CN114044684A - LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing LTCC green tape and method - Google Patents
LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing LTCC green tape and method Download PDFInfo
- Publication number
- CN114044684A CN114044684A CN202111664361.2A CN202111664361A CN114044684A CN 114044684 A CN114044684 A CN 114044684A CN 202111664361 A CN202111664361 A CN 202111664361A CN 114044684 A CN114044684 A CN 114044684A
- Authority
- CN
- China
- Prior art keywords
- green tape
- slurry
- preparing
- parts
- ltcc green
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6264—Mixing media, e.g. organic solvents
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/22—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in calcium oxide, e.g. wollastonite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/36—Glass starting materials for making ceramics, e.g. silica glass
- C04B2235/365—Borosilicate glass
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses an LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing the LTCC green tape and a method, wherein the preparation of the slurry comprises the following processes: preparing a multi-element organic carrier: mixing 2.5-7.5 parts of 4-methyl-2-pentanone, 2.5-7.5 parts of n-butanol and 4 parts of oil-soluble PVB (polyvinyl butyral), and completely dissolving the oil-soluble PVB to obtain the multi-component organic carrier; preparing a powder suspension: uniformly mixing 55 parts of glass powder, 7.25-21.75 parts of 4-methyl-2-pentanone, 7.25-21.75 parts of n-butyl alcohol and 0.75 part of BKY-110 dispersing agent to obtain the powder suspension; preparing slurry: and uniformly mixing the multi-element organic carrier, the powder suspension and 1.25 parts of OE400 plasticizer to obtain the slurry for preparing the LTCC green tape. The LTCC green tape can improve the mechanical property of the LTCC green tape under the condition of not increasing the using amount of the binder.
Description
Technical Field
The invention relates to the technical field of low temperature co-fired ceramics (LTCC), in particular to an LTCC green tape, slurry for preparing the LTCC green tape and a method for preparing the LTCC green tape.
Background
LTCC (low temperature co-fired ceramic) green tape has been widely used as a ceramic substrate of a multi-chip module, and has advantages of easy integration, high wiring density, light weight, etc. The green tape technology is of great importance to the whole LTCC technology, and the green tape with excellent performance is the premise for preparing the LTCC substrate with excellent performance. The raw porcelain belt is required to have certain tensile strength in the technological processes of demoulding, preservation, punching, hot pressing and lamination, and if the tensile strength and toughness are not high enough, the problems of low processing precision and possible waste products can be caused in the processing process. Since mechanical properties rarely appear in the LTCC process standard as performance indexes, there is still a large gap in the research on the mechanical properties of the LTCC green tape, and thus the research on the mechanical properties of the LTCC green tape is particularly urgent.
In the prior art, a more common method for improving the tensile strength of LTCC green tape is to increase the amount of binder. However, this method has the following disadvantages: (1) the viscosity of the slurry is increased, and the fluidity is reduced; (2) the production cost of the slurry is increased; (3) the incomplete dissolution of the binder can cause the problem that insoluble particles exist on the surface of the LTCC green tape, and further the rate of finished products is influenced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an LTCC green tape, a slurry for preparing the LTCC green tape and a method for preparing the LTCC green tape.
The technical scheme adopted by the invention is as follows:
a preparation method of slurry for preparing LTCC green tapes comprises the following steps:
preparing a multi-element organic carrier: mixing 2.5-7.5 parts of 4-methyl-2-pentanone, 2.5-7.5 parts of n-butanol and 4 parts of oil-soluble PVB (polyvinyl butyral), and completely dissolving the oil-soluble PVB to obtain the multi-component organic carrier;
preparing a powder suspension: uniformly mixing 55 parts of glass powder, 7.25-21.75 parts of 4-methyl-2-pentanone, 7.25-21.75 parts of n-butyl alcohol and 0.75 part of BKY-110 dispersing agent to obtain the powder suspension;
preparing slurry: and uniformly mixing the multi-element organic carrier, the powder suspension and 1.25 parts of OE400 plasticizer to obtain the slurry for preparing the LTCC green tape.
Preferably, CaO-B is adopted as the glass powder2O3-SiO2Is a glass ceramic.
Preferably, the glass powder comprises the following components in percentage by mass:
CaO content is 50% -60%, SiO230-35 percent of the total weight of the composition, and the balance of B2O3。
Preferably: when the multi-component organic carrier is prepared, a mixture of 4-methyl-2-pentanone, n-butanol and oil-soluble PVB is subjected to water bath heating, the water bath heating temperature is 35-40 ℃, and the water bath heating time is 40-50 minutes;
preferably: when the powder suspension is prepared, glass powder, 4-methyl-2-pentanone, n-butanol and BKY-110 dispersing agent are uniformly mixed in a ball milling mode, the rotating speed of ball milling is 247-253 r/min, and the ball milling time is 115-125 min.
Preferably: when the slurry is prepared, the multielement organic carrier, the powder suspension and the OE400 plasticizer are uniformly mixed in a ball milling mode, the rotating speed of the ball milling is 247-253 r/min, and the ball milling time is 115-125 min.
Preferably, when the slurry is used for preparing the LTCC green tape, the slurry firstly passes through a 200-mesh screen, then defoaming treatment is carried out, and the slurry after defoaming treatment is prepared into the LTCC green tape by a tape casting process.
The invention also provides the slurry for preparing the LTCC green tape, and the slurry for preparing the LTCC green tape is prepared by the preparation method.
The invention also provides a method for preparing the LTCC green tape, which comprises the following steps: the LTCC green tape is prepared by the paste for preparing the LTCC green tape.
The invention also provides the LTCC green tape which is prepared by the method for preparing the LTCC green tape.
The invention has the following beneficial effects:
in the preparation method of the slurry for preparing the LTCC green porcelain tape, the main components of the multi-component organic carrier are organic solvents (namely the reinforcing agent 4-methyl-2-pentanone and the toughening agent n-butyl alcohol), so that the purpose of improving the tensile strength of the LTCC green porcelain tape can be realized under the condition of not increasing the using amount of the binder. Specifically, the following expression is provided: (1) the main component in the multi-component organic carrier is an organic solvent, so that the final slurry has good fluidity and can realize surface self-healing. (2) The production cost of the invention is reduced, and due to good fluidity, when the slurry is used for preparing the LTCC green tape, the surface quality of the LTCC green tape can be improved without adding a defoaming agent, and the cost is reduced; (3) the yield of the prepared LTCC green tape is improved, and the oil-soluble PVB is pre-dissolved in a multielement organic carrier, so that insoluble substances on the surface of the LTCC green tape can be reduced when the slurry is used for preparing the LTCC green tape, and the quality and the yield of finished products are improved. (4) The tensile strength of the LTCC green tape is improved: the n-butyl alcohol serving as the toughening agent can increase the movement of an oil-soluble PVB molecular chain segment, and 4-methyl-2-pentanone can be inserted into the oil-soluble PVB molecular chain segment, so that the movement of the oil-soluble PVB molecular chain segment is hindered in the stretching process of the LTCC green tape, and the tensile strength is increased.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a process flow chart of the LTCC green tape manufacturing method of the invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any inventive step, are intended to be within the scope of the present invention.
Example 1
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 2.5 parts of 4-methyl-2-pentanone, 7.5 parts of n-butyl alcohol and 4 parts of oil-soluble PVB into a round-bottom flask, and heating in a water bath at the temperature of 35-40 ℃ for 50 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier;
step (2): adding 55 parts of glass powder into a ball milling tank, adding 7.25 parts of 4-methyl-2-pentanone, 21.75 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 115min, thus obtaining a powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 55%, SiO2The content is 30 percent, and the balance is B2O3。
And (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 115min to obtain slurry with good fluidity after ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Comparative example 1
The preparation method of the LTCC green tape in the comparative example adopts the conventional preparation process, and specifically comprises the following steps:
step (1): adding 55 parts of glass powder into a ball milling tank, adding 9.75 parts of 4-methyl-2-pentanone, 29.25 parts of n-butyl alcohol, 4 parts of oil-soluble PVB and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, setting the ball milling time to be 115min, and obtaining powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 55%, SiO2The content is 30 percent, and the balance is B2O3。
Step (2): and (2) adding 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (1), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, setting the ball milling time to be 115min, and obtaining slurry with good fluidity after the ball milling is finished.
And (3): and (3) passing the slurry prepared in the step (2) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The casting process was set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Example 2
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 3.33 parts of 4-methyl-2-pentanone, 6.67 parts of n-butanol and 4 parts of oil-soluble PVB into a round-bottom flask, and heating in a water bath at 35-40 ℃ for 45 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier;
step (2): adding 55 parts of glass powder into a ball milling tank, adding 9.67 parts of 4-methyl-2-pentanone, 19.33 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120min, thus obtaining a powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 55%, SiO2The content is 30 percent, and the balance is B2O3。
And (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120 min. And obtaining slurry with good fluidity after the ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Example 3
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 5 parts of 4-methyl-2-pentanone, 5 parts of n-butyl alcohol and 4 parts of oil-soluble PVB into a round-bottomed flask, and heating in a water bath at the temperature of 35-40 ℃ for 45 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier;
step (2): adding 55 parts of glass powder into a ball milling tank, and carrying out ball millingAdding 14.5 parts of 4-methyl-2-pentanone, 14.5 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into a tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120min to obtain powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 55%, SiO2The content is 30 percent, and the balance is B2O3。
And (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120 min. And obtaining slurry with good fluidity after the ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Example 4
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 6.67 parts of 4-methyl-2-pentanone, 3.33 parts of n-butyl alcohol and 4 parts of oil-soluble PVB into a round-bottom flask, and heating in a water bath at 35-40 ℃ for 45 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 55%, SiO2The content is 30 percent, and the balance is B2O3。
Step (2): adding 55 parts of glass powder into a ball milling tank, adding 19.33 parts of 4-methyl-2-pentanone, 9.67 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120min, thus obtaining a powder suspension with good dispersibility after the ball milling is finished;
and (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120 min. And obtaining slurry with good fluidity after the ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Example 5
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 7.5 parts of 4-methyl-2-pentanone, 2.5 parts of n-butanol and 4 parts of oil-soluble PVB into a round-bottom flask, and heating in a water bath at the temperature of 35-40 ℃ for 40 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier;
step (2): adding 55 parts of glass powder into a ball milling tank, adding 21.75 parts of 4-methyl-2-pentanone, 7.25 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 125min, thus obtaining a powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 55%, SiO2In an amount of30% and the balance B2O3。
And (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 125 min. And obtaining slurry with good fluidity after the ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Example 6
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 3.33 parts of 4-methyl-2-pentanone, 6.67 parts of n-butanol and 4 parts of oil-soluble PVB into a round-bottom flask, and heating in a water bath at 35-40 ℃ for 45 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier;
step (2): adding 55 parts of glass powder into a ball milling tank, adding 9.67 parts of 4-methyl-2-pentanone, 19.33 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120min, thus obtaining a powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content of 60%, SiO2The content is 33 percent, and the balance is B2O3。
And (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120 min. And obtaining slurry with good fluidity after the ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
Example 7
The preparation method of the LTCC green tape comprises the following steps:
step (1): putting 3.33 parts of 4-methyl-2-pentanone, 6.67 parts of n-butanol and 4 parts of oil-soluble PVB into a round-bottom flask, and heating in a water bath at 35-40 ℃ for 45 minutes to completely dissolve the oil-soluble PVB to obtain a multi-component organic carrier;
step (2): adding 55 parts of glass powder into a ball milling tank, adding 9.67 parts of 4-methyl-2-pentanone, 19.33 parts of n-butanol and 0.75 part of BKY-110 dispersing agent into the ball milling tank, setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120min, thus obtaining a powder suspension with good dispersibility after the ball milling is finished; wherein, the glass powder adopted in the embodiment is CaO-B2O3-SiO2The glass powder is microcrystalline glass, and comprises the following components in percentage by mass: CaO content 50%, SiO235% of the total amount of the components and B2O3。
And (3): and (3) adding the multielement organic carrier prepared in the step (1) and 1.25 parts of OE400 plasticizer into the powder suspension prepared in the step (2), setting the ball milling rotation speed to be 250r/min, setting the rotation speed deviation to be +/-3 r/min, and setting the ball milling time to be 120 min. And obtaining slurry with good fluidity after the ball milling is finished.
And (4): and (4) passing the slurry prepared in the step (3) through a 200-mesh screen, then carrying out vacuum defoamation on the slurry at the rotating speed of 30r/min for 30 minutes, then stabilizing for 20 minutes, and then transferring to a casting process. The parameters of the casting process are set as follows: the height of a casting machine is set to be 250 mu m, the flow rate is 0.5m/min, auxiliary exhaust air is 1400r/min, the temperatures of 6 heating procedures are respectively set to be 25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃ and 75 ℃, and the LTCC green tape with good surface quality is finally obtained, and the related performance test data of the LTCC green tape prepared in the embodiment is shown in the table 1.
The method for testing the performance of the LTCC green tape prepared by the embodiment of the invention comprises the following steps:
and (3) viscosity testing: viscosity data were obtained using viscometer # 14 spindle at 25 ℃ circulating water temperature and 60rpm rotational speed.
Tensile strength: an electronic universal testing machine is used for testing the tensile strength (the tensile rate is 5 mm/min) of the raw porcelain tape, a raw porcelain tape sample is a standard 100mm long dumbbell-shaped tensile sample, and in order to avoid the raw porcelain tape from being damaged by a clamp during stretching, thick paper sheets are pasted at two ends of the raw porcelain tape.
Dielectric constant: the dielectric constant and dielectric loss were measured at l0MHz using an Agilent4294A impedance meter.
TABLE 1
As can be seen from Table 1, the tensile strength of the LTCC green tape reaches 2.23-3.57 MPa, and other parameters meet the use requirements. From the comparison result between the example 1 and the comparative example 1, it can be seen that the mechanical property of the LTCC green tape prepared by the invention is improved under the condition that the usage amount of the binder is not increased.
In conclusion, the composite multi-component organic carrier is prepared, the multi-component organic carrier is mainly composed of the organic solvent, and the purpose of improving the tensile strength of the LTCC green ceramic tape can be achieved under the condition that the binder is not added.
The composite multi-element organic carrier provided by the invention has the following beneficial effects: (1) the slurry has good fluidity and can realize surface self-healing. The dosage of the solvent is adjusted, so that the viscosity of the slurry is not too high, and the proper slurry fluidity can enable the surface of the slurry to be self-healed; (2) the production cost is low: the surface quality of the raw porcelain tape can be improved under the condition of not adding a defoaming agent, so that the cost can be reduced; (3) the finished product yield of the LTCC green tape can be improved: the multi-component organic carrier realizes the pre-dissolution of the oil-soluble PVB of the binder, the pre-dissolution of the binder reduces insoluble substances on the surface of the green porcelain tape, and the quality and the yield of finished products are improved. (4) The tensile strength of the LTCC green tape can be improved: the n-butyl alcohol dissolves a solution formed by the oil-soluble PVB, so that the movement of an oil-soluble PVB molecular chain segment is increased, the 4-methyl-2-pentanone is added to be inserted into the oil-soluble PVB molecular chain segment, and the movement of the oil-soluble PVB molecular chain segment can be hindered in the stretching process of the LTCC green tape, so that the tensile strength is increased.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of slurry for preparing LTCC green tape is characterized by comprising the following steps:
preparing a multi-element organic carrier: mixing 2.5-7.5 parts of 4-methyl-2-pentanone, 2.5-7.5 parts of n-butanol and 4 parts of oil-soluble PVB (polyvinyl butyral), and completely dissolving the oil-soluble PVB to obtain the multi-component organic carrier;
preparing a powder suspension: uniformly mixing 55 parts of glass powder, 7.25-21.75 parts of 4-methyl-2-pentanone, 7.25-21.75 parts of n-butyl alcohol and 0.75 part of BKY-110 dispersing agent to obtain the powder suspension;
preparing slurry: and uniformly mixing the multi-element organic carrier, the powder suspension and 1.25 parts of OE400 plasticizer to obtain the slurry for preparing the LTCC green tape.
2. The method for preparing the paste for preparing the LTCC green tape according to claim 1, wherein the glass powder adopts CaO-B2O3-SiO2Is a glass ceramic.
3. The method for preparing the paste for preparing the LTCC green tape according to claim 2, wherein the glass powder comprises the following components in percentage by mass:
CaO content is 50% -60%, SiO230-35 percent of the total weight of the composition, and the balance of B2O3。
4. The method of preparing a slurry for use in the preparation of LTCC green tape as claimed in claim 1, wherein:
when the multi-component organic carrier is prepared, a mixture of 4-methyl-2-pentanone, n-butanol and oil-soluble PVB is subjected to water bath heating, the water bath heating temperature is 35-40 ℃, and the water bath heating time is 40-50 minutes.
5. The method of preparing a slurry for use in the preparation of LTCC green tape as claimed in claim 1, wherein:
when the powder suspension is prepared, glass powder, 4-methyl-2-pentanone, n-butanol and BKY-110 dispersing agent are uniformly mixed in a ball milling mode, the rotating speed of ball milling is 247-253 r/min, and the ball milling time is 115-125 min.
6. The method of preparing a slurry for use in the preparation of LTCC green tape as claimed in claim 1, wherein:
when the slurry is prepared, the multielement organic carrier, the powder suspension and the OE400 plasticizer are uniformly mixed in a ball milling mode, the rotating speed of the ball milling is 247-253 r/min, and the ball milling time is 115-125 min.
7. The method as claimed in claim 1, wherein when the slurry is used to prepare the LTCC green tape, the slurry is firstly screened by a 200-mesh screen, then the slurry is defoamed, and the defoamed slurry is cast into the LTCC green tape.
8. A paste for producing an LTCC green tape, characterized in that the paste for producing an LTCC green tape is produced by the production method of any one of claims 1 to 7.
9. A method for preparing LTCC green tape is characterized by comprising the following steps:
an LTCC green tape made from the slurry for making LTCC green tape of claim 8.
10. An LTCC green tape produced by the method for producing an LTCC green tape according to claim 9.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111664361.2A CN114044684A (en) | 2021-12-31 | 2021-12-31 | LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing LTCC green tape and method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111664361.2A CN114044684A (en) | 2021-12-31 | 2021-12-31 | LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing LTCC green tape and method |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114044684A true CN114044684A (en) | 2022-02-15 |
Family
ID=80213631
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111664361.2A Pending CN114044684A (en) | 2021-12-31 | 2021-12-31 | LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing LTCC green tape and method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114044684A (en) |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0166400A2 (en) * | 1984-06-25 | 1986-01-02 | International Business Machines Corporation | Method for forming a ceramic slurry |
US5632942A (en) * | 1993-05-24 | 1997-05-27 | Industrial Technoology Research Institute | Method for preparing multilayer ceramic/glass substrates with electromagnetic shielding |
US20030214715A1 (en) * | 2002-05-20 | 2003-11-20 | Eastman Kodak Company | Polyvinyl butyral films prepared by coating methods |
CN101410763A (en) * | 2006-03-30 | 2009-04-15 | 三菱化学株式会社 | Image forming apparatus |
CN103435358A (en) * | 2013-08-29 | 2013-12-11 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
CN107739203A (en) * | 2017-09-01 | 2018-02-27 | 广东风华高新科技股份有限公司 | The preparation method and ceramic slurry of ceramic slurry |
CN108956699A (en) * | 2018-06-22 | 2018-12-07 | 西安创联电气科技(集团)有限责任公司 | A kind of NOXSensor ceramic chip insulating film band and insulating layer preparation process |
CN110372221A (en) * | 2018-04-13 | 2019-10-25 | 上海晶材新材料科技有限公司 | A kind of low-temperature co-fired ceramics green tape material and preparation method thereof |
CN110683769A (en) * | 2019-10-25 | 2020-01-14 | 赣州中瓷科技有限公司 | Reinforced calcium-boron-silicon glass-ceramic composite material and preparation method thereof |
CN110790568A (en) * | 2019-11-29 | 2020-02-14 | 中国电子科技集团公司第四十三研究所 | Low-dielectric LTCC green tape and preparation method and application thereof |
CN113045204A (en) * | 2021-03-10 | 2021-06-29 | 安徽华封电子科技有限公司 | Low-loss low-temperature co-fired ceramic green tape and preparation method thereof |
-
2021
- 2021-12-31 CN CN202111664361.2A patent/CN114044684A/en active Pending
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0166400A2 (en) * | 1984-06-25 | 1986-01-02 | International Business Machines Corporation | Method for forming a ceramic slurry |
US5632942A (en) * | 1993-05-24 | 1997-05-27 | Industrial Technoology Research Institute | Method for preparing multilayer ceramic/glass substrates with electromagnetic shielding |
US20030214715A1 (en) * | 2002-05-20 | 2003-11-20 | Eastman Kodak Company | Polyvinyl butyral films prepared by coating methods |
CN101410763A (en) * | 2006-03-30 | 2009-04-15 | 三菱化学株式会社 | Image forming apparatus |
CN103435358A (en) * | 2013-08-29 | 2013-12-11 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
CN107739203A (en) * | 2017-09-01 | 2018-02-27 | 广东风华高新科技股份有限公司 | The preparation method and ceramic slurry of ceramic slurry |
CN110372221A (en) * | 2018-04-13 | 2019-10-25 | 上海晶材新材料科技有限公司 | A kind of low-temperature co-fired ceramics green tape material and preparation method thereof |
CN108956699A (en) * | 2018-06-22 | 2018-12-07 | 西安创联电气科技(集团)有限责任公司 | A kind of NOXSensor ceramic chip insulating film band and insulating layer preparation process |
CN110683769A (en) * | 2019-10-25 | 2020-01-14 | 赣州中瓷科技有限公司 | Reinforced calcium-boron-silicon glass-ceramic composite material and preparation method thereof |
CN110790568A (en) * | 2019-11-29 | 2020-02-14 | 中国电子科技集团公司第四十三研究所 | Low-dielectric LTCC green tape and preparation method and application thereof |
CN113045204A (en) * | 2021-03-10 | 2021-06-29 | 安徽华封电子科技有限公司 | Low-loss low-temperature co-fired ceramic green tape and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
方亮主编: "《药用高分子材料学》", 31 August 2015, 北京:中国医药科技出版社 * |
甘孟瑜 等: "《大学化学 第4版》", 31 October 2014, 重庆大学出版社 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104193340B (en) | Doctor-blade casting process is for the preparation of the method for the AlN ceramic chips of multi-layer wire substrate and obtained AlN ceramic chips | |
CN113233773B (en) | LTCC substrate material and preparation method thereof | |
CN115958730B (en) | Processing method of flame-retardant hydrocarbon resin-based copper-clad plate | |
CN113754295B (en) | Low-dielectric modified glass fiber and preparation method and application thereof | |
CN114044684A (en) | LTCC (Low temperature Co-fired ceramic) green tape, slurry for preparing LTCC green tape and method | |
CN114213105A (en) | Preparation method for improving finished product yield of LTCC green tape | |
CN113999032A (en) | Silicon-boron-nitrogen fiber reinforced quartz ceramic material and preparation method thereof | |
CN108314430A (en) | A kind of Cellulose nanocrystal modified ceramic curtain coating green body and preparation method thereof | |
CN116284914B (en) | Preparation method and application of composite dielectric substrate | |
CN112420237A (en) | Conductive silver paste of filter and preparation method thereof | |
CN113149631B (en) | Method for preparing YAG transparent ceramic by colloidal state curing molding | |
CN107188407B (en) | Circuit board glass substrate manufactured by using alkali-free glass fiber waste silk and preparation method | |
CN113248256B (en) | Preparation method of strong toughness paste for ceramic optical fiber extrusion molding | |
CN111370217B (en) | Method for preparing permanent magnet through photocuring-assisted direct-writing 3D printing | |
CN113416066A (en) | LTCC substrate and preparation method and application thereof | |
CN111138172A (en) | Tape casting sheet and manufacturing method thereof | |
CN110937902A (en) | Preparation method of aluminum nitride ceramic substrate | |
CN117105640A (en) | Alumina ceramic substrate and preparation method thereof | |
CN113881082B (en) | High-tensile-strength ultrathin film material and preparation method thereof | |
CN110171957B (en) | Slurry, preparation method and application | |
CN116655392B (en) | Method for preparing alumina slurry and application of prepared alumina slurry in preparation of green ceramic chips | |
CN117164349A (en) | Alumina ceramic casting slurry, preparation method thereof and alumina ceramic green ceramic tape | |
CN115974531B (en) | Low-temperature cofired ceramic tape casting slurry and preparation method thereof | |
CN114133721B (en) | Preparation method of BMC resin and application of BMC resin in aspect of car lamp | |
CN113658756B (en) | Preparation method of electrode silver paste for 5G ceramic pedestal filter |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220215 |