and a hydroxyl group; r3Is an aliphatic linking group having 3 or more carbon atoms or an aromatic linking group having at least 2 aromatic rings, wherein at least two aromatic rings in the aromatic linking group are linked by an oxygen atom, a sulfur atom, an isopropylidene group or a hexafluoroisopropylidene group, and R is3A molecular structure having a soft segment; and R' is a terminal group containing an epoxy functional group; n is 30 to 200, preferably 38 to 194.
Of the general structural formulas of formula I, those having the following formula (I-a) are preferred:
wherein R is4、R5、R12、R13Can be independently hydrogen, chlorine, bromine or a group containing an aromatic ring structure, and can be the same or different, a, b, c, d are 0-4 respectively; r3R', n are as defined in the preceding paragraph.
R is as defined above3Can be C3-C10 linear chain or branched chain alkylene, C3-C10 linear chain or branched chain alkeneA group comprising a C3-C20 alicyclic linkage and wherein a C3-C10 straight or branched chain alkylene group is unsubstituted, one or more methylene groups (-CH2-) are substituted with a carbonyl (-C ═ O-) or an oxy (-O-) group and wherein the carbonyl (-C ═ O-) or oxy (-O-) substituents are not directly attached to each other; or a linking group comprising the general structural formula of the following formula (II):
y is oxygen atom, sulfur atom, isopropylidene or hexafluoroisopropylidene;
wherein R is3Preferably, it is
Wherein R is14、R15、R16、R17、R18、R19May each independently be hydrogen or methyl.
The above R' may be a structure containing ethylene oxide, propylene oxide, cyclopentane epoxide or cyclohexane epoxide, and is preferably a structure containing ethylene oxide, propylene oxide, cyclopentane epoxide or cyclohexane epoxide
The linking group having both an ester group and a hydroxyl group is obtained by reacting an acid group of a dicarboxylic acid compound with an epoxy group of a sulfonyl group-containing diepoxide.
The sulfonyl-containing epoxide has the following structural general formula (V):
wherein R is6～R9May be hydrogen, chlorine, bromine or a group containing an aromatic ring structure, R10、R11The structure may be a chain structure containing a carbon chain having 1 or more carbon atoms or an ether or aromatic ring structure.
The dicarboxylic acid is a dicarboxylic acid including a linear or branched alkyl group, a dicarboxylic acid including an alicyclic group structure, or a dicarboxylic acid in which at least two aromatic rings are linked with an oxygen atom, a sulfur atom, an isopropylidene group, or a hexafluoroisopropylidene group, and may be, but not limited to, at least one of cis-butenedioic acid, trans-butenedioic acid, oxaloacetic acid (oxaloacetic acid), adipic acid, an adipic acid derivative, glutaric acid, a glutaric acid derivative, succinic acid, malonic acid, a malonic acid derivative, pimelic acid, 1, 8-octanedioic acid, azelaic acid, sebacic acid, ketopimelic acid, 4' -diphenyl ether dicarboxylic acid, cis-4-cyclohexene-1, 2-dicarboxylic acid, trans-4-cyclohexene-1, 2-dicarboxylic acid, or a combination thereof; preferably a dicarboxylic acid comprising a linear alkylene group, a dicarboxylic acid comprising an alicyclic structure, or a dicarboxylic acid in which at least two aromatic rings are linked by an oxygen atom, a sulfur atom, an isopropylidene group or a hexafluoroisopropylidene group; preferred are dicarboxylic acids comprising an alicyclic structure or dicarboxylic acids in which at least two aromatic rings are linked by an oxygen atom, a sulfur atom, an isopropylidene group or a hexafluoroisopropylidene group, such as, but not limited to, 4' -diphenyletherdicarboxylic acid, cis-4-cyclohexene-1, 2-dicarboxylic acid, trans-4-cyclohexene-1, 2-dicarboxylic acid.
According to the invention, the method for preparing the polysulfone polymer comprises the following steps: providing a reaction mixture of a dicarboxylic acid and a sulfonyl-containing diepoxide, and the equivalent ratio of sulfonyl-containing diepoxide to dicarboxylic acid is greater than 1; adding the reaction mixture into a solvent, and heating to enable the dicarboxylic acid in the reaction mixture and the diepoxide containing sulfonyl to carry out polymerization reaction in the presence of a catalyst; and stopping heating and polymerization after the dicarboxylic acid in the reaction mixture is completely reacted. The synthesis is carried out in a mode of excessive diepoxide containing sulfonyl group, so that the tail end of the polysulfone polymer after the reaction is finished is a structure containing an epoxy functional group.
A resin composition according to the present invention comprises: polysulfone polymers as described above; having sulfonyl groups in the main chain
The organic solvent has a function of dissolving and facilitating coating, but is not limited to, at least one of pyrrolidone solvents such as N-Methyl-2-pyrrolidone and N-ethyl-2-pyrrolidone, amide solvents such as Propylene glycol Methyl ether acetate and gamma-butyrolactone, amide solvents such as dimethylacetamide and dimethylformamide, sulfone solvents such as dimethylsulfoxide, ether solvents such as Propylene glycol monomethyl ether and Tetrahydrofuran, or a mixture thereof, provided that the polymerization of the polymer is not affected; the solvent may be a mixture of a non-protonic polar solvent such as NMP used in the present application, and a solvent of a different kind may be used to adjust the dissolving power of the entire resin solution and to adjust the volatilization rate in coating application.
The main chain having a sulfonyl group
The polysulfone polymer according to the present invention may be contained in an amount of 5 to 55 wt%, preferably 10 to 40 wt%, more preferably 10 to 35 wt%, based on 100 wt% of the composition according to the present invention; another main chain different from the structure of formula (I) or formula (I-a) has a sulfonyl groupThe content of the high polymer with the structure can be 1-25 weight percent, preferably 5-15 weight percent, and more preferably 5-10 weight percent; the content of the organic solvent may be 30 to 90 wt%, preferably 35 to 75 wt%, and more preferably 50 to 75 wt%.
The resin composition may further contain a leveling agent, a cosolvent, a surfactant, a silane coupling agent, or other additives for other purposes, as required. Wherein the silane coupling agent can be, but is not limited to, BYK 3620, LAPONITE-EP, BYK 302, BYK307, BYK331, BYK333, BYK342, BYK346, BYK347, BYK348, BYK349, BYK375, BYK377, BYK378, BYK3455, BYK SILCLEAN 3720; the leveling agent can be, but not limited to, silicone leveling agents such as BYK-375, polyacrylate leveling agents such as BYK381, and low molecular weight surface active polymer leveling agents such as BYKETOL-WS; the surfactant can be, but is not limited to, a surfactant compound such as BYK-3410; the cosolvent can be, but not limited to, ester-based solvents such as Propylene glycol methyl ether acetate (Propylene glycol methyl ether acetate), γ -butyrolactone (γ -butyrolactone), and the like; in addition, the content of the leveling agent can be 0 to 5 weight percent, preferably 0.05 to 1 weight percent, and more preferably 0.1 to 0.5 weight percent; the content of the cosolvent may be 1 to 30 weight percent, preferably 5 to 15 weight percent, and more preferably 5 to 10 weight percent.
According to the invention, the substrate attaching method comprises the following steps: providing a first substrate; providing the resin composition, coating the resin composition on the surface of the first substrate, and performing heating treatment to remove the organic solvent in the resin composition; and providing a second substrate, bonding the second substrate to the first substrate, and sandwiching the resin composition between the first substrate and the second substrate.
The temperature of the heating treatment step is between 80 ℃ and 180 ℃, and the solvent in the resin composition can be completely removed by applying a fixed temperature, preferably increasing the heating temperature in a gradient manner, for example, after applying 80 ℃ for several minutes, increasing the temperature to 130 ℃ and continuing to heat for a while, and then increasing the temperature to 180 ℃ until the solvent is completely removed.
The temperature of the step of attaching the second substrate to the first substrate may be set to 220 ℃ or lower, so as to avoid the second substrate from being damaged due to an excessively high temperature, and is preferably performed in an environment of 180 ℃ to 220 ℃.
Before the step of coating the resin composition on the surface of the first substrate, the method for bonding the substrates further comprises a step of forming a surface treatment layer on the surface of the first substrate, so that the resin composition is clamped between the surface treatment layer and the second substrate after the second substrate is bonded to the first substrate.
The surface treatment layer is a release material, which may include one or a combination of acryl resin, polyimide, polyamide, polyamic acid, polybenzoxazole, and may further include a plurality of inorganic particles, such as but not limited to carbon black.
The above summary is intended to provide a simplified summary of the disclosure in order to provide a basic understanding to the reader of the disclosure. This summary is not an extensive overview of the disclosure and is intended to neither identify key/critical elements of the embodiments nor delineate the scope of the embodiments. The basic spirit of the present invention and the technical means and implementation state of the present invention will be easily understood by those skilled in the art after referring to the following embodiments.
In order to make the aforementioned and other objects, features, and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Synthesis example: preparation of the Polymer mixture
Synthesis example 1
Synthesis of mixture (P-I)
67g of Bisphenol S Diglycidyl Ether (CAS 3878-43-1), 22.5g of adipic acid (CAS 124-04-9), 0.18g of 1-Methylimidazole (CAS616-47-7), and 179g of N-Methyl-2-pyrrolidone (N-Methyl-2-pyrrolidone) (CAS872-50-4) as a solvent were placed in a glass kettle, and a dry gas was introduced below the surface of the liquid for 30 minutes. And then heating the glass kettle to 100 ℃ for reaction for 10-12 hours. Continuously monitoring the reaction rate in an acid value titration mode in the reaction process, cooling after the acid value titration confirms that the acid has completely reacted, and stopping the reaction to obtain a mixture (P-I) containing a macromolecule (I) with the following structural formula:
the weight average molecular weight Mw of the mixture (P-I) was determined to be 31000 using gas chromatography (GPC). 10g of the mixture (P-I) was placed in a rotary vacuum concentration flask, and the solvent was removed by heating under reduced pressure to obtain a solid composition weighing 3.25g, which was calculated as a solid content of 32.5 wt%.
Synthesis example 2
Synthesis of mixture (P-II)
67g of bisphenol S diglycidyl ether (CAS.3878-43-1), 39.8g of 4-4-oxybis (benzoic acid) (CAS.2215-89-6), 0.21g of 1-methylimidazole (CAS616-47-7) and 213g of N-methyl-2-pyrrolidone (CAS872-50-4) as a solvent were placed in a glass kettle. And introducing dry gas below the liquid level for 30 minutes, and then heating the glass kettle to 100 ℃ for reaction for 10-12 hours. Continuously monitoring the reaction rate in an acid value titration mode in the reaction process, cooling after the acid value titration confirms that the acid has completely reacted, and stopping the reaction to obtain a mixture (P-II) containing a macromolecule (II) with the following structural formula:
the weight average molecular weight Mw of the mixture (P-II) was determined to be 40000 using gas chromatography (GPC). 10g of the mixture (P-II) was placed in a rotary vacuum concentration flask, and the solvent was removed by heating under reduced pressure to obtain a solid composition weighing 3.25g, which was calculated as a solid content of 32.5 wt%.
Synthesis example 3
Synthesis of mixture (P-III)
67g of bisphenol S diglycidyl ether (CAS.3878-43-1), 26.2g of 1,2,3,6-tetrahydrophthalic acid (1,2,3,6-tetrahydrophthalic acid) (CAS 88-98-2), 0.19g of 1-methylimidazole (616-47-7), and 186g of N-methyl-2-pyrrolidone (872-50-4) as a solvent were placed in a glass kettle. And introducing dry gas below the liquid level for 30 minutes, and then heating the glass kettle to 100 ℃ for reaction for 10-12 hours. Continuously monitoring the reaction rate in an acid value titration mode in the reaction process, cooling after the acid value titration confirms that the acid has completely reacted, and stopping the reaction to obtain a mixture (P-III) containing a macromolecule (III) with the following structural formula:
the weight average molecular weight Mw of the mixture (P-III) was determined to be 34000 using gas chromatography (GPC). 10g of the mixture (P-III) was placed in a rotary vacuum concentration flask, and the solvent was removed by heating under reduced pressure to obtain a solid composition weighing 3.25g, which was calculated as a solid content of 32.5 wt%.
Synthesis example 4
Synthesis of mixture (P-IV)
62.8g of Bisphenol A Diglycidyl Ether (Bisphenol A Diglycidyl Ether) (CAS.1675-54-3), 22.5g of adipic acid (CAS 64-19-7), 0.21g of 1-methylimidazole (CAS616-47-7), and 175g of N-methyl-2-pyrrolidone (CAS872-50-4) as a solvent were placed in a glass kettle. And introducing dry gas below the liquid level for 30 minutes, and then heating the glass kettle to 100 ℃ for reaction for 10-12 hours. Continuously monitoring the reaction rate in an acid value titration mode in the reaction process, cooling after the acid value titration confirms that the acid has completely reacted, and stopping the reaction to obtain a mixture (P-IV) containing a macromolecule (IV) with the following structural formula:
the weight average molecular weight Mw of the mixture (P-IV) was determined to be 42000 using gas chromatography (GPC). 10g of the mixture (P-IV) was placed in a rotary vacuum concentration flask, and the solvent was removed by heating under reduced pressure to obtain a solid composition weighing 3.25g, which was calculated as a solid content of 32.5 wt%.
Synthesis example 5
Synthesis of mixture (P-V)
62.8g of bisphenol S diglycidyl ether (CAS.3878-43-1), 39.8g of 4-4-oxybis (benzoic acid) (CAS.2215-89-6), 3.7g of acetic acid (CAS 64-19-7), 0.21g of 1-methylimidazole (CAS616-47-7) and 205g of solvent N-methyl-2-pyrrolidone (CAS872-50-4) are placed in a glass kettle. And introducing dry gas below the liquid level for 30 minutes, and then heating the glass kettle to 100 ℃ for reaction for 10-12 hours. Continuously monitoring the reaction rate in an acid value titration mode in the reaction process, cooling after the acid value titration confirms that the acid has completely reacted, and stopping the reaction to obtain a mixture (P-V) containing a macromolecule (V) with the following structural formula:
the weight average molecular weight Mw of the mixture (P-V) was identified to be 39500 using gas chromatography (GPC). 10g of the mixture (P-V) was placed in a rotary vacuum concentration flask, and the solvent was removed by heating under reduced pressure to obtain a solid composition weighing 3.25g, which was calculated as a solid content of 32.5 wt%.
Preparation of the resin composition formulation:
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