CN111333333A - Preparation method of low-temperature co-fired ceramic material for 3D printing molding - Google Patents

Preparation method of low-temperature co-fired ceramic material for 3D printing molding Download PDF

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CN111333333A
CN111333333A CN202010139249.6A CN202010139249A CN111333333A CN 111333333 A CN111333333 A CN 111333333A CN 202010139249 A CN202010139249 A CN 202010139249A CN 111333333 A CN111333333 A CN 111333333A
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temperature
low
microcrystalline glass
ceramic material
ceramic
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仲怀民
孟祥龙
肖悦
肖皓中
蔡爱武
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Jiangsu New Lihe Grinding Tool Technology Co ltd
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Jiangsu New Lihe Grinding Tool Technology Co ltd
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    • 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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • 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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • 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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • 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
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax

Abstract

The invention discloses a preparation method of low-temperature co-fired ceramic for 3D printing and molding, which relates to an additive manufacturing domain2、Al2O3、B2O3、Na2O, CaO, and the like, and the microcrystalline glass material is obtained after melting and crushing。Al2O3、ZrO2And ball-milling the ceramic material and the glass ceramics to obtain the low-temperature co-fired ceramic material. The microcrystalline glass and the ceramic can be reliably connected in the 3D printing process, and meanwhile, the microcrystalline ceramic can permeate into gaps of ceramic particles, so that the compactness of the material is effectively improved.

Description

Preparation method of low-temperature co-fired ceramic material for 3D printing molding
Technical Field
The invention relates to a preparation method of a 3D printing formed low-temperature co-fired ceramic material, belonging to the field of additive manufacturing and rapid prototyping manufacturing.
Background
The 3D printing technique, also called additive manufacturing technique, is a technique of constructing a solid body by using high-energy beams such as laser, electron beam, or arc as heat sources and by using powdered or filamentous materials in a layer-by-layer stacking manner on the basis of a digital model. 3D printing is a representative advanced manufacturing technology, and compared with the traditional manufacturing process, the method has fundamental transformation on the aspects of forming principle, raw material form, product performance and the like, and is considered as a revolutionary breakthrough of the manufacturing technology. The 3D printing technology covers the advantages of multiple high technologies such as graphic processing, digital information and control, laser technology, electromechanical technology and material technology of a computer, wherein the material technology is a key common technology of the 3D printing technology and is an important mark for measuring the advanced manufacturing development level of the state.
Materials currently available for 3D printing technology fall into three broad categories, metal, ceramic and polymer. Wherein the metal includes magnesium alloys, aluminum alloys, and superalloys. The polymer is mainly acrylonitrile-butadiene-styrene (ABS), polylactic acid (PLA) and the like. The ceramic comprises Al2O3、ZrO2、Si3N4Mixtures thereof and the like. The ceramic material has the properties of high strength, high hardness, high temperature resistance, corrosion resistance and the like, and is widely applied to the fields of aerospace, biomedicine, electronic information, mechanical manufacturing and the like.
In the 3D printing of ceramic materials, lasers are often used as heat sources to scan paths to selected areas that are digitized. Heat is transferred in the laser beam onto the ceramic material. Under the action of heat, the ceramic material completes the stages of material migration, crystal boundary movement, crystal boundary disappearance and the like to grow crystal grains, thereby realizing the molding of the ceramic material. At present, the ceramic material needs to be formed under the action of a bonding agent in the sintering process. The adhesive needs to meet the characteristics of low melting point, low liquid phase viscosity, good wettability with a base material and the like. The adhesive includes inorganic adhesive, organic adhesive and metal adhesiveAdhesives of three general classes, e.g. NH4H2PO4Epoxy, nylon, Al powder, and the like.
The low-temperature co-fired ceramic material consists of microcrystalline glass and ceramic and has the characteristics of high strength, good chemical property stability and the like. Due to the addition of the ceramic phase, the thermal expansion coefficient of the low-temperature co-fired ceramic material can be conveniently regulated and controlled. In the aspect of a microscopic interface, ceramic particles in the ceramic phase can play a pinning role in crack expansion and play a toughening and reinforcing effect. Meanwhile, the microcrystalline glass and the ceramic can be effectively combined at the interface, and the microcrystalline glass and the ceramic can penetrate into gaps of ceramic particles in a high-temperature environment, so that the density of the ceramic material is improved. At present, in the aspect of manufacturing and application of 3D printing materials, no related research report of low-temperature co-fired ceramic materials exists, and the technology of the invention aims to make up for the blank in the prior art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a preparation method of a low-temperature co-fired ceramic material for 3D printing and forming, which mixes microcrystalline glass frit powder and ceramic powder in proportion, simultaneously limits the respective components and proportions of the microcrystalline glass frit powder and the ceramic powder, makes up the blank that the low-temperature co-fired ceramic material does not exist in the prior art, and can improve the strength and the compactness of the 3D printing and forming material.
The technology of the invention is realized as follows:
a preparation method of a low-temperature co-fired ceramic material for 3D printing molding is characterized by comprising the following steps:
step one, weighing microcrystalline glass raw materials in proportion, uniformly mixing, carrying out ball milling for 1-12 h, then carrying out high-temperature smelting, carrying out water quenching, drying and crushing after smelting, and carrying out ball milling for 1-12 h to obtain microcrystalline glass powder;
step two, weighing ceramic raw materials according to a proportion, uniformly mixing, and performing ball milling for 1-12 hours to obtain ceramic powder;
and step three, mixing the microcrystalline glass material powder obtained in the step one with the ceramic powder obtained in the step two in proportion, ball-milling the mixture for 1-12 hours by taking absolute ethyl alcohol as a medium, and drying and sieving the mixture to obtain the low-temperature co-fired ceramic material for 3D printing and forming.
Further, the smelting process in the step one comprises the following steps: and smelting the ball-milled microcrystalline glass raw material for 0.5-4 h at 1200-1500 ℃. Wherein the preferable smelting temperature is 1200-1400 ℃.
Further, the microcrystalline glass raw material in the first step comprises SiO2、Al2O3、B2O3The microcrystalline glass raw material also contains Na2O、Li2One or more of O, MgO and ZnO; wherein the mass ratio of each component is 50-60% SiO2、5~10%Al2O3、10~20%B2O3、5~10%Na2O、5~10%Li2O, 5-10% of MgO and 5-10% of ZnO. Wherein SiO is2、Al2O3、B2O3A network skeleton constituting the microcrystalline glass material, and Na2O、Li2The refractoriness, hardness and bending strength of the microcrystalline glass can be adjusted by O, MgO and ZnO, so that the physical properties of the material can be controlled more thoroughly. At the same time, Na is added2O、Li2The O, MgO and ZnO can also adjust the fluidity of the microcrystalline glass in a high-temperature state, so that the microcrystalline glass can flow to fill the pores among ceramic particles, and the compactness of the low-temperature co-fired ceramic material is improved.
Further, the ceramic raw material in the second step contains Al2O3、ZrO2One or a combination of the two, wherein the mass ratio of each component is 0-100% of Al2O3，0~50%ZrO2。Al2O3And ZrO2All are ceramic materials with excellent performance, and all have the characteristics of high hardness, good wear resistance and the like. Due to Al2O3And ZrO2Is dispersed and distributed in the microcrystalline glass, so that the ceramic Al2O3And ZrO2Can play a role of pinning and prevent cracks from continuously propagating in the microcrystalline glass, thereby improving the bending strength of the low-temperature co-fired ceramic.
Further, in the second step, the addition ratio of the microcrystalline glass frit powder to the ceramic powder is 1: 9-9: 1.
furthermore, in the second step, the preferable adding ratio of the microcrystalline glass frit powder to the ceramic powder is 1: 1.
The beneficial effects of the invention and the prior art are as follows:
the low-temperature co-fired ceramic material prepared by the invention has the characteristic of simple and convenient preparation method. After 3D printing, the low-temperature co-fired ceramic material has the advantages of high strength, high density, good chemical stability, easy adjustment of thermal expansion coefficient and the like.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention more clear, the present invention is further described in detail by the following examples. It should be noted that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The microcrystalline glass raw materials are weighed according to the following proportion: 50% SiO2、5%Al2O3、10%B2O3、5%Na2O、10%Li2And O, 10% of MgO and 10% of ZnO are uniformly mixed, the smelting temperature is 1400 ℃, the mixture is smelted for 1h, and the microcrystalline glass material is obtained after water quenching, drying and crushing and ball milling for 6 h. Weighing the following ceramic raw materials in proportion: 90% Al2O3And 10% ZrO2And uniformly mixing, and ball-milling for 6 hours to obtain the ceramic material. Mixing the microcrystalline glass material and the ceramic material according to a ratio of 1:1, ball-milling for 6 hours in an absolute ethyl alcohol medium, drying and sieving to obtain the low-temperature co-fired ceramic material.
And (3) testing results: bending strength: 106.7 MPa; vickers hardness: 5.2 GPa; density: 3.5g/mm3。
Example 2
The microcrystalline glass raw materials are weighed according to the following proportion: 50% SiO2、10%Al2O3、20%B2O3、5%Na2O、5%Li2O, 5 percent of MgO and 5 percent of ZnO are evenly mixed, the smelting temperature is 1300 ℃, the smelting is carried out for 1.5h, and the microcrystalline glass material is obtained after water quenching, drying and crushing and ball milling for 5 h. Weighing the following ceramic raw materials in proportion: 50% Al2O3And 50% ZrO2Mixing evenly, ball milling for 6 hours to obtain ceramic material. Mixing the microcrystalline glass material and the ceramic material according to a ratio of 2:1, ball-milling for 6 hours in an absolute ethyl alcohol medium, drying and sieving to obtain the low-temperature co-fired ceramic material.
And (3) testing results: bending strength: 119.1 MPa; vickers hardness: 4.3 GPa; density: 3.9g/mm3。
Example 3
The microcrystalline glass raw materials are weighed according to the following proportion: 60% SiO2、5%Al2O3、10%B2O3、10%Na2O、5%Li2O, 5 percent of MgO and 5 percent of ZnO are evenly mixed, the smelting temperature is 1500 ℃, the smelting is carried out for 1.5h, and the microcrystalline glass material is obtained after water quenching, drying and crushing and ball milling for 5 h. Weighing the following ceramic raw materials in proportion: 100% Al2O3And ball-milling the ceramic material for 6 hours. Mixing the microcrystalline glass material and the ceramic material according to a ratio of 1:1, ball-milling for 6 hours in an absolute ethyl alcohol medium, drying and sieving to obtain the low-temperature co-fired ceramic material.
And (3) testing results: bending strength: 126.7 MPa; vickers hardness: 5.5 GPa; density: 3.3g/mm3。
Comparative example
The microcrystalline glass raw materials are weighed according to the following proportion: 60% SiO2、5%Al2O3、10%B2O3、10%Na2O、5%Li2O, 5 percent of MgO and 5 percent of ZnO are evenly mixed, the smelting temperature is 1500 ℃, the smelting is carried out for 1.5h, and the microcrystalline glass material is obtained after water quenching, drying and crushing and ball milling for 5 h.
And (3) testing results: bending strength: 70.5 MPa; vickers hardness: 4.0 GPa; density: 3.1g/mm3。
Through the examples 1-3 and the comparative example, the bending strength, the Vickers hardness and the density of the low-temperature co-fired ceramic are higher than those of the microcrystalline glass material. The contrast test shows that the low-temperature ceramic material has better performance than the microcrystalline glass material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.

Claims (6)

1. A preparation method of a low-temperature co-fired ceramic material for 3D printing molding is characterized by comprising the following steps:
step one, weighing microcrystalline glass raw materials in proportion, uniformly mixing, carrying out ball milling for 1-12 h, then carrying out high-temperature smelting, carrying out water quenching, drying and crushing after smelting, and carrying out ball milling for 1-12 h to obtain microcrystalline glass powder;
step two, weighing ceramic raw materials according to a proportion, uniformly mixing, and performing ball milling for 1-12 hours to obtain ceramic powder;
and step three, mixing the microcrystalline glass material powder obtained in the step one with the ceramic powder obtained in the step two in proportion, ball-milling the mixture for 1-12 hours by taking absolute ethyl alcohol as a medium, and drying and sieving the mixture to obtain the low-temperature co-fired ceramic material for 3D printing and forming.
2. The preparation method of the low-temperature co-fired ceramic material for 3D printing and forming according to claim 1, wherein the melting process in the first step is as follows: and smelting the ball-milled microcrystalline glass raw material for 0.5-4 h at 1200-1500 ℃.
3. The method for preparing a low-temperature co-fired ceramic material for 3D printing and forming according to claim 1, wherein the microcrystalline glass raw material in the first step comprises SiO2、Al2O3、B2O3And Na2O、Li2One or more of O, MgO and ZnO; wherein the mass ratio of each component is 50-60% SiO2、5~10%Al2O3、10~20%B2O3、5~10%Na2O、5~10%Li2O、5~10%MgO、5~10%ZnO。
4. The method according to claim 1, wherein the ceramic material in the second step comprises Al2O3、ZrO2One or both ofWherein the mass ratio of each component is 0-100% of Al2O3、0~50%ZrO2。
5. The preparation method of the low-temperature co-fired ceramic material for 3D printing and forming according to claim 1, wherein the addition ratio of the microcrystalline glass frit powder to the ceramic powder in the second step is 1: 9-9: 1.
6. the method for preparing the low-temperature co-fired ceramic material for 3D printing and forming according to claim 5, wherein the addition ratio of the microcrystalline glass frit powder to the ceramic powder in the second step is 1: 1.
CN202010139249.6A 2020-03-03 2020-03-03 Preparation method of low-temperature co-fired ceramic material for 3D printing molding Pending CN111333333A (en)

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Cited By (8)

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CN113415999A (en) * 2021-05-25 2021-09-21 赵凤宇 Micro glass metal 3D printing micro powder for liquid printer
CN113754409A (en) * 2021-09-17 2021-12-07 深圳陶陶科技有限公司 Low-temperature sintered glass ceramic powder and preparation method and application thereof
CN114230321A (en) * 2021-12-08 2022-03-25 山东工业陶瓷研究设计院有限公司 Preparation method of LTCC substrate
CN114477968A (en) * 2022-03-09 2022-05-13 上海晶材新材料科技有限公司 LTCC raw material belt material, LTCC substrate and preparation method
CN114890776A (en) * 2022-05-07 2022-08-12 山东工业陶瓷研究设计院有限公司 Low-temperature co-fired glass/ceramic composite material and preparation method thereof
CN115124329A (en) * 2022-06-27 2022-09-30 清华大学深圳国际研究生院 LTCC substrate and preparation method thereof
CN115340376A (en) * 2022-06-28 2022-11-15 清华大学深圳国际研究生院 Ceramic substrate for LTCC (Low temperature Co-fired ceramic), and preparation method and application thereof
CN115385666A (en) * 2022-08-29 2022-11-25 安徽工业技术创新研究院 High-thermal-conductivity low-temperature co-fired ceramic material and preparation method thereof

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