CN114560683A - Environment-friendly low-toxicity ceramic tape-casting slurry and preparation method and application thereof - Google Patents
Environment-friendly low-toxicity ceramic tape-casting slurry and preparation method and application thereof Download PDFInfo
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- CN114560683A CN114560683A CN202210142334.7A CN202210142334A CN114560683A CN 114560683 A CN114560683 A CN 114560683A CN 202210142334 A CN202210142334 A CN 202210142334A CN 114560683 A CN114560683 A CN 114560683A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 106
- 231100000053 low toxicity Toxicity 0.000 title claims abstract description 38
- 238000010345 tape casting Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000007613 slurry method Methods 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 43
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- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 150000004767 nitrides Chemical class 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims description 82
- 239000010408 film Substances 0.000 claims description 38
- 239000000758 substrate Substances 0.000 claims description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
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- 238000000498 ball milling Methods 0.000 claims description 15
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- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 3
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- MQHNKCZKNAJROC-UHFFFAOYSA-N dipropyl phthalate Chemical compound CCCOC(=O)C1=CC=CC=C1C(=O)OCCC MQHNKCZKNAJROC-UHFFFAOYSA-N 0.000 description 2
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- 229910052574 oxide ceramic Inorganic materials 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
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- 206010029240 Neuritis Diseases 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- CASOXAYOCHCWQU-UHFFFAOYSA-N butan-2-one;ethanol Chemical compound CCO.CCC(C)=O CASOXAYOCHCWQU-UHFFFAOYSA-N 0.000 description 1
- LPRSRULGRPUBTD-UHFFFAOYSA-N butan-2-one;hydrate Chemical compound O.CCC(C)=O LPRSRULGRPUBTD-UHFFFAOYSA-N 0.000 description 1
- UVZGOOXAARJPHD-UHFFFAOYSA-N butan-2-one;methanol Chemical compound OC.CCC(C)=O UVZGOOXAARJPHD-UHFFFAOYSA-N 0.000 description 1
- 229940043232 butyl acetate Drugs 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- GCFHZZWXZLABBL-UHFFFAOYSA-N ethanol;hexane Chemical compound CCO.CCCCCC GCFHZZWXZLABBL-UHFFFAOYSA-N 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000000622 irritating effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 description 1
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
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- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
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- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- 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
- C04B35/10—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 aluminium oxide
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- 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
- C04B35/18—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 aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- 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
- C04B35/44—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 aluminates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- 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
Abstract
The invention provides environment-friendly low-toxicity ceramic tape-casting slurry which comprises the following components in parts by weight: 100 parts by weight of oxide and/or nitride ceramic powder; 55-70 parts by weight of a low-toxicity organic solvent; 1-4 parts by weight of a dispersant; 8-11 parts of a binder; 3-8 parts of a plasticizer; the low-toxicity organic solvent is a mixed solvent of absolute ethyl alcohol and butyl acetate, the solid content of powder of the tape-casting slurry is 50% -58%, and the viscosity is 1.5-10 Pa.s. The invention also provides a preparation method and application of the environment-friendly low-toxicity ceramic tape-casting slurry. The ceramic tape-casting slurry provided by the invention has wide universality of a tape-casting slurry system, can be applied to the preparation of ceramic slurries such as oxides, nitrides and the like, and has good thickness uniformity of a prepared biscuit film strip.
Description
Technical Field
The invention belongs to the field of preparation of casting slurry, and particularly relates to environment-friendly low-toxicity ceramic casting slurry as well as a preparation method and application thereof.
Background
The tape casting method is an important molding method for preparing a thin Ceramic material, is particularly suitable for industrial mass production, and is widely applied to the fields of Ceramic substrates for thick and thin film circuits, LTCC (Low Temperature Co-fired Ceramic), HTCC (High Temperature Co-fired Ceramic), MLCC (Multi-layer Ceramic Capacitors) and the like. With the development of the electronic ceramic industry, tape casting processes are also continuously developed to adapt to different types of ceramic powder and processes such as cutting, punching, printing and the like at the later stage.
For the tape casting of ceramic powder, it is most important to prepare tape casting slurry with high dispersibility and good stability, which puts high requirements on additives such as solvent, dispersant, binder and plasticizer. Common organic solvents include one or a mixture of two of absolute ethanol, butanone, toluene, xylene, butanol, and the like. Benzene solvents are the most commonly used and better choice for preparing excellent slurry, but the benzene solvents have high toxicity, and as human attention to environmental protection and personal health is gradually increased, benzene-containing solvent systems are gradually replaced by people, so that the selection of novel non-toxic or low-toxic organic solvents and additives becomes a development trend.
Absolute ethyl alcohol is widely used for preparing casting slurry as an organic solvent with low toxicity and low price, and general researchers can select two solvents to mix so as to improve the solubility of a dispersing agent, a binder, a plasticizer and the like in the organic solvent. Common benzene-free binary mixed solvents include ethanol-water, ethanol-butanone, ethanol-n-hexane, butanone-water, butanone-methanol, and the like. For example, patent document CN101483417A discloses a method for producing a black alumina substrate for multilayer wiring, in which a mixed solvent of ethanol and methyl ethyl ketone is used as a solvent. Wherein, butanone is a toxic solvent, has strong volatility, has obvious harm to respiratory tract mucous membrane and nerve center of human body, and has irritation to eyes, nose, throat and mucous membrane. N-hexane has anesthetic and irritant effects, and can irritate eyes and respiratory tract, and long-term contact can cause peripheral neuritis. Methanol has the greatest impact on the nervous system and the blood system of the human body, and methanol vapor can damage respiratory mucosa and vision of the human body. The above illustrates that several commonly used organic solvents are harmful to human body, and for the industrial production of ceramic substrates by tape casting, the harm to human body and environment must be one of important consideration conditions, and meanwhile, the purchase of these reagents is in the forbidden control range, which is not favorable for the large-scale popularization of these solvent systems in industrial production.
In addition to the low toxicity of the solvent, the relationship between the amount of the solvent, the solid content of the slurry and the viscosity of the slurry is also considered in order to prepare a casting slurry with high dispersibility and good stability. For example, under the condition of the same solvent dosage, the viscosity of the slurry taking esters as the solvent is higher, and a high-quality casting thick film cannot be obtained; and to obtain the same viscosity, the amount of solvent is increased, so that the solid content of the slurry is reduced, the film forming performance of the casting slurry is reduced due to the slurry with low solid content, the thickness size deviation of the prepared multilayer ceramic substrate is increased, and the shrinkage is increased, so that the later-stage debonding and sintering deformation are caused, and the performance of the ceramic substrate product is influenced.
Therefore, there is a need to further study a casting slurry having a high solid content and a relatively small amount of solvent for preparing a high-performance multilayer ceramic substrate.
Disclosure of Invention
Aiming at the limitations of the prior art, the invention aims to provide environment-friendly low-toxicity ceramic tape-casting slurry and a preparation method and application thereof.
In a first aspect, the invention provides an environment-friendly low-toxicity ceramic tape-casting slurry, which comprises the following components in parts by weight:
100 parts by weight of oxide and/or nitride ceramic powder;
55-70 parts by weight of a low-toxicity organic solvent;
1-4 parts by weight of a dispersant;
8-11 parts of a binder;
3-8 parts of a plasticizer;
the low-toxicity organic solvent is a mixed solvent of absolute ethyl alcohol and butyl acetate, the solid content of powder of the tape-casting slurry is 50% -58%, and the viscosity is 1.5-10 Pa.s.
Preferably, the oxide and/or nitride ceramic powder is selected from one of alumina powder, yttrium aluminum garnet powder, mullite powder and aluminum nitride powder.
Preferably, the dispersant is one or two mixtures selected from glycerol trioleate and polyvinylpyrrolidone.
Preferably, the binder is polyvinyl butyral.
Preferably, the plasticizer is one or two mixtures of dibutyl phthalate and polyethylene glycol.
In a second aspect, the present invention also provides a method for preparing the environment-friendly low-toxicity ceramic casting slurry, which comprises the following steps:
putting oxide and/or nitride ceramic powder, a low-toxicity organic solvent and a dispersing agent into a ball mill for primary ball milling;
and then adding a binder and a plasticizer for secondary ball milling to obtain the environment-friendly low-toxicity ceramic tape-casting slurry.
The rotation speed of the ball mill is 200-250 rpm, the primary ball milling time is 20-48 hours, and the secondary ball milling time is 16-24 hours.
Preferably, the method further comprises the steps of filtering and vacuum defoaming the slurry after the secondary ball milling.
Preferably, the viscosity of the obtained environment-friendly low-toxicity ceramic tape-casting slurry is 1.5-10 Pa.s.
In a third aspect, the invention also provides an application of the environment-friendly low-toxicity ceramic casting slurry in a ceramic substrate for a multilayer thick film or thin film circuit, wherein the ceramic substrate comprises a plurality of layers of thin films coated by the environment-friendly low-toxicity ceramic casting slurry, the thickness of each layer of thin film is 0.020-0.300 mm, and the thickness deviation of a single layer of thin film is not more than +/-0.007 mm.
According to the invention, the ceramic tape-casting slurry provided by the invention takes absolute ethyl alcohol and butyl acetate as solvents, and has relatively low cost, good environmental compatibility and low toxicity to human bodies. The solvent can be adjusted to have a volatilization speed close to the volatilization speed of the traditional toluene and xylene by adopting a mixed solvent of absolute ethyl alcohol and butyl acetate, and the control of a casting process is facilitated. The mixed solvent has good solubility to the binder, so that casting slurry with low viscosity and high solid content can be obtained, for example, the ceramic casting slurry provided by the invention has the powder solid content of 50-58%, the viscosity of the ceramic casting slurry in the solid content range can still be kept in a low viscosity state of 1.5-10 Pa.s, and the ceramic casting slurry is particularly suitable for preparing a multilayer thin film ceramic substrate by a casting method, for example, a ceramic biscuit film band with the thickness of tens of micrometers or even millimeter can be prepared, and the prepared biscuit film band has good thickness uniformity and wide application prospect.
The invention has the beneficial effects that:
(1) the ceramic tape-casting slurry provided by the invention adopts low-toxicity absolute ethyl alcohol and butyl acetate to replace the conventional common solvents of tape-casting slurry such as toluene, xylene and butanone, thereby avoiding serious environmental pollution and harm to human bodies.
(2) The ceramic tape-casting slurry provided by the invention has wide universality of a tape-casting slurry system, can be applied to the preparation of ceramic slurries such as oxides, nitrides and the like, and has good thickness uniformity of a prepared biscuit film strip.
(3) The ceramic tape-casting slurry provided by the invention has the advantages of simple slurry preparation process and low equipment cost, and is suitable for large-scale batch industrial production.
Drawings
Fig. 1 is a graph showing the tendency of viscosity to vary with shear rate in the casting slurry prepared in example 1 of the present invention.
Fig. 2 is a graph showing the tendency of viscosity to vary with shear rate in the casting slurry prepared in example 2 of the present invention.
Fig. 3 is a graph showing the tendency of viscosity to vary with the shear rate in the casting slurry prepared in example 3 of the present invention.
Fig. 4 is a graph showing the tendency of viscosity to vary with the shear rate in the casting slurry prepared in example 4 of the present invention.
FIG. 5 shows a green film of alumina ceramic prepared in example 1 of the present invention.
FIG. 6 is a yttrium aluminum garnet ceramic green film prepared in example 2 of the present invention.
FIG. 7 shows a mullite ceramic green film produced in example 3 of the present invention.
FIG. 8 shows an aluminum nitride ceramic green film produced in example 4 of the present invention.
FIG. 9 is a photograph of alumina ceramic substrates of different specifications prepared in example 1 of the present invention.
FIG. 10 shows the yttrium aluminum garnet and doped Ce prepared in example 2 of the present invention2O3A photograph of the yttrium aluminum garnet ceramic substrate.
FIG. 11 is a photograph of a mullite ceramic substrate made in accordance with example 3 of the present invention.
FIG. 12 is a photograph of an aluminum nitride ceramic substrate prepared in example 4 of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting.
The ceramic tape-casting slurry of the present invention is prepared by the following steps.
Step 1), putting oxide and/or nitride ceramic powder, a low-toxicity organic solvent and a dispersing agent into a ball mill for primary ball milling;
step 2), adding a binder and a plasticizer for secondary ball milling;
and 3), filtering and defoaming the slurry subjected to secondary ball milling in vacuum to obtain the environment-friendly low-toxicity ceramic tape-casting slurry.
In the invention, the rotation speed of the ball mill can be 200-250 rpm, the primary ball milling time can be 20-48 hours, and the secondary ball milling time can be 16-24 hours.
The ceramic powder in the ceramic tape-casting slurry comprises but is not limited to one of alumina powder, yttrium aluminum garnet powder, mullite powder and aluminum nitride powder, and the grain size of the ceramic powder can be 0.1-10 mu m.
The mixed solvent in the ceramic tape-casting slurry can be composed of alcohols and esters, wherein the alcohols can be one or a mixture of more of ethanol, propanol, isopropanol, glycol, n-butyl alcohol, isobutanol and tert-butyl alcohol, the esters are one or a mixture of more of methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate and isobutyl acetate, the mixed solvent is defined as the mixed solvent of absolute ethyl alcohol and butyl acetate, the mass percent of the mixed solvent in the ceramic powder can be 55-70%, and the volume ratio of the absolute ethyl alcohol to the butyl acetate in the mixed solvent can be 1: 1-1: 2. In the ceramic tape-casting slurry, the dosage of the solvent is relatively less, the viscosity of the formed tape-casting slurry is lower, and the solvent is volatilized quickly.
The dispersant in the ceramic casting slurry of the present invention may be one or a mixture of two of triolein and polyvinylpyrrolidone, and triolein is preferred in the embodiment of the present invention. In the ceramic tape-casting slurry of the present invention, the dispersant may account for 1% to 4% by mass of the ceramic powder.
The binder in the ceramic tape-casting slurry can be polyvinyl butyral, and the molecular weight of the binder can be 40000-70000. The plasticizer may be a phthalate, polyethylene glycol or a mixture of both. Wherein the phthalate is at least one of dioctyl phthalate, di (2-ethylhexyl) phthalate, dibutyl phthalate, butyl benzyl phthalate, diethyl phthalate, dipropyl phthalate and diisobutyl phthalate. The molecular weight of the polyethylene glycol can be 200-600. In the plasticizer consisting of the mixture of the phthalic acid ester and the polyethylene glycol, the mass ratio of the phthalic acid ester to the polyethylene glycol is 1: 3-3: 1, and 1:1 is preferred. In the ceramic tape-casting slurry, the mass percent of the binder in the ceramic powder can be 8-11%, the mass percent of the plasticizer in the ceramic powder can be 3-8%, and the mass ratio of the binder to the plasticizer can be 1: 1-4: 1.
The environment-friendly low-toxicity ceramic tape-casting slurry provided by the invention can be prepared into a ceramic substrate for a multilayer thick film or thin film circuit, and comprises the following steps:
step (1), preparing uniform and compact film-shaped ceramic biscuit by adopting a tape casting method. And (3) defoaming and filtering the prepared ceramic casting slurry, casting on a clean and smooth plastic film belt by using a scraper, setting the drying temperature of a casting machine, and drying and coiling the biscuit film when the biscuit film reaches a reel.
And (2) cutting the film-shaped biscuit obtained by casting into blank sheets, and laminating and carrying out warm isostatic pressing treatment on the cut blank sheets.
And (3) cutting the substrate biscuit subjected to the warm isostatic pressing treatment into a proper size, and then performing debonding and sintering to obtain the ceramic substrate.
The ceramic tape-casting slurry provided by the invention takes absolute ethyl alcohol and butyl acetate as solvents, and has relatively low cost, good environmental compatibility and low toxicity to human bodies. The solvent can be adjusted to have a volatilization speed close to the volatilization speed of the traditional toluene and xylene by adopting a mixed solvent of absolute ethyl alcohol and butyl acetate, and the control of a casting process is facilitated. The mixed solvent has good solubility to the adhesive, so that casting slurry with low viscosity and high solid content can be obtained, for example, the ceramic casting slurry of the invention has the powder solid content of 50-58%, the viscosity of the ceramic casting slurry in the solid content range can still be kept in a low viscosity state of 1.5-10 Pa.s, the ceramic casting slurry is particularly suitable for preparing multilayer thin film ceramic substrates by a casting method, for example, ceramic biscuit film bands with the size of tens of microns or even millimeters can be prepared, and the prepared biscuit film bands have good thickness uniformity and good flexibility and have wide application prospect.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and do not necessarily limit the specific values to the examples below.
Example 1:
selecting high-purity alumina powder as raw material, wherein the content of alumina is above 99.9%, and the grain diameter D is preferred50In the alumina powder of about 400nm, the mixture of absolute ethyl alcohol and butyl acetate is used as a solvent, and triolein is used as a dispersant, and the mixture is mixed for 24 hours on a horizontal tank mill, wherein the mixing speed is about 250 revolutions per minute. Then polyvinyl butyral is added into the uniformly dispersed slurry to serve as a binder, dibutyl phthalate and polyethylene glycol are used as plasticizers, and the mass ratio of the binder to the plasticizers is about 3.7. The solids content of the powder in the slurry was 58%. Mixing was then continued on the horizontal jar mill for 16 hours to obtain a casting slurry.
And filtering the casting slurry, defoaming for 1 hour through vacuum stirring, testing the viscosity of the slurry to be 4.19 Pa.s at 100/s, and obtaining the aluminum oxide ceramic blank film by casting on a casting machine.
By adopting the alumina ceramic casting slurry prepared by the embodiment, a biscuit film strip with uniform thickness is obtained through casting forming, when the height of the casting scraper is set to be 0.560mm, the average thickness of the biscuit film strip is 0.165mm, the thickness deviation is +/-0.006 mm, and when the number of laminated layers is 5, an alumina ceramic substrate with the thickness of about 0.635mm can be prepared through sintering. The slurry preparation process and equipment are simple, and low-cost batch production is easy to realize.
Example 2:
high-purity alumina and yttria powder (the molar ratio of the two is 5:3) are selected as raw materials, and 0.3 wt% and 0.4 wt% Ce are added in a comparative way2O3The mixed powder of (1) is prepared by mixing a mixture of absolute ethyl alcohol and butyl acetate as a solvent and triolein as a dispersing agent on a horizontal tank mill for 48 hours at a mixing speed of about 250 revolutions per minute. Then polyvinyl butyral is added into the uniformly dispersed slurry to serve as a binder, dibutyl phthalate and polyethylene glycol are used as plasticizers, and the mass ratio of the binder to the plasticizers is about 2.5. The solids content of the powder in the slurry was 52%. Mixing was then continued on a horizontal jar mill for 24 hours to obtain a casting slurry.
Filtering the casting slurry, removing bubbles for 2 minutes at high speed by adopting a non-intrusive material homogenizer, testing the viscosity of the slurry to be 2.13 Pa.s when the viscosity is 100/s, and obtaining the yttrium aluminum garnet ceramic blank film by casting on the casting machine.
By adopting the yttrium aluminum garnet ceramic casting slurry prepared in the embodiment, a green body film strip with uniform thickness is obtained through casting forming, when the height of a casting scraper is set to be 0.300mm, the average thickness of the green body film strip is 0.082mm, the thickness deviation is +/-0.005 mm, and when the number of laminated layers is 4, the yttrium aluminum garnet ceramic substrate with the thickness of about 0.26mm can be prepared through vacuum sintering. The slurry preparation process and equipment are simple, and low-cost batch production is easy to realize.
Example 3:
high-purity alumina and silicon dioxide powder (the molar ratio of the two is 63:37) are selected as raw materials, a mixture of absolute ethyl alcohol and butyl acetate is used as a solvent, triolein is used as a dispersing agent, and the raw materials are mixed on a horizontal tank mill for 24 hours, wherein the mixing speed is about 200 revolutions per minute. Then polyvinyl butyral is added into the uniformly dispersed slurry to serve as a binder, dibutyl phthalate and polyethylene glycol are used as plasticizers, and the mass ratio of the binder to the plasticizers is about 2.5. The solids content of the powder in the slurry was 55.6%. Mixing was then continued on the horizontal jar mill for 20 hours to obtain a casting slurry.
And filtering the casting slurry, defoaming for 2 minutes at a high speed by adopting a non-intrusive material homogenizer, testing that the viscosity of the slurry is 3.53 Pa.s when the viscosity is 100/s, and the slurry has the shear thinning performance, and then casting on the casting machine to obtain the mullite ceramic biscuit film.
By adopting the mullite ceramic casting slurry prepared by the embodiment, a biscuit film band with uniform thickness is obtained through casting forming, when the height of the casting scraper is set to be 0.300mm, the average thickness of the biscuit film band is 0.081mm, the thickness deviation is +/-0.002 mm, and when the number of laminated layers is 12, the mullite ceramic substrate with the thickness of about 0.81mm can be prepared through sintering. The slurry preparation process and equipment are simple, and low-cost batch production is easy to realize.
Example 4:
high-purity aluminum nitride powder is selected as a raw material, the particle size of the powder is about 1.5 mu m, a mixture of absolute ethyl alcohol and butyl acetate is used as a solvent, triglyceride is used as a dispersing agent, and the mixture is mixed for 20 hours on a horizontal tank mill at the mixing speed of about 250 revolutions per minute. Then polyvinyl butyral is added into the uniformly dispersed slurry to serve as a binder, dibutyl phthalate and polyethylene glycol are used as plasticizers, and the mass ratio of the binder to the plasticizers is about 2.5. The solid content of the powder in the slurry was 50%. Mixing was then continued on the horizontal jar mill for 24 hours to obtain a casting slurry.
And filtering the casting slurry, defoaming for 2 minutes at a high speed by adopting a non-intrusive material homogenizer, testing that the viscosity of the slurry is 1.78 Pa.s when the viscosity is 100/s, and the slurry has the shear thinning performance, and then casting on the casting machine to obtain the aluminum nitride ceramic blank film.
By adopting the aluminum nitride ceramic casting slurry prepared by the embodiment, a biscuit film belt with uniform thickness is obtained through casting forming, when the height of the casting scraper is set to be 0.300mm, the average thickness of the biscuit film belt is 0.075mm, the thickness deviation is +/-0.004 mm, and when the number of laminated layers is 6, an aluminum nitride ceramic substrate with the thickness of about 0.38mm can be prepared through sintering. The slurry preparation process and equipment are simple, and low-cost batch production is easy to realize.
Comparative example 1:
high-purity alumina powder is selected as a raw material, the content of alumina is more than 99.9 percent, and the grain diameter D50The method is characterized in that a mixture of absolute ethyl alcohol and xylene is used as a solvent with the mass ratio of the absolute ethyl alcohol to the xylene being 1:2, triolein is used as a dispersing agent, and the mixture is mixed for 24 hours on a horizontal tank mill at the mixing speed of about 250 revolutions per minute. Then polyvinyl butyral is added into the uniformly dispersed slurry to serve as a binder, dibutyl phthalate and polyethylene glycol are used as plasticizers, and the mass ratio of the binder to the plasticizers is about 3.7. The solids content of the powder in the slurry was 58%. Mixing was then continued on the horizontal jar mill for 16 hours to obtain a casting slurry.
And filtering the casting slurry, defoaming for 1 hour through vacuum, testing the viscosity of the slurry to be 4.89 Pa.s at 100/s, and obtaining the aluminum oxide ceramic blank film by casting on a casting machine.
The alumina biscuit film belt is obtained by casting and molding by adopting the alumina ceramic casting slurry prepared by the comparative example, when the height of the casting scraper is set to be 0.450mm, the average thickness of the biscuit film belt is 0.116mm, the thickness deviation is +/-0.009 mm, and when the laminated layer number is 8, the alumina ceramic substrate with the thickness of about 0.74mm can be prepared by sintering. This comparative example demonstrates that the low-toxicity mixed solvents (absolute ethyl alcohol and butyl acetate) of the present invention can obtain casting slurry with similar solid content and viscosity compared with the toxic mixed solvents (absolute ethyl alcohol and xylene), the thickness uniformity of the prepared casting film band is even better than that of the toxic mixed solvents (absolute ethyl alcohol and xylene), and the ceramic casting slurry can be prepared by replacing the toxic mixed solvents.
Fig. 1 is a graph showing the tendency of viscosity to vary with shear rate in the casting slurry prepared in example 1 of the present invention.
Fig. 2 is a graph showing the tendency of viscosity to vary with shear rate in the casting slurry prepared in example 2 of the present invention.
Fig. 3 is a graph showing the tendency of viscosity to vary with the shear rate in the casting slurry prepared in example 3 of the present invention.
Fig. 4 is a graph showing the tendency of viscosity to vary with the shear rate in the casting slurry prepared in example 4 of the present invention.
FIG. 5 shows a green alumina ceramic film prepared in example 1 of the present invention.
FIG. 6 is a yttrium aluminum garnet ceramic green film prepared in example 2 of the present invention.
FIG. 7 shows a mullite ceramic green film produced in example 3 of the present invention.
FIG. 8 shows an aluminum nitride ceramic green film produced in example 4 of the present invention.
FIG. 9 is a photograph of alumina ceramic substrates of different specifications prepared in example 1 of the present invention.
FIG. 10 shows the yttrium aluminum garnet and doped Ce prepared in example 2 of the present invention2O3A photograph of the yttrium aluminum garnet ceramic substrate.
FIG. 11 is a photograph of a mullite ceramic substrate made in accordance with example 3 of the present invention.
FIG. 12 is a photograph of an aluminum nitride ceramic substrate prepared in example 4 of the present invention.
As can be seen from FIGS. 1 to 12, the viscosity of the ceramic casting slurry prepared by the invention can still be kept in a low viscosity state of 1.5 to 10 Pa.s under the condition that the solid content of the ceramic casting slurry is 50 to 58 percent, a ceramic biscuit film strip with the thickness of dozens of micrometers or even millimeter can be prepared, and the prepared biscuit film strip has good thickness uniformity and good flexibility.
Claims (10)
1. The environment-friendly low-toxicity ceramic tape-casting slurry is characterized by comprising the following components in parts by weight:
the low-toxicity organic solvent is a mixed solvent of absolute ethyl alcohol and butyl acetate, the solid content of powder of the tape-casting slurry is 50% -58%, and the viscosity is 1.5-10 Pa.s.
2. The cast slurry of environmentally friendly and low toxicity ceramic as claimed in claim 1, wherein the oxide and/or nitride ceramic powder is selected from one of alumina powder, yttrium aluminum garnet powder, mullite powder and aluminum nitride powder.
3. The environmentally friendly, low toxicity ceramic casting slurry of claim 1, wherein the dispersant is one or a mixture of two of glyceryl trioleate or polyvinylpyrrolidone.
4. The environmentally friendly, low toxicity ceramic casting slurry of claim 1, wherein the binder is polyvinyl butyral.
5. The casting slurry for environment-friendly and low-toxicity ceramics according to claim 1, wherein the plasticizer is one or a mixture of two of dibutyl phthalate and polyethylene glycol.
6. A method for preparing environment-friendly low-toxicity ceramic casting slurry according to any one of claims 1 to 5, which comprises the following steps:
putting oxide and/or nitride ceramic powder, a low-toxicity organic solvent and a dispersing agent into a ball mill for primary ball milling;
and then adding a binder and a plasticizer for secondary ball milling to obtain the environment-friendly low-toxicity ceramic tape-casting slurry.
7. The preparation method according to claim 6, wherein the rotation speed of the ball mill is 200-250 rpm, the primary ball milling time is 20-48 hours, and the secondary ball milling time is 16-24 hours.
8. The preparation method according to claim 6 or 7, further comprising the steps of filtering and vacuum defoaming the slurry after the secondary ball milling.
9. The preparation method according to claim 8, wherein the viscosity of the obtained environment-friendly low-toxicity ceramic casting slurry is 1.5-10 Pa-s.
10. Use of the environmentally friendly low toxicity ceramic casting paste according to any one of claims 1 to 5 in ceramic substrates for multilayer thick film or thin film circuits, wherein the ceramic substrates comprise a plurality of thin films prepared from the environmentally friendly low toxicity ceramic casting paste according to any one of claims 1 to 5, the thickness of each thin film is 0.020-0.300 mm, and the thickness deviation of a single layer of the thin film is not more than ± 0.007 mm.
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