CN114694898A - Preparation method of MLCC nickel inner electrode slurry - Google Patents

Preparation method of MLCC nickel inner electrode slurry Download PDF

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CN114694898A
CN114694898A CN202210613821.7A CN202210613821A CN114694898A CN 114694898 A CN114694898 A CN 114694898A CN 202210613821 A CN202210613821 A CN 202210613821A CN 114694898 A CN114694898 A CN 114694898A
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aqueous suspension
terpineol
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刘振国
王经伟
蔡昌华
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Northwestern Polytechnical University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract

A preparation method of MLCC nickel inner electrode slurry relates to a preparation method of electrode slurry, and BaTiO is used for preparing electrode slurry3Mixing powder, an aqueous suspending agent, deionized water and hydroxyethyl cellulose to obtain aqueous suspension; mixing octanol, terpineol and ethyl cellulose to obtain an organic carrier; mixing the aqueous suspension, an organic carrier, Ni powder, terpineol, an emulsifier and a phosphate ester dispersing agent NP-4, and grinding by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion droplets in a terpineol system to obtain a barium titanate emulsion system; and carrying out suction filtration on the prepared emulsion to obtain the nickel inner electrode slurry. Slurry inThe stable emulsion is finally formed in the material system, has more uniform dispersion effect and long-term stability, not only can fully exert the capability of barium titanate for inhibiting shrinkage, but also can realize smaller surface roughness of the sintered nickel electrode film, so that the lamination number of the MLCC is increased, and higher electric capacity is obtained.

Description

Preparation method of MLCC nickel inner electrode slurry
Technical Field
The invention relates to a preparation method of electrode paste, in particular to a preparation method of MLCC nickel inner electrode paste.
Background
At present, nickel slurry used in ultra-high capacity multilayer chip ceramic capacitor products such as 0201X104, 0201X105, 0201X224, 0402X106 and the like requires that the particle size of nickel powder is 0.3 micron and the particle size of barium titanate powder is 0.1 micron, and the particle size of powder with such small particle size becomes very high for dispersion requirements. However, most of the current studies focus on the dispersion of nickel powder, and neglect the ceramic powder studies. The preparation method of the nickel inner electrode slurry for MLCC mainly comprises the steps of grinding and dispersing metal powder, mixing and stirring the metal powder, the ceramic powder, a dispersing agent, a binder and an organic solvent, and then rolling the mixture by using a three-roll mill.
At the moment, the slurry system is a suspension, and the long-time standing inevitably causes layering, so that the inorganic particles are agglomerated. The nickel powder has larger particle size than the ceramic powder, and the dispersant is added at one time, so the dispersant often acts with the nickel powder and cannot fully act on the ceramic powder, and the dispersing effect is poor. Therefore, the ceramic powder in the prepared nickel slurry is more prone to agglomerate to form large particles, and the MLCC capacitance is affected.
Disclosure of Invention
The invention aims to overcome the defects, adopts a novel preparation process to solve the problems, and has the innovation point that the high dispersibility of the ceramic powder in the slurry is realized by adopting a form of forming emulsion in a slurry system, so that the high-capacitance MLCC is realized.
The method is implemented in particular as follows:
a preparation method of MLCC nickel inner electrode slurry is characterized by comprising the following process steps: (1) mixing BaTiO with average diameter of 100nm3Mixing powder, water suspending agent, deionized water, hydroxyethyl cellulose, BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent accounts for 0.5 to 2.5 percent of the mass of the ceramic powder, the mixture is stirred for at least 10min, and the mixture is emulsified for 30 to 60 minutes by 3000 revolutions of an emulsifying machine until no large particles exist, so that BaTiO is obtained3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, an emulsifier accounts for 1-3% of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
The invention adopts the form of forming ceramic powder emulsion in a slurry system to realize high dispersibility of ceramic powder in the slurry, firstly adopts an aqueous suspending agent to modify the surface of the ceramic powder, an adsorption chain of the aqueous suspending agent is anchored on the ceramic powder, a hydrophilic group at the other end of the aqueous suspending agent is deep into a water phase, and the suspension is stably dispersed by electrostatic repulsion among particles. And then the water suspension can form stable emulsion in the organic solvent by the hydrophilic and oleophylic characteristics of the emulsifier, so as to realize uniform dispersion. The process results in a stable emulsion with more uniform dispersion and long term stability than suspensions formed by conventional mechanical dispersion. The barium titanate can be uniformly dispersed, so that the shrinkage inhibition capability of the barium titanate can be fully exerted, smaller surface roughness of a nickel electrode film after sintering can be realized, the lamination number of the MLCC is increased, and higher capacitance is obtained.
Further, the water suspending agent is one of Tween80, maleic acid-acrylic acid sodium salt, calcium lignosulfonate, isotridecanol polyoxyethylene ether, polycarboxylate dispersing agent SD-819 and sodium lignosulfonate. The molecular skeleton of the water suspending agent consists of a main chain and a plurality of branched chains, the main chain contains a plurality of active groups and has stronger polarity, the main chain can be anchored on the ceramic powder by virtue of the active groups, the side chains have hydrophilicity and can be stretched in water to form a stereo adsorption structure on the surface of particles to generate a steric hindrance effect, so that the ceramic powder is dispersed and stabilized.
Further, the emulsifier is one of Sodium Dodecyl Sulfate (SDS), glycerol monostearate and octyl phenol polyoxyethylene ether (10). Lipophilic groups and hydrophilic groups in the emulsifier can be inserted into one side with the same property, so that the emulsifier is positioned at a water-oil interface, and finally the emulsifier is formed to wrap the water phase and is uniformly distributed in the oil phase.
The invention has the beneficial effects that: finally, stable emulsion is formed in the slurry system, and compared with the suspension formed by conventional mechanical dispersion, the stable emulsion has more uniform dispersion effect and long-term stability. The barium titanate can be uniformly dispersed, so that the shrinkage inhibition capability of the barium titanate can be fully exerted, smaller surface roughness of a nickel electrode film after sintering can be realized, the lamination number of the MLCC is increased, and higher capacitance is obtained.
Drawings
FIG. 1 is a surface roughness characterization chart of a comparative example.
FIG. 2 is a surface roughness characterization chart of example 1.
FIG. 3 is a surface roughness characterization chart of example 2.
FIG. 4 is a surface roughness characterization plot for example 3.
FIG. 5 is a surface roughness characterization chart for example 4.
FIG. 6 is a surface roughness characterization plot for example 5.
FIG. 7 is a surface roughness characterization plot for example 6.
Fig. 8 is an SEM image of the comparative example.
FIG. 9 is an SEM photograph of example 1.
FIG. 10 is an SEM photograph of example 2.
FIG. 11 is an SEM photograph of example 3.
FIG. 12 is an SEM photograph of example 4.
FIG. 13 is an SEM photograph of example 5.
FIG. 14 is an SEM photograph of example 6.
Detailed Description
Example 1
A preparation method of MLCC nickel inner electrode slurry comprises the following process steps:
(1) mixing BaTiO with average diameter of 100nm3Powder, water suspending agent Tween80, deionized water, hydroxyethyl cellulose, BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent Tween80 accounts for 0.5 percent of the mass of the ceramic powder, the stirring is carried out for at least 10min, and the emulsifying machine rotates 3000 to emulsify for 30 min until no large particles exist, so as to obtain the BaTiO3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, emulsifier Sodium Dodecyl Sulfate (SDS) and phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, emulsifying agent Sodium Dodecyl Sulfate (SDS) accounts for 1 percent of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding for 10 times by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
Example 2
A preparation method of MLCC nickel inner electrode slurry comprises the following process steps:
(1) mixing BaTiO with average diameter of 100nm3Mixing the powder, maleic acid-sodium acrylate as water suspending agent, deionized water, hydroxyethyl cellulose, BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent maleic acid-sodium acrylate accounts for 1.5 percent of the mass of the ceramic powder, stirring is carried out for 15min, and 3000 revolutions of an emulsifying machine are carried out for emulsifying for 45 min until no large particles exist, so as to obtain BaTiO3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier glycerin monostearate and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, emulsifying agent monostearyl fatty glyceride accounts for 2% of the mass of the water suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding for 10 times by a three-roll mill until the water suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
Example 3
A preparation method of MLCC nickel inner electrode slurry comprises the following process steps:
(1) mixing BaTiO with average diameter of 100nm3Mixing powder, water suspending agent calcium lignosulfonate, deionized water, hydroxyethyl cellulose, and BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent calcium lignosulfonate accounts for 2.5 percent of the mass of the ceramic powder, the mixture is stirred for 15min, and the mixture is emulsified for 60 min by 3000 revolutions of an emulsifying machine until no large particles exist, so that BaTiO is obtained3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier octylphenol polyoxyethylene ether (10) and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, emulsifier octylphenol polyoxyethylene ether (10) accounts for 3% of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding for 10 times by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
Example 4
A preparation method of MLCC nickel inner electrode slurry comprises the following process steps:
(1) mixing BaTiO with average diameter of 100nm3Mixing the powder, aqueous suspension agent of isotridecanol polyoxyethylene ether, deionized water, hydroxyethyl cellulose and BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent of isotridecanol polyoxyethylene ether accounts for 1.5 percent of the mass of the ceramic powder, the mixture is stirred for 15min, and the mixture is emulsified for 45 minutes by 3000 revolutions of an emulsifying machine until no large particles exist, so that BaTiO is obtained3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier octylphenol polyoxyethylene ether (10) and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, emulsifying agent octylphenol polyoxyethylene ether (10) accounts for 2% of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding for 15 times by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
Example 5
A preparation method of MLCC nickel inner electrode slurry comprises the following process steps:
(1) mixing BaTiO with average diameter of 100nm3Mixing powder, water suspending agent polycarboxylate dispersant SD-819, deionized water, hydroxyethyl cellulose and BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20:1, the water suspending agent polycarboxylate dispersant SD-819 accounts for 1.5 percent of the mass of the ceramic powder, the mixture is stirred for 15min, and the mixture is emulsified for 45 minutes by 3000 revolutions of an emulsifying machine until no large particles exist, so that BaTiO is obtained3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier octylphenol polyoxyethylene ether (10) and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, emulsifying agent octylphenol polyoxyethylene ether (10) accounts for 2% of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding for 15 times by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering paper with 600 meshes to obtain the nickel inner electrode slurry.
Example 6
A preparation method of MLCC nickel inner electrode slurry comprises the following process steps:
(1) mixing BaTiO with average diameter of 100nm3Mixing the powder, sodium lignosulfonate as aqueous suspension agent, deionized water, hydroxyethyl cellulose, and BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent sodium lignosulfonate accounts for 1.5 percent of the mass of the ceramic powder, the mixture is stirred for 15min, and the mixture is emulsified for 45 min by 3000 revolutions of an emulsifying machine until no large particles exist, so that BaTiO is obtained3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier octylphenol polyoxyethylene ether (10) and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, emulsifying agent octylphenol polyoxyethylene ether (10) accounts for 2% of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding for 15 times by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
Comparative example
(1) Octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10 and mechanically stirring for 5 hours at 60 ℃ to obtain the organic carrier.
(2) Adopting a traditional preparation method to prepare Ni powder with the average diameter of 300nm, BaTiO3 powder with the average diameter of 100nm, (1) prepared organic carrier, terpineol and phosphate dispersant NP-4 according to the mass ratio of 50: 12.5: 25: 11: 1.5, uniformly stirring, premixing by a rotation revolution stirrer, and grinding for 15 times by a three-high mill.
(3) And (3) carrying out suction filtration on the slurry prepared in the step (2), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
The nickel internal electrode pastes prepared in examples 1 to 6 and comparative examples were subjected to surface roughness Rp test (see fig. 1 to 7), SEM characterization test (see fig. 8 to 14), and electrical property test (see table 1).
The electrical property test adopts a four-parameter tester, and can simultaneously test the capacitance value, loss, insulation resistance and withstand voltage of the MLCC, the test voltage is 1V, and the frequency is 1 KHZ. The MLCC capacitor for 0603X105K250NBH has electrical performance requirements of: the allowable range of the capacitance value is 0.9-1.1 muF, the loss DF is less than or equal to 3.5 percent, the withstand voltage BV is more than or equal to 62.5V, and the insulation resistance IR multiplied by C is more than or equal to 100 s. The test data are shown in table 1.
Figure 747418DEST_PATH_IMAGE002
Remarking: in the table, the capacitance, loss and insulation resistance are the average values of 50 MLCC finished capacitors, and the withstand voltage is a range value.
As shown in fig. 1 to 7, the surface roughness of each example is greatly improved as compared to the comparative example, which is only 36% to 64% of the comparative example, and the small surface roughness means that the MLCC can be stacked in a larger number and have a higher capacitance.
Through the SEM characterization graphs of FIGS. 8-14, the particles of each example were uniformly distributed without significant agglomeration, which is significantly improved over the comparative example.
From the electrical property characterization in table 1, it is known that the parameters of each example have a significant improvement effect compared with the comparative example, and can obtain higher capacitance, smaller loss and higher withstand voltage.
In each embodiment of the invention, the embodiment 2 is the optimal proportion.

Claims (5)

1. A preparation method of MLCC nickel inner electrode slurry is characterized by comprising the following process steps: (1) mixing BaTiO with average diameter of 100nm3Mixing powder, water suspending agent, deionized water, hydroxyethyl cellulose, BaTiO3The mass ratio of the powder to the deionized water to the hydroxyethyl cellulose is 20: 20: 1, the water suspending agent accounts for 0.5 to 2.5 percent of the mass of the ceramic powder, the mixture is stirred for at least 10min, and the mixture is emulsified for 30 to 60 minutes by 3000 revolutions of an emulsifying machine until no large particles exist, so that BaTiO is obtained3An aqueous suspension of (a);
(2) octanol, terpineol and ethyl cellulose are mixed according to the mass ratio of 18: 72: 10, mixing, and mechanically stirring for 5 hours at 60 ℃ to obtain an organic carrier;
(3) mixing the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), Ni powder with the average diameter of 300nm, terpineol, an emulsifier and a phosphate ester dispersing agent NP-4, wherein the mass ratio of the aqueous suspension prepared in the step (1), the organic carrier prepared in the step (2), the Ni powder, the terpineol and the phosphate ester dispersing agent NP-4 is 18: 20: 50: 11: 1, an emulsifier accounts for 1-3% of the mass of the aqueous suspension prepared in the step (1), premixing by a rotation revolution stirrer, and grinding by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion liquid drops in a terpineol system to obtain a barium titanate emulsion system;
(4) and (4) carrying out suction filtration on the emulsion prepared in the step (3), and filtering with 600-mesh filter paper to obtain the nickel inner electrode slurry.
2. The method for preparing the MLCC nickel inner electrode paste as claimed in claim 1, wherein the aqueous suspending agent is one of Tween80, maleic acid-acrylic acid sodium salt, calcium lignosulfonate, isotridecanol polyoxyethylene ether, polycarboxylate dispersing agent SD-819 and sodium lignosulfonate.
3. The method for preparing nickel inner electrode paste for MLCC according to claim 1, wherein the emulsifier is one of Sodium Dodecyl Sulfate (SDS), glycerol monostearate and polyoxyethylene octylphenol ether (10).
4. The method for preparing the nickel inner electrode paste for the MLCC according to claim 1, wherein the step (3) is carried out by grinding for 10-15 times through a three-high mill.
5. The method for preparing nickel inner electrode paste for MLCC according to claim 1, wherein the method comprises the following steps: the water suspending agent selected in the step (1) is maleic acid-sodium acrylate, and the mass of the water suspending agent, namely maleic acid-sodium acrylate, is 1.5% of that of the ceramic powder; in the step (3), the emulsifier adopts monostearin, and the emulsifier monostearin accounts for 2% of the mass of the water suspension prepared in the step (1).
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