Environment-friendly MLCC ceramic slurry, thin film and preparation method

Abstract

The invention belongs to the technical field of ceramic preparation, and discloses environment-friendly MLCC ceramic slurry, a film and a preparation method.The preparation method of the environment-friendly MLCC ceramic slurry comprises the steps that ceramic powder, a dispersing agent and propylene carbonate are subjected to first ball-milling mixing, and a first mixture is obtained; carrying out second ball-milling mixing on an adhesive, propylene carbonate, a plasticizer and the first mixture to obtain a second mixture, and carrying out vacuum defoaming treatment on the second mixture to obtain environment-friendly MLCC ceramic slurry; the problems of poisoning risk of operators and environmental pollution caused by volatilization of an organic solvent can be avoided.

Description

Technical Field

[0001] This invention relates to the field of ceramic preparation technology, specifically to an environmentally friendly MLCC ceramic slurry, thin film, and preparation method. Background Technology

[0002] Multilayer ceramic capacitors (MLCCs) are a key electronic component widely used in consumer electronics, communications, industrial applications, automotive, and aerospace. MLCCs offer advantages such as small size, high specific capacitance, and high precision, aligning with the trend towards miniaturization and lightweighting in consumer electronics, and accounting for over 90% of the ceramic capacitor market.

[0003] MLCCs are made by dissolving adhesive resin in an organic solvent to form an adhesive solution, then adding the adhesive solution to a well-dispersed ceramic powder suspension for ball milling and filtration to obtain a ceramic slurry. The ceramic slurry is then coated using a casting method to obtain a stable ceramic dielectric film. Internal electrodes are printed on the cast ceramic dielectric film and stacked in a staggered manner. After high-temperature calcination, metal layers (terminal electrodes) are sealed at both ends to form a multilayer ceramic capacitor.

[0004] Cast coating is a method for preparing large-area, flat, thin ceramic materials. It includes processes such as ceramic slurry preparation, forming, and drying, aiming to obtain sufficiently thin and stable ceramic films. It has become an important technology for multilayer ceramic capacitors and ceramic substrates. In existing cast coating processes, the preparation of the ceramic slurry requires the use of large amounts of organic solvents, such as toluene and xylene. These organic solvents are highly toxic and volatile, posing a significant health hazard to operators and also polluting the air.

[0005] Chinese invention patent application CN103130511A discloses a ceramic slurry composition containing sec-butyl acetate and the use of sec-butyl acetate in the preparation of the ceramic slurry composition. The sec-butyl acetate, as a solvent and dispersant in the ceramic slurry, can effectively dissolve the binder and disperse the ceramic powder with high stability; however, this solvent has an irritating odor. Chinese invention patent application CN111470862A discloses a ceramic slurry, a method for preparing ceramic cast films, and a chip-type multilayer ceramic capacitor. Ethanol is used as a solvent in the ceramic slurry; however, ethanol also has an irritating odor.

[0006] Therefore, there is an urgent need for a new technology that can solve the problem of poisoning caused by the volatile organic solvents used in existing casting coating processes. Summary of the Invention

[0007] The purpose of this invention is to provide an environmentally friendly MLCC ceramic slurry, film, and preparation method that can avoid the risk of operator poisoning and environmental pollution caused by the volatilization of organic solvents.

[0008] To achieve the above objectives, the technical solution adopted by the present invention is as follows: In a first aspect, the present invention provides a method for preparing an environmentally friendly MLCC ceramic slurry, comprising the following steps: Step 1: The ceramic powder, dispersant, and propylene carbonate are ball-milled and mixed to obtain a first mixture; Step 2: The adhesive, propylene carbonate, plasticizer, and the first mixture are ball-milled together to obtain the second mixture; Step 3: The second mixture is subjected to vacuum degassing to obtain an environmentally friendly MLCC ceramic slurry.

[0009] In some embodiments, the ceramic powder comprises one of barium titanate-based materials, lead zirconate titanate-stannate-based materials, alumina (Al2O3), and aluminum nitride (AlN); The adhesive comprises one or a mixture of two of polyvinyl alcohol (PVA) and polyvinyl acetal resin (PVB). The dispersant includes one of trioleic acid glyceride and fish oil; The plasticizer is a citrate ester.

[0010] In some embodiments, the barium titanate-based material includes Ba(Ti) 0.90 Zr 0.05 Hf 0.05 O3、(Ba 0.96 Ca 0.02 Mg 0.02 (Ti) 0.95 Hf 0.05 One of the O3 compounds.

[0011] In some embodiments, the lead zirconate titanate-stannate based material includes Pb 0.95 La 0.02 Ce 0.01 (Zr 0.552 Sn 0.416 Ti 0.032 O3; The polyvinyl acetal resin includes polyvinyl butyral; The citrates include tributyl citrate.

[0012] In some embodiments, when preparing the first mixture, the mass ratio of the ceramic powder, dispersant and propylene carbonate is (90-110):(0.5-1.5):(30-50). The first ball milling mixing time is 10-15 h.

[0013] In some embodiments, when preparing the first mixture, the mass ratio of the ceramic powder, dispersant and propylene carbonate is 100:1:40.

[0014] In some embodiments, when preparing the second mixture, the mass ratio of the adhesive, propylene carbonate and plasticizer is (6-8):(30-40):(3-6). The second ball milling mixing time is 13~18 h.

[0015] In some embodiments, the vacuum degassing treatment takes 1 to 3 hours.

[0016] Secondly, the present invention provides an environmentally friendly MLCC ceramic slurry, which is obtained based on the above-mentioned method for preparing an environmentally friendly MLCC ceramic slurry.

[0017] Thirdly, the present invention provides an environmentally friendly MLCC ceramic film, including a PET film, wherein the aforementioned environmentally friendly MLCC ceramic slurry is attached to the PET film.

[0018] The above technical solution has the following advantages or beneficial effects: Firstly, this invention provides a method for preparing an environmentally friendly MLCC ceramic slurry. Firstly, compared to volatile organic solvents such as toluene and xylene used in traditional casting coating processes, the propylene carbonate used in this invention has low volatility, high boiling point, and non-toxic properties, effectively avoiding the risk of operator poisoning and environmental pollution caused by organic solvent volatilization. Secondly, under the same addition ratio, the solubility of propylene carbonate as a solvent is comparable to that of toluene and ethanol. Furthermore, the product (environmentally friendly MLCC ceramic slurry) prepared using propylene carbonate as the main solvent is more uniform. Finally, this invention also ensures uniform dispersion of ceramic powder and high stability of the slurry through a two-step ball milling process (first ball milling mixing, second ball milling mixing) and vacuum degassing, giving the resulting environmentally friendly MLCC ceramic slurry excellent casting coating performance. This invention not only improves the health and safety of the production process but also conforms to the development trend of green manufacturing in the electronic materials industry.

[0019] In some embodiments, the present invention further defines the key components of the environmentally friendly MLCC ceramic slurry: the ceramic powder is preferably a dielectric material such as barium titanate-based material or lead zirconate titanate-stannate-based material, which has broad applicability; the binder is polyvinyl alcohol and / or polyvinyl acetal resin, which can ensure the green strength; the dispersant is trioleic acid glyceride or fish oil, which can effectively improve the dispersibility of the first mixture; the plasticizer is an environmentally friendly citrate ester; the above components are highly compatible with the core solvent propylene carbonate, and synergistically construct a formulation system with extremely low volatility and safety and non-toxicity, eliminating the toxicity risks of traditional processes, and achieving a green and safe manufacturing process while ensuring the rheological properties of the environmentally friendly MLCC ceramic slurry.

[0020] In some embodiments, the present invention employs Ba(Ti) 0.90 Zr 0.05 Hf 0.05 )O3 and (Ba 0.96 Ca 0.02 Mg 0.02 (Ti) 0.95 Hf 0.05 By precisely combining and doping O3 with elements such as Zr, Hf, Ca, and Mg, the Curie temperature range of the material can be significantly widened while maintaining a high dielectric constant, thus improving the temperature stability of dielectric properties. This results in environmentally friendly MLCC ceramic slurries with low capacitance change rate and high reliability over a wider temperature range.

[0021] In some embodiments, the present invention employs Pb 0.95 La 0.02 Ce 0.01 (Zr 0.552 Sn 0.416 Ti 0.032 O3, as a lead zirconate titanate-stannate-based material, significantly improves the antiferroelectric-ferroelectric phase transition stability and fatigue resistance of environmentally friendly MLCC ceramic pastes by doping with La and Ce and adjusting the Zr / Sn / Ti ratio. At the same time, the use of polyvinyl butyral as a binder and tributyl citrate as a plasticizer not only enhances the flexibility of environmentally friendly MLCC ceramic pastes, but also avoids the health risks of traditional phthalic plasticizers, making the preparation process safer and greener.

[0022] In some embodiments, the present invention optimizes key process parameters by precisely defining the mass ratio of ceramic powder, dispersant, and propylene carbonate, as well as the first ball milling mixing time. The mass ratio of (90-110):(0.5-1.5):(30-50) ensures that the dispersant can fully wet and coat the powder particles at high solid content, and the first ball milling mixing can effectively break up soft agglomerates of powder, achieving highly uniform and stable dispersion of nano- or submicron-sized ceramic powder in propylene carbonate. This lays a key foundation for the subsequent addition of binders and the formation of a uniform, dense, and environmentally friendly MLCC ceramic slurry structure.

[0023] In some embodiments, by precisely optimizing the mass ratio to 100:1:40, the present invention can ensure high solid content while achieving optimal dispersant content, thereby enabling the dispersant to most effectively wet and completely coat ceramic powder particles. Under the action of the first ball milling mixing, an ideal balance between powder dispersibility and slurry flowability can be achieved, providing the most reliable proportional benchmark for forming a highly uniform, stable, and environmentally friendly MLCC ceramic slurry suitable for precision casting coating.

[0024] In some embodiments, the present invention ensures that the adhesive and plasticizer are fully dissolved and uniformly dispersed in the solvent by precisely controlling the ratio of the adhesive, propylene carbonate, and plasticizer, as well as the time of the second ball milling. After a long period of second ball milling, the polymer chains of the adhesive are fully extended and uniformly coated with the dispersed ceramic particles, forming a stable and dense three-dimensional network structure. This endows the environmentally friendly MLCC ceramic slurry with excellent flexibility, strength, and uniform casting and coating film-forming properties, providing an ideal material state for subsequent vacuum degassing treatment.

[0025] In some embodiments, the present invention can eliminate air bubbles introduced during the first ball milling and the second ball milling processes, as well as air bubbles trapped inside the environmentally friendly MLCC ceramic slurry, by setting a vacuum degassing treatment of 1 to 3 hours, thereby effectively avoiding defects caused by residual air bubbles.

[0026] Secondly, this invention also provides an environmentally friendly MLCC ceramic slurry. First, by completely replacing traditional toxic solvents with low-volatility, non-toxic propylene carbonate and optimizing the component ratio, the environmentally friendly MLCC ceramic slurry possesses excellent dispersion stability, rheological properties, and film-forming performance. It can eliminate the risk of poisoning and environmental pollution during the production process and is a key material for achieving safe and green manufacturing. Second, the environmentally friendly MLCC ceramic slurry system prepared with propylene carbonate as a solvent is more uniform.

[0027] Thirdly, the present invention also provides an environmentally friendly MLCC ceramic film. The environmentally friendly MLCC ceramic film prepared by the environmentally friendly MLCC ceramic slurry has the characteristics of uniform thickness, smooth surface, non-toxicity and no emission of volatile organic compounds. Specifically, the environmentally friendly MLCC ceramic film not only has good flexibility and high strength, and is easy to laminate and process, but also can significantly improve the working environment and eliminate the toxicity risks of traditional processes. Attached Figure Description

[0028] Figure 1 This is a schematic flowchart of a method for preparing an environmentally friendly MLCC ceramic slurry according to the present invention; Figure 2 The roughness box plots are for Embodiment 1, Embodiment 2 and Comparative Example 1 of the present invention; Figure 3 This is a density box plot of Embodiments 3, 4 and Comparative Example 1 of the present invention; Figure 4 This is a viscosity diagram of Examples 1-4 and Comparative Example 1 of the present invention; Figure 5 This is a SEM image of the environmentally friendly MLCC ceramic thin film of Example 1 of the present invention; Figure 6 This is a SEM image of the environmentally friendly MLCC ceramic film of Example 2 of the present invention; Figure 7 This is a SEM image of the environmentally friendly MLCC ceramic film of Example 3 of the present invention; Figure 8 This is a SEM image of the environmentally friendly MLCC ceramic film of Example 4 of the present invention. Detailed Implementation

[0029] In the following description, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments can be modified in various ways without departing from the spirit or scope of the invention. Therefore, the drawings and description are considered to be exemplary in nature and not restrictive.

[0030] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.

[0031] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0032] The purpose of this invention is to provide an environmentally friendly MLCC ceramic paste, thin film, and preparation method, wherein, see [link to relevant documentation]. Figure 1 A method for preparing an environmentally friendly MLCC ceramic slurry includes the following steps: Step 1: The ceramic powder, dispersant, and propylene carbonate are ball-milled and mixed to obtain a first mixture; Step 2: The adhesive, propylene carbonate, plasticizer, and the first mixture are ball-milled together to obtain the second mixture; Step 3: The second mixture is subjected to vacuum degassing to obtain an environmentally friendly MLCC ceramic slurry.

[0033] The core of the above preparation method is physical dispersion and system compatibility construction: using low-toxicity and environmentally friendly propylene carbonate as the core solvent, the mixture is first ball-milled to break down the soft agglomerate structure of the ceramic powder with mechanical force. Combined with the wetting and coating effect of the dispersant, the ceramic powder is uniformly dispersed in the solvent to form a stable suspension. Then, a binder, propylene carbonate, and plasticizer are added for a second ball-milling mixture, which allows the binder to fully dissolve and adsorb onto the surface of the ceramic powder particles, and the plasticizer to penetrate between the polymer chains of the binder, constructing a three-dimensional network structure in which the ceramic powder and the organic phase are uniformly compatible. Finally, vacuum degassing is performed to eliminate the air bubbles introduced by the first and second ball-milling mixtures, further improving the dispersion stability and uniformity of the environmentally friendly MLCC ceramic slurry.

[0034] The method of this invention uses propylene carbonate to replace traditional toxic and volatile solvents, eliminating the risk of poisoning and environmental pollution in production from the source, which is in line with the trend of green manufacturing. The ceramic powder is graded and dispersed through a two-step ball milling process (first ball milling and second ball milling), and combined with vacuum degassing treatment, so that the environmentally friendly MLCC ceramic slurry has both excellent rheological properties and dispersion stability.

[0035] Example 1: This embodiment provides a method for preparing an environmentally friendly MLCC ceramic slurry, including the following steps: Step 1, add 50 g Ba(Ti) 0.90 Zr 0.05 Hf 0.05O3, 0.5 g of trioleic acid glyceride, and 20 g of propylene carbonate were placed in a ball mill jar and ball-milled for 10 h to obtain a uniformly mixed first mixture.

[0036] Step 2: Dissolve 3 g of polyvinyl butyral in 15 g of propylene carbonate to obtain a dissolved product. Place the dissolved product, the first mixture, and 1.5 g of tributyl citrate into a ball mill jar and ball mill for 15 h to obtain a second mixture. The second mixture is a high-performance ceramic slurry semi-finished product.

[0037] Step 3: Vacuum degas the second mixture for 2 hours to obtain environmentally friendly MLCC ceramic slurry 1.

[0038] This embodiment also provides a method for preparing an environmentally friendly MLCC ceramic thin film, including the following steps: Environmentally friendly MLCC ceramic slurry 1 was coated onto a PET (Polyethylene Terephthalate) film using a doctor blade casting machine at a casting speed of 0.5 m / min. After drying at 40 °C for 5 h, a smooth and dense environmentally friendly MLCC ceramic film was obtained. (See [link to relevant documentation]). Figure 5 The environmentally friendly MLCC ceramic film of Embodiment 1 of the present invention is dense and flat with few pores.

[0039] Example 2: This embodiment provides a method for preparing an environmentally friendly MLCC ceramic slurry, including the following steps: Step 1: Place 50 g of alumina, 0.5 g of trioleic acid glyceride, and 20 g of propylene carbonate into a ball mill jar and ball mill for 10 h to obtain a uniformly mixed first mixture.

[0040] Step 2: Dissolve 4 g of polyvinyl butyral in 20 g of propylene carbonate to obtain a dissolved product. Place the dissolved product, the first mixture, and 2 g of tributyl citrate into a ball mill jar and ball mill for 15 h to obtain a second mixture. The second mixture is a high-performance ceramic slurry semi-finished product.

[0041] Step 3: Vacuum degas the second mixture for 2 hours to obtain environmentally friendly MLCC ceramic slurry 2.

[0042] This embodiment also provides a method for preparing an environmentally friendly MLCC ceramic thin film, including the following steps: Environmentally friendly MLCC ceramic slurry 2 was coated onto a PET film using a doctor blade casting machine at a casting speed of 0.5 m / min, and then dried at 60 ℃ for 2 h to obtain a smooth and dense environmentally friendly MLCC ceramic film. (See [link to relevant documentation]). Figure 6The environmentally friendly MLCC ceramic film of Embodiment 2 of the present invention is dense and flat with few pores.

[0043] Example 3: This embodiment provides a method for preparing an environmentally friendly MLCC ceramic slurry, including the following steps: Step 1: Place 100 g of aluminum nitride, 1 g of trioleic acid glyceride, and 40 g of propylene carbonate into a ball mill jar and ball mill for 15 h to obtain a homogeneous first mixture.

[0044] Step 2: Dissolve 8 g of polyvinyl butyral in 30 g of propylene carbonate to obtain a dissolved product. Place the dissolved product, the first mixture, and 5 g of tributyl citrate into a ball mill jar and ball mill for 15 h to obtain a second mixture. The second mixture is a high-performance ceramic slurry semi-finished product.

[0045] Step 3: Vacuum degas the second mixture for 2 hours to obtain environmentally friendly MLCC ceramic slurry 3.

[0046] This embodiment also provides a method for preparing an environmentally friendly MLCC ceramic thin film, including the following steps: Environmentally friendly MLCC ceramic slurry 3 was coated onto a PET film using a doctor blade casting machine at a casting speed of 0.5 m / min, and then dried at 50 ℃ for 3.5 h to obtain a smooth and dense environmentally friendly MLCC ceramic film. (See [link to relevant documentation]). Figure 7 The environmentally friendly MLCC ceramic film of Embodiment 3 of the present invention is dense and flat with few pores.

[0047] Example 4: This embodiment provides a method for preparing an environmentally friendly MLCC ceramic slurry, including the following steps: Step 1, take 100 g of Pb 0.95 La 0.02 Ce 0.01 (Zr 0.552 Sn 0.416 Ti 0.032 O3, 1 g of trioleic acid glyceride, and 40 g of propylene carbonate were placed in a ball mill jar and ball-milled for 15 h to obtain a uniformly mixed first mixture.

[0048] Step 2: Dissolve 8 g of polyvinyl butyral in 35 g of propylene carbonate to obtain a dissolved product. Place the dissolved product, the first mixture, and 6 g of tributyl citrate into a ball mill jar and ball mill for 15 h to obtain a second mixture. The second mixture is a high-performance ceramic slurry semi-finished product.

[0049] Step 3: Vacuum degas the second mixture for 2 hours to obtain environmentally friendly MLCC ceramic slurry 4.

[0050] This embodiment also provides a method for preparing an environmentally friendly MLCC ceramic thin film, including the following steps: Environmentally friendly MLCC ceramic slurry 4 was coated onto a PET film using a doctor blade casting machine at a casting speed of 0.5 m / min, and then dried at 50 ℃ for 4 h to obtain a smooth and dense environmentally friendly MLCC ceramic film. (See [link to relevant documentation]). Figure 8 The environmentally friendly MLCC ceramic film of Embodiment 4 of the present invention is dense and flat with few pores.

[0051] Comparative Example 1: Step 1: Place 100 g of ceramic powder, 0.5 g of trioleic acid glyceride, 20 g of toluene, and 20 g of ethanol into a ball mill jar and ball mill for 10 h to obtain the first mixture.

[0052] Step 2: Dissolve 8 g of polyvinyl butyral in a mixture of 20 g of toluene and 20 g of ethanol to obtain a dissolved product. Place the dissolved product, the first mixture, and 6 g of dioctyl phthalate into a ball mill jar and ball mill for 20 h to obtain a second mixture.

[0053] Step 3: Vacuum degas the second mixture for 2 h to obtain ceramic slurry 5. Apply ceramic slurry 5 to PET film using a doctor blade casting machine at a casting speed of 0.5 m / min, and then dry it at 30 ℃ for 3 h to obtain ceramic film.

[0054] See Figure 2 The average roughness of the environmentally friendly MLCC ceramic film in Example 1 of this invention is 0.49 μm, the average roughness of the environmentally friendly MLCC ceramic film in Example 2 is 0.52 μm, and the average roughness of the ceramic film in Comparative Example 1 is 0.51 μm. Analysis and comparison of the roughness box plots show that the roughness distribution of the ceramic film in Comparative Example 1 is wider, while the roughness distribution of the environmentally friendly MLCC ceramic films in Examples 1 and 2 is relatively concentrated. This indicates that the environmentally friendly MLCC ceramic slurry system prepared using propylene carbonate as a solvent is more uniform, resulting in a more uniform surface smoothness of the environmentally friendly MLCC ceramic film.

[0055] See Figure 3 The density distribution of the environmentally friendly MLCC ceramic films in Examples 3 and 4 of this invention is more concentrated than that of the ceramic film in Comparative Example 1, indicating that the environmentally friendly MLCC ceramic film obtained by using propylene carbonate as a solvent has a smoother surface and a more uniform structure.

[0056] See Figure 4The viscosity of the environmentally friendly MLCC ceramic slurry 1 in Example 1 of this invention is 180 mPa·s, the viscosity of the environmentally friendly MLCC ceramic slurry 2 in Example 2 is 193 mPa·s, the viscosity of the environmentally friendly MLCC ceramic slurry 3 in Example 3 is 214 mPa·s, the viscosity of the environmentally friendly MLCC ceramic slurry 4 in Example 4 is 205 mPa·s, and the viscosity of the ceramic slurry 5 in Comparative Example 1 is 195 mPa·s. It can be seen that, under the same addition ratio, the solubility of propylene carbonate as a solvent is comparable to that of toluene and ethanol as solvents.

[0057] Example 5: This embodiment provides a method for preparing an environmentally friendly MLCC ceramic slurry, including the following steps: Step 1, take 90 g (Ba 0.96 Ca 0.02 Mg 0.02 (Ti) 0.95 Hf 0.05 O3, 0.5 g fish oil, and 30 g propylene carbonate were placed in a ball mill jar and ball-milled for 13 h to obtain a uniformly mixed first mixture.

[0058] Step 2: Dissolve 3 g of polyvinyl alcohol in 15 g of propylene carbonate to obtain a dissolved product. Place the dissolved product, the first mixture, and 1.5 g of tributyl citrate into a ball mill jar and ball mill for 13 h to obtain a second mixture. The second mixture is a high-performance ceramic slurry semi-finished product.

[0059] Step 3: Vacuum degas the second mixture for 1 hour to obtain environmentally friendly MLCC ceramic slurry 6.

[0060] This embodiment also provides a method for preparing an environmentally friendly MLCC ceramic thin film, including the following steps: Environmentally friendly MLCC ceramic slurry 6 was coated onto a PET film using a doctor blade casting machine at a casting speed of 0.3 m / min, and then dried at 40 ℃ for 5 h to obtain a smooth and dense environmentally friendly MLCC ceramic film.

[0061] Example 6: This embodiment provides a method for preparing an environmentally friendly MLCC ceramic slurry, including the following steps: Step 1: Place 110 g of alumina, 1.5 g of fish oil and 50 g of propylene carbonate into a ball mill jar and ball mill for 14 hours to obtain a uniformly mixed first mixture.

[0062] Step 2: Dissolve 7 g of a mixture of polyvinyl alcohol and polyvinyl butyral in 30 g of propylene carbonate to obtain a dissolved product. Place the dissolved product, the first mixture, and 5 g of tributyl citrate into a ball mill jar and ball mill for 18 h to obtain a second mixture. The second mixture is a high-performance ceramic slurry semi-finished product.

[0063] Step 3: Vacuum degas the second mixture for 3 hours to obtain environmentally friendly MLCC ceramic slurry 7.

[0064] This embodiment also provides a method for preparing an environmentally friendly MLCC ceramic thin film, including the following steps: Environmentally friendly MLCC ceramic slurry 7 was coated onto a PET film using a doctor blade casting machine at a casting speed of 0.8 m / min, and then dried at 50 ℃ for 3 h to obtain a smooth and dense environmentally friendly MLCC ceramic film.

[0065] In Examples 1-6 of this invention, propylene carbonate was used as the solvent for environmentally friendly MLCC ceramic slurry. The plasticizer and dispersant were both environmentally friendly organic solvents such as citrate esters and trioleic acid glycerides. While obtaining a stable and environmentally friendly MLCC ceramic slurry, the harm to operators and the surrounding environment was also greatly reduced.

[0066] By limiting the proportions of ceramic powder, dispersant, propylene carbonate, binder and plasticizer, the present invention (Examples 1-6) enables environmentally friendly MLCC ceramic slurry to have good rheological properties, resulting in a smooth surface and dense structure of the environmentally friendly MLCC ceramic film after casting.

[0067] The solvent used in Examples 1-6 of this invention is propylene carbonate, which is defined as having low toxicity in chemical handbooks. This avoids the use of toxic organic solvents. Furthermore, propylene carbonate, as a colorless and odorless solvent, can effectively dissolve polyvinyl butyral, making the casting coating process stable and controllable, resulting in environmentally friendly MLCC ceramic films with stable performance. Simultaneously, the plasticizers and dispersants used in Examples 1-6 are citrate esters and trioleic acid glycerides, respectively, both of which are environmentally friendly additives that are non-toxic, odorless, and biodegradable. By using environmentally friendly solvents and plasticizers, Examples 1-6 of this invention effectively reduce the risk of health damage to operators during production and lessen the degree of damage to the natural ecological environment. This constitutes a green manufacturing technology, contributing to the construction and development of an environmentally friendly society.

[0068] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or basic characteristics. Therefore, the embodiments should be considered exemplary and non-limiting in all respects.

[0069] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can be appropriately combined to form other embodiments that can be understood by those skilled in the art. The above content is only for illustrating the technical concept of the present invention and should not be used to limit the scope of protection of the present invention. Any modifications made to the technical solutions based on the technical concept proposed in this invention fall within the scope of protection of this invention.

Claims

1. A method for preparing an environmentally friendly MLCC ceramic slurry, characterized in that, Includes the following steps: Ceramic powder, dispersant and propylene carbonate are ball-milled and mixed to obtain a first mixture. When preparing the first mixture, the mass ratio of ceramic powder, dispersant and propylene carbonate is (90~110):(0.5~1.5):(30~50). The adhesive, propylene carbonate, plasticizer, and the first mixture are then ball-milled together to obtain a second mixture. The second mixture was subjected to vacuum degassing to obtain an environmentally friendly MLCC ceramic slurry.

2. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 1, characterized in that, The ceramic powder includes one of barium titanate-based materials, lead zirconate titanate-stannate-based materials, alumina, and aluminum nitride. The adhesive comprises one or a mixture of two of polyvinyl alcohol and polyvinyl acetal resin. The dispersant includes one of trioleic acid glyceride and fish oil; The plasticizer is a citrate ester.

3. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 2, characterized in that, The barium titanate-based material includes Ba(Ti) 0.90 Zr 0.05 Hf 0.05 O3、(Ba 0.96 Ca 0.02 Mg 0.02 (Ti) 0.95 Hf 0.05 One of the O3 compounds.

4. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 2, characterized in that, The lead zirconate-titanium stannate-based material includes Pb 0.95 La 0.02 Ce 0.01 (Zr 0.552 Sn 0.416 Ti 0.032 O3; The polyvinyl acetal resin includes polyvinyl butyral; The citrates include tributyl citrate.

5. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 1, characterized in that, The first ball milling mixing time is 10-15 h.

6. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 1, characterized in that, When preparing the first mixture, the mass ratio of the ceramic powder, dispersant and propylene carbonate is 100:1:

40.

7. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 1, characterized in that, When preparing the second mixture, the mass ratio of the adhesive, propylene carbonate and plasticizer is (6-8):(30-40):(3-6). The second ball milling mixing time is 13~18 h.

8. The method for preparing an environmentally friendly MLCC ceramic slurry according to claim 1, characterized in that, The vacuum degassing treatment takes 1 to 3 hours.

9. An environmentally friendly MLCC ceramic slurry, characterized in that, This is obtained based on the preparation method of an environmentally friendly MLCC ceramic slurry according to any one of claims 1-8.

10. An environmentally friendly MLCC ceramic film, comprising a PET film, characterized in that, The PET film is coated with an environmentally friendly MLCC ceramic slurry as described in claim 9.

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