CN114752082B - Solvent system and preparation method and application thereof - Google Patents
Solvent system and preparation method and application thereof Download PDFInfo
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- CN114752082B CN114752082B CN202210506652.7A CN202210506652A CN114752082B CN 114752082 B CN114752082 B CN 114752082B CN 202210506652 A CN202210506652 A CN 202210506652A CN 114752082 B CN114752082 B CN 114752082B
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- 239000002904 solvent Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 73
- 230000000996 additive effect Effects 0.000 claims abstract description 47
- 239000003292 glue Substances 0.000 claims abstract description 30
- 239000003985 ceramic capacitor Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000002148 esters Chemical class 0.000 claims abstract description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 55
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004014 plasticizer Substances 0.000 claims description 11
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
- 238000005266 casting Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- QSJXEFYPDANLFS-UHFFFAOYSA-N Diacetyl Chemical compound CC(=O)C(C)=O QSJXEFYPDANLFS-UHFFFAOYSA-N 0.000 claims description 4
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical group 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000009713 electroplating Methods 0.000 claims description 3
- 230000002706 hydrostatic effect Effects 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- AQEFLFZSWDEAIP-UHFFFAOYSA-N di-tert-butyl ether Chemical compound CC(C)(C)OC(C)(C)C AQEFLFZSWDEAIP-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 17
- 239000011347 resin Substances 0.000 abstract description 17
- 239000000693 micelle Substances 0.000 abstract description 9
- 239000012046 mixed solvent Substances 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 125000000468 ketone group Chemical group 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 230000009878 intermolecular interaction Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000012454 non-polar solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000008863 intramolecular interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/095—Oxygen containing compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a solvent system and a preparation method and application thereof, and relates to the field of ceramic capacitor slurry systems. The invention provides a solvent system which comprises the following components in parts by weight: 0.3-10 parts of trace additives; the micro additives comprise a micro additive A, a micro additive B and a micro additive C; the trace additive A is alcohol, the trace additive B is ketone/ester, and the trace additive C is ether; the weight ratio of the trace additive A to the trace additive B to the trace additive C is as follows: trace additive A: trace additive B: minor additive C = (20-70): (10-50): (15-35). According to the invention, through compounding solvents with different molecular structures, a mixed solvent system capable of effectively dissolving high molecular weight PVB resin is provided, good dissolving of PVB can be realized, the amount of micelle in glue water is reduced to the maximum extent, and the reliability of an MLCC finished product is guaranteed.
Description
Technical Field
The invention relates to the field of ceramic capacitor slurry systems, in particular to a solvent system and a preparation method and application thereof.
Background
With the vigorous development in the fields of 5G communication, intelligent wearing and the like, miniaturization and high capacity become important development directions of MLCC (chip multilayer ceramic capacitor) products, and are also technical difficulties in the production and manufacturing of MLCCs. This technical difficulty is strongly dependent on the technique of thinning the ceramic media, which requires that the green tape of the cast film must be sufficiently thin and strong. At present, the main strategy for improving the strength of the MLCC casting film belt is to adopt PVB resin with high molecular weight as an adhesive, and dissolve the PVB resin through a nonpolar/polar mixed solvent system of toluene and/or absolute ethyl alcohol and/or isopropyl alcohol to prepare glue with certain viscosity for preparing ceramic slurry.
In a PVB dissolving solvent system, the nonpolar solvent mainly plays a role in swelling, so that polymer networks which are mutually entangled are fluffy, and the polar solvent permeates into polymer molecular chains to destroy the interaction among the PVB molecular chains, so that the PVB molecular chains are dissolved. For the PVB resin with high molecular weight, molecular chains of the PVB resin are more entangled, the intermolecular interaction is stronger, and a good dissolving effect cannot be achieved by adopting a conventional dissolving means. The PVB resin with poor dissolution exists in the glue (adhesive solution) in the form of swelling micelle, and the micelle is difficult to completely remove by filtration in the glue and slurry production process due to good deformability. Because the film tape green body for preparing the small-size high-capacity MLCC product is extremely thin, the large micelle particles remained in the film tape are easy to cause the electrode of the MLCC product to bulge and leave holes after glue discharging and sintering, and finally, the reliability of the product is reduced or even the product fails, thereby causing the quality hidden trouble. Therefore, it is necessary to develop a dissolving system and a sol process of high molecular weight PVB resin for the ultra-thin cast film belt of small-size and high-capacity products.
For small-size, high-capacity MLCC products, high molecular weight PVB resin must be used to increase the tape strength. However, high molecular weight PVB resin is difficult to dissolve completely, and undissolved PVB resin exists as large particles of micelles, and the greater the number of micelles, the greater the reliability impact on the MLCC. The macromolecular molecular chains exist in a random coil conformation form, the molecular chains penetrate and wind mutually to form entanglement, and intramolecular and intermolecular interaction is formed through groups with different polarities, so that intermolecular force is improved, and a polymer network is formed. The complete dissolution of the polymer network must fully destroy the intermolecular interaction, open the entanglement points in the network, and fully stretch the molecular chains. Currently, PVB is typically dissolved in a mixed nonpolar/polar solvent system of toluene and/or absolute ethanol and/or isopropanol. According to the principle of similar intermiscibility, nonpolar toluene permeates into a PVB molecular network structure and acts with a nonpolar part of the PVB molecular network structure, so that entangled PVB molecular chains are fluffy and a polymer network is swelled; and the polar alcohol solvent interacts with polar groups on the side chain of the PVB molecule to destroy hydrogen bonds among the PVB molecular chains, thereby achieving the dissolving effect. However, for high molecular weight PVB resin, due to the increased molecular chain length, there are more entanglement between molecular chains, and due to the more pendant groups, the different polar pendant groups respond differently to different solvents, and thus conventional solvent systems do not achieve complete dissolution of the high molecular weight PVB resin and result in the presence of micelles.
Disclosure of Invention
Based on the above, the present invention aims to overcome the defects of the prior art and provide a solvent system, a preparation method and an application thereof.
In order to realize the purpose, the technical scheme adopted by the invention is as follows: a solvent system comprises the following components in parts by weight: 0.3-10 parts of trace additives; the micro additives comprise a micro additive A, a micro additive B and a micro additive C; the trace additive A is alcohol, the trace additive B is ketone/ester, and the trace additive C is ether; the weight ratio of the trace additive A to the trace additive B to the trace additive C is as follows: trace additive A: trace additive B: minor additives C = (20-70): (10-50): (15-35).
The inventor of the application selects trace additives A, B and C to compound, and utilizes the difference of the affinity of solvents with different polarities and different groups of PVB to pertinently destroy the interaction between different side groups among PVB molecular chains. The inventor selects a solvent system suitable for dissolving the PVB with high molecular weight, and reduces the micelle number in glue to the maximum extent. After a large number of experimental tests, the inventor of the application finds that when the total weight of the trace additives is less than 0.3 part, PVB cannot be effectively dissolved, and the viscosity of the prepared glue is higher; when the total amount of the minor additives is more than 10 parts, the compactness of the tape applied to the casting film is poor and the durability of the finished MLCC is deteriorated because the excessive minor additives affect the volatilization characteristics of the solvent during the solid-liquid transition of the ceramic slurry at the time of casting. When the proportion of the trace additives A, B and C is not in the specific protection range, the solvent system cannot fully dissolve PVB, and the viscosity of the obtained glue is higher.
Preferably, the solvent system comprises the following components in parts by weight: 5-8 parts of trace additives. After a large number of experimental tests, the inventor of the present application finds that when the trace additive is selected at the above weight portion, the obtained solvent system has a better effect.
Preferably, the alcohol is at least one of methanol, propanol, n-butanol and isobutanol; the ketone/ester is at least one of acetone, butanone, butanedione, pentanone, methyl acetate, ethyl acetate and butyl acetate; the ether is at least one of dioxane, methyl tert-butyl ether and tert-butyl ether.
Preferably, the weight ratio of the trace additive A, the trace additive B and the trace additive C is as follows: trace additive A: trace additive B: minor additives C = (45-60): (20-35): (20-25). After a large number of experimental tests, the inventor of the present application finds that when the weight ratio of the trace additive is in the above selection, the obtained solvent system has better effect.
Preferably, the solvent system further comprises 90-99.7 parts by weight of a base component, wherein the base component comprises toluene, anhydrous ethanol and/or isopropanol; wherein the weight ratio of the toluene to the absolute ethyl alcohol to the isopropanol is as follows: toluene: absolute ethanol: isopropyl alcohol = (30 to 50): (0-60): (0-60).
Preferably, the preparation method of the solvent system comprises the following steps: weighing the components in parts by weight, and uniformly stirring to obtain the solvent system.
In addition, the invention provides for the use of the solvent system described for dissolving high molecular weight polyvinyl butyral.
Further, the invention provides an application of the solvent system in preparing a chip multilayer ceramic capacitor.
Preferably, the specific method for applying the solvent system in the preparation of the chip multilayer ceramic capacitor is as follows:
(1) Weighing the basic components and the trace additives in parts by weight, and uniformly stirring to obtain the solvent system;
(2) Adding polyvinyl butyral and a plasticizer into the solvent system obtained in the step (1), uniformly stirring, and filtering to obtain an adhesive glue solution;
(3) Adding the adhesive glue solution obtained in the step (2) into a chip multilayer ceramic capacitor slurry system for sanding dispersion to obtain chip multilayer ceramic capacitor slurry;
(4) Preparing a casting film belt from the slurry of the chip multilayer ceramic capacitor obtained in the step (3), and printing, laminating, hydrostatic pressing, cutting, removing glue, sintering, chamfering, terminating, burning copper and electroplating the casting film belt to obtain the chip multilayer ceramic capacitor.
Preferably, in the step (2), the stirring speed is 800-1500rpm, the stirring temperature is less than or equal to 70 ℃, and the weight ratio of the polyvinyl butyral to the plasticizer is as follows: polyvinyl butyral: plasticizer =100: (20-45).
Preferably, the plasticizer is at least one of dibutyl phthalate, dioctyl adipate and epoxidized soybean oil.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, through compounding solvents with different molecular structures, a mixed solvent system capable of effectively dissolving PVB resin with high molecular weight is provided, good dissolving of PVB can be realized, the number of micelles in glue water is reduced to the maximum extent, and the reliability of the MLCC finished product is guaranteed.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
The PVB types selected by the invention are as follows: BH-3 (Japan hydronic chemistry), B-74 (U.S. Sono), B75H (Japan Coly), BH-A (Japan hydronic chemistry);
examples 1 to 14 and comparative examples 1 to 4
The components and the weight parts of the examples and the comparative examples are selected as shown in tables 1 to 3, and the total amount of the toluene, the absolute ethyl alcohol and/or the isopropyl alcohol and the trace additives is 100 percent by weight; the total amount of the trace additive A, the trace additive B and the trace additive C is 100 percent;
the adhesive glue solutions of examples and comparative examples and the methods of manufacturing the chip type multilayer ceramic capacitors were as follows:
(1) Weighing the basic components and the trace additives in parts by weight, and uniformly stirring to obtain the solvent system;
(2) Adding polyvinyl butyral and a plasticizer into the solvent system obtained in the step (1), uniformly stirring, and filtering to obtain an adhesive glue solution; the stirring speed is 1000rpm, the stirring temperature is less than or equal to 70 ℃, and the weight ratio of the polyvinyl butyral to the plasticizer is as follows: polyvinyl butyral: plasticizer =100:30, of a nitrogen-containing gas; the plasticizer is dibutyl phthalate (DBP);
(3) Adding the adhesive glue solution obtained in the step (2) into a chip multilayer ceramic capacitor slurry system for sanding dispersion to obtain chip multilayer ceramic capacitor slurry;
(4) Preparing a casting film belt from the slurry of the chip multilayer ceramic capacitor obtained in the step (3), and printing, laminating, hydrostatic pressing, cutting, removing glue, sintering, chamfering, terminating, burning copper and electroplating the casting film belt to obtain the chip multilayer ceramic capacitor.
The polyvinyl butyral PVB used in examples 1 to 11 was all BH-3; the polyvinyl butyral PVB used in example 12 was B-74; the polyvinyl butyral PVB used in example 13 was B75H; the polyvinyl butyral PVB used in example 14 was BH-A; the polyvinyl butyral PVB used in comparative examples 1-4 was BH-3;
TABLE 1
TABLE 2
TABLE 3
Performance test
(1) Viscosity test method: PVB resin is dissolved according to the required process, after the PVB resin is placed for 24 hours, the test is carried out on a digital rotary viscometer, and the temperature of glue needs to be kept to 25 ℃ at constant temperature before the test. Wherein the standard of reaching standards is that the viscosity is lower than 400cps/25 ℃;
(2) Durability evaluation method: the durability test of the MLCC finished product is carried out according to the GB/T21042-2007 standard, and the number of the tests is one million. Wherein the standard of reaching the standard is that the reject ratio is not higher than 10ppm;
the results of the performance tests are shown in tables 4 and 5 below;
TABLE 4
TABLE 5
| Performance test | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Glue viscosity (cps/25 ℃ C.) | 276 | 436 | 412 | 422 |
| Durability (ppm) | 19 | 15 | 12 | 13 |
Wherein, the addition amount and the proportion of the trace additives of the embodiments 1-14 are all within the required range, so the viscosity of the prepared glue reaches the standard, and the durability of the produced product reaches the standard.
The addition range and the total amount of the trace additives of examples 1 to 4 are in the preferable range, so that the prepared glue has low viscosity and excellent product durability. The addition range and the total addition amount of the trace additives of examples 5-10 are not in the preferable range, and from the result, the viscosity and the durability of the prepared glue are slightly poorer than those of examples 1-4, but the viscosity of the prepared glue reaches the standard, and the durability of the produced product reaches the standard.
The addition range and the total amount of the trace additives of examples 11 to 14 were the same as those of examples 1 to 4, and only the types of the base solvent, the resin or the trace additives were changed, so that the viscosity and the product durability of the prepared glue were similar to those of examples 1 to 4. In particular, the base solvent formulation of example 11 has an increased toluene content, decreased solubility in resin, and a relatively higher glue viscosity than examples 1-4.
In the comparative example 1, the proportion of the trace additives is within the required range, the viscosity of the glue reaches the standard, but the trace additives account for over 10 percent and form an azeotrope with the basic component, and the solvent volatilizes too fast in the drying process of the film belt, so that the pores of the tape casting film are increased, the compactness is reduced, and the durability of the product does not reach the standard. Comparative example 2 has no trace additive and has insufficient dissolving capacity for PVB, so the viscosity of the glue exceeds the standard and the durability of the product is deteriorated. The proportion of the trace additives of the comparative example 3 and the comparative example 4 is not in the standard range, the dissolving capacity to different polarity side groups of PVB molecules is insufficient, the mixed solvent cannot fully damage the interaction between the PVB molecular chain side groups, the PVB is not well dissolved, the viscosity of the glue is over 400cps/25 ℃, the product durability is over 10ppm, and the standard is not met.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. The solvent system is characterized by comprising the following components in parts by weight: 0.3-8 parts of trace additive and 92-99.7 parts of basic component; the trace additives comprise a trace additive A, a trace additive B and a trace additive C; the trace additive A is alcohol, the trace additive B is ketone/ester, and the trace additive C is ether; the weight ratio of the trace additive A to the trace additive B to the trace additive C is as follows: trace additive A: trace additive B: minor additive C = (45-60): (20-35): (20-25); the alcohol is at least one of methanol, propanol, n-butanol and isobutanol; the ketone/ester is at least one of acetone, butanone, butanedione, pentanone, methyl acetate, ethyl acetate and butyl acetate; the ethers are at least one of dioxane, methyl tert-butyl ether and tert-butyl ether; the base component includes toluene, anhydrous ethanol, and/or isopropanol.
2. The solvent system of claim 1, comprising the following components in parts by weight: 5-8 parts of trace additives.
3. A method of preparing the solvent system of claim 1, comprising the steps of: weighing the components in parts by weight, and uniformly stirring to obtain the solvent system.
4. Use of the solvent system of claim 1 for dissolving high molecular weight polyvinyl butyral.
5. Use of the solvent system of claim 1 in the manufacture of a chip multilayer ceramic capacitor.
6. The use according to claim 5, wherein the solvent system is applied in the preparation of chip multilayer ceramic capacitors by a specific method comprising:
(1) Weighing the basic components and the trace additives in parts by weight, and uniformly stirring to obtain the solvent system;
(2) Adding polyvinyl butyral and a plasticizer into the solvent system obtained in the step (1), uniformly stirring, and filtering to obtain an adhesive glue solution;
(3) Adding the adhesive glue solution obtained in the step (2) into a chip multilayer ceramic capacitor slurry system for sanding dispersion to obtain chip multilayer ceramic capacitor slurry;
(4) Preparing a casting film belt from the slurry of the chip multilayer ceramic capacitor obtained in the step (3), and printing, laminating, hydrostatic pressing, cutting, removing glue, sintering, chamfering, terminating, burning copper and electroplating the casting film belt to obtain the chip multilayer ceramic capacitor.
7. The use according to claim 6, wherein in the step (2), the stirring speed is 800-1500rpm, the stirring temperature is less than or equal to 70 ℃, and the weight ratio of the polyvinyl butyral to the plasticizer is as follows: polyvinyl butyral: plasticizer =100: (20-45).
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| CN86108230A (en) * | 1986-12-15 | 1988-06-29 | 上海无线电六厂 | Electronic Ceramic Casting Film Adhesive |
| WO2004087613A1 (en) * | 2003-03-31 | 2004-10-14 | Tdk Corporation | Coating composition for green sheet, green sheet, method for producing green sheet, and method for producing electronic component |
| CN102093577B (en) * | 2010-12-01 | 2013-07-17 | 深圳顺络电子股份有限公司 | Environmental-protection solvent and laminated sheet type component dry-process casting slurry prepared from same |
| JP2012184124A (en) * | 2011-03-03 | 2012-09-27 | Tdk Corp | Coating material for green sheet, method for manufacturing green sheet, and method for manufacturing electronic component |
| CN111087248A (en) * | 2019-12-23 | 2020-05-01 | 厦门华信安电子科技有限公司 | Special adhesive for MLCC and preparation method thereof |
| CN113264764A (en) * | 2021-07-05 | 2021-08-17 | 山东国瓷功能材料股份有限公司 | Solvent system, barium titanate tape-casting slurry and ceramic membrane |
| CN113698212A (en) * | 2021-08-18 | 2021-11-26 | 江苏富乐德半导体科技有限公司 | Ceramic tape-casting slurry and preparation method thereof |
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