CN113336479B - Cordierite-based microcrystalline glass high-temperature binder and preparation method and application thereof - Google Patents
Cordierite-based microcrystalline glass high-temperature binder and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a cordierite-based microcrystalline glass high-temperature binder, which comprises the following raw materials in parts by weight: cordierite micropowder, low-temperature glass frit powder and adhesive; the cordierite micropowder comprises 46-54 wt% of clay, 33-37 wt% of talcum, 11-19 wt% of alumina, and the low-temperature glass frit powder comprises 12-15 wt% of MgO, 36-10 wt% of Al2O and SiO 2 58～60wt％、B 2 O 3 1～3wt％、ZrO 2 4～6wt％、K 2 O 3～5wt％、Na 2 3-5 wt% of O; low-temperature glass frit powder and cordierite micro powder with the mass ratio of = 2-7:3; the amount of the binder is 15-18 wt% of the total amount of the cordierite micro powder and the low-temperature glass frit powder. In addition, a preparation method and application of the cordierite-based microcrystalline glass high-temperature binder are provided. The invention directly uses the synthesized cordierite micro powder, and can better control the types, the quantity and the particle size of crystals in the glass, thereby achieving the purpose of regulating and controlling the performance of the cordierite-based microcrystalline glass; and greatly simplifies the heat treatment process, thereby effectively reducing the product cost.
Description
Technical Field
The invention relates to the technical field of binder materials, in particular to a cordierite-based microcrystalline glass high-temperature binder, a preparation method and application thereof.
Background
The cordierite-based glass ceramic is a widely applied material, has the advantages of low thermal expansion coefficient, small dielectric constant, good mechanical property and the like, and can be used as building materials, circuit substrate packaging agents, ceramic binders and the like. However, in the traditional preparation method, the microcrystalline precipitated in the base glass usually adopts a multi-stage heat treatment mode, so that the requirements on temperature, time and equipment are very strict, the crystallization behavior of the glass is difficult to regulate and control, and as a result, the types, the number and the size of crystals are difficult to effectively control, and the difficulty is increased for regulating and controlling the performance of the material. In addition, the conventional method includes firing steps such as sintering heat treatment and nucleation heat treatment in addition to the crystallization heat treatment, which not only prolongs the preparation time, but also increases the number of equipment and sites, and affects the production cost. Therefore, how to simplify the preparation process of cordierite-based glass ceramics is a problem to be solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a cordierite-based microcrystalline glass high-temperature binder, and adopts a mode of directly adding cordierite micro powder so as to better control the types, the number and the particle sizes of crystals in glass, thereby achieving the purpose of regulating and controlling the performance of the cordierite-based microcrystalline glass. The invention also aims to provide a preparation method and application of the cordierite-based microcrystalline glass high-temperature binder.
The aim of the invention is realized by the following technical scheme:
the invention provides a cordierite-based microcrystalline glass high-temperature binder, which comprises the following raw materials: cordierite micropowder, low-temperature glass frit powder and adhesive; the cordierite micro powder comprises 46-54 wt% of clay, 33-37 wt% of talcum and 11-19 wt% of alumina, and the low-temperature glass frit powder comprises 12-15 wt% of MgO and 12-15 wt% of Al 2 O 3 6～10wt％、SiO 2 58～60wt％、B 2 O 3 1～3wt％、ZrO 2 4～6wt％、K 2 O 3～5wt％、Na 2 3-5 wt% of O; the mass ratio of the low-temperature glass frit powder to the cordierite micro powder is=2-7:3; the usage amount of the binder is 15-18 wt% of the total amount of the cordierite micro powder and the low-temperature glass frit powder.
Further, the clay is kaolin, ball clay or montmorillonite; the alumina is alpha-alumina or gamma-alumina. The particle size of the cordierite micro powder is 10-75 mu m; the particle size of the low-temperature glass frit powder is 100-325 meshes. The adhesive is one or two of water, PVA water solution with the concentration of 6wt%, dextrin and waste paper pulp.
The other object of the invention is achieved by the following technical scheme:
the preparation method of the cordierite-based microcrystalline glass high-temperature binder provided by the invention comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing the mixture at 1200-1350 ℃ and then carrying out crushing and ball milling to obtain micron-sized cordierite micro powder;
(2) Preparation of low-temperature glass frit powder
Proportioning the raw materials of the low-temperature glass frit powder, uniformly mixing, melting to prepare glass liquid, clarifying, homogenizing, performing water quenching treatment to obtain glass particles, crushing, ball milling and sieving to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
And uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and then doping the binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder.
The application of the binder obtained by the preparation method of the cordierite-based microcrystalline glass high-temperature binder provided by the invention is as follows: the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 1-2 hours at 800-900 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
The invention has the following beneficial effects:
(1) The invention directly adopts the synthesized cordierite micropowder as the microcrystal in the glass, and the type, the number and the size of crystals in the glass are easy to control, so that the properties of the microcrystal glass are easier to regulate and control, and the problems faced by the traditional method are solved.
(2) The cordierite-based glass ceramic obtained by the invention only needs one sintering heat treatment, no nucleation and crystallization heat treatment, and greatly simplifies the heat treatment process, thereby reducing the use of equipment, time and places and being beneficial to reducing the product cost.
(3) The invention adopts a mode of mixing cordierite micro powder and glass frit powder to obtain a microcrystalline glass precursor, so that the microcrystalline glass precursor is used as a binder in the form of pug. And the particle size of the glass frit powder is small in requirement limit, and the size effect of the glass frit powder is not required to be considered as in the traditional method, so that the operability of the glass ceramic is improved.
(4) The cordierite-based microcrystalline glass high-temperature binder has the advantages of good thermal shock resistance, high shear strength, low thermal expansion coefficient and low firing temperature, and the main performance indexes are as follows: thermal expansion coefficient is less than 4 multiplied by 10- 6 ℃- 1 The firing temperature is less than 900 ℃, the thermal conductivity is more than 10W/(m.K), the shearing strength is more than or equal to 40MPa, and the thermal shock resistance circulation is carried out for 30 times at 800 ℃ without cracking.
(5) The invention has simple process and low firing temperature, and has important significance for improving the quality of cordierite-based glass ceramics and saving the cost of products, thus having wide market prospect and being beneficial to promotion and application and the progress and development of industry technology.
Drawings
The invention will be described in further detail with reference to examples and figures:
FIG. 1 is a cross-sectional microstructure of a cordierite-based glass-ceramic high-temperature binder prepared in accordance with an embodiment of the present invention (scanning electron microscope secondary electron image, a: bonding site of the cordierite-based glass-ceramic binder to a ceramic substrate, b: partial enlarged image of FIG. a).
Detailed Description
Embodiment one:
1. the cordierite-based microcrystalline glass high-temperature binder comprises the following raw materials in parts by weight: cordierite micropowder, low-temperature glass frit powder and binder. Wherein, the cordierite micro powder comprises 46 weight percent of ball clay, 35 weight percent of talcum and 19 weight percent of gamma-alumina, and the low-temperature glass frit powder comprises 12 weight percent of MgO and 12 weight percent of Al 2 O 3 10 wt％、SiO 2 60wt％、B 2 O 3 3 wt％、ZrO 2 6 wt％、K 2 O 5wt％、Na 2 O4 wt%. Low-temperature glass frit powder and cordierite micro powder with the mass ratio of=2:3; the binder is formed by mixing water and dextrin (according to the mass ratio of 1:1), and the dosage of the binder is 16 weight percent of the total amount of cordierite micro powder and low-temperature glass frit powder.
2. The preparation method of the cordierite-based microcrystalline glass high-temperature binder comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing the mixture at 1350 ℃ and then carrying out crushing and ball milling to obtain cordierite micro powder with the granularity of 10 mu m;
(2) Preparation of low-temperature glass frit powder
The raw materials of the low-temperature glass frit powder are proportioned, uniformly mixed, melted into glass liquid at the temperature of more than 1500 ℃, clarified and homogenized, subjected to water quenching treatment to obtain glass particles, crushed and ball-milled, and sieved by a 100-mesh sieve to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
And uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and doping a binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder.
3. The application of the binder obtained by the preparation method of the cordierite-based microcrystalline glass high-temperature binder in the embodiment is as follows:
the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 1h at 900 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
Embodiment two:
1. the cordierite-based microcrystalline glass high-temperature binder comprises the following raw materials in parts by weight: cordierite micropowder, low-temperature glass frit powder and binder. Wherein, the cordierite micro powder comprises 48 weight percent of montmorillonite, 33 weight percent of talcum and 19 weight percent of alpha-alumina, and the low-temperature glass frit powder comprises 15 weight percent of MgO and 15 weight percent of Al 2 O 3 10wt％、SiO 2 60 wt％、B 2 O 3 1 wt％、ZrO 2 6 wt％、K 2 O 3wt％、Na 2 O5 wt%. Low-temperature glass frit powder and cordierite micro powder with the mass ratio of=1:1; the binder is PVA water solution with the concentration of 6wt%, and the dosage of the binder is 15wt% of the total amount of cordierite micro powder and low-temperature glass frit powder.
2. The preparation method of the cordierite-based microcrystalline glass high-temperature binder comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing the mixture at 1300 ℃, and carrying out crushing and ball milling to obtain cordierite micro powder with the granularity of 75 mu m;
(2) Preparation of low-temperature glass frit powder
The raw materials of the low-temperature glass frit powder are proportioned, uniformly mixed, melted into glass liquid at the temperature of more than 1500 ℃, clarified and homogenized, subjected to water quenching treatment to obtain glass particles, crushed and ball-milled, and sieved by a 325-mesh sieve to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
And uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and doping a binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder.
3. The application of the binder obtained by the preparation method of the cordierite-based microcrystalline glass high-temperature binder in the embodiment is as follows:
the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 2 hours at 800 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
Embodiment III:
1. the cordierite-based microcrystalline glass high-temperature binder comprises the following raw materials in parts by weight: cordierite micropowder, low-temperature glass frit powder and binder. Wherein, the cordierite micro powder comprises 50 weight percent of kaolin, 35 weight percent of talcum and 15 weight percent of gamma-alumina, and the low-temperature glass frit powder comprises 15 weight percent of MgO and 15 weight percent of Al 2 O 3 10wt％、SiO 2 58 wt％、B 2 O 3 3 wt％、ZrO 2 4 wt％、K 2 O 5wt％、Na 2 O5 wt%. Low-temperature glass frit powder and cordierite micro powder with the mass ratio of=1:1; the binder is waste paper slurry, and the amount of the binder is 18 weight percent of the total amount of cordierite micro powder and low-temperature glass frit powder.
2. The preparation method of the cordierite-based microcrystalline glass high-temperature binder comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing at 1280 ℃, and then crushing and ball milling to obtain the cordierite micro powder with the granularity of 45 mu m;
(2) Preparation of low-temperature glass frit powder
The raw materials of the low-temperature glass frit powder are proportioned, uniformly mixed, melted into glass liquid at the temperature of more than 1500 ℃, clarified and homogenized, subjected to water quenching treatment to obtain glass particles, crushed and ball-milled, and sieved by a 200-mesh sieve to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
And uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and doping a binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder.
3. The application of the binder obtained by the preparation method of the cordierite-based microcrystalline glass high-temperature binder in the embodiment is as follows:
the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 2 hours at 800 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
Embodiment four:
1. the cordierite-based microcrystalline glass high-temperature binder comprises the following raw materials in parts by weight: cordierite micropowder, low-temperature glass frit powder and binder. Wherein, the cordierite micro powder comprises 52 weight percent of kaolin, 37 weight percent of talcum and 11 weight percent of alpha-alumina, and the low-temperature glass frit powder comprises 14 weight percent of MgO and 14 weight percent of Al 2 O 3 10wt％、SiO 2 60 wt％、B 2 O 3 3 wt％、ZrO 2 6 wt％、K 2 O 4wt％、Na 2 O3 wt%. Low-temperature glass frit powder and cordierite micro powder with the mass ratio of 7:3; the binder is formed by mixing water and waste paper slurry (according to the mass ratio of 1:1), and the dosage of the binder is 17 weight percent of the total amount of cordierite micro powder and low-temperature glass frit powder.
2. The preparation method of the cordierite-based microcrystalline glass high-temperature binder comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing the mixture at 1250 ℃, and then carrying out crushing and ball milling to obtain the cordierite micro powder with the granularity of 35 mu m;
(2) Preparation of low-temperature glass frit powder
The raw materials of the low-temperature glass frit powder are proportioned, uniformly mixed, melted into glass liquid at the temperature of more than 1500 ℃, clarified and homogenized, subjected to water quenching treatment to obtain glass particles, crushed and ball-milled, and sieved by a 120-mesh sieve to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
And uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and doping a binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder.
3. The application of the binder obtained by the preparation method of the cordierite-based microcrystalline glass high-temperature binder in the embodiment is as follows:
the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 1h at 900 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
Fifth embodiment:
1. the cordierite-based microcrystalline glass high-temperature binder comprises the following raw materials in parts by weight: cordierite micropowder, low-temperature glass frit powder and binder. Wherein, the cordierite micro powder comprises 54 weight percent of montmorillonite, 35 weight percent of talcum and 11 weight percent of gamma-alumina, and the low-temperature glass frit powder comprises 15 weight percent of MgO and 15 weight percent of Al 2 O 3 6 wt％、SiO 2 60 wt％、B 2 O 3 3 wt％、ZrO 2 6 wt％、K 2 O 5wt％、Na 2 O5 wt%. Low-temperature glass frit powder and cordierite micro powder with the mass ratio of 7:3; the binder is PVA water solution with the concentration of 6wt%, and the dosage of the binder is 16wt% of the total amount of cordierite micro powder and low-temperature glass frit powder.
2. The preparation method of the cordierite-based microcrystalline glass high-temperature binder comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing the mixture at 1200 ℃ and then carrying out crushing and ball milling to obtain cordierite micro powder with the granularity of 75 mu m;
(2) Preparation of low-temperature glass frit powder
The raw materials of the low-temperature glass frit powder are proportioned, uniformly mixed, melted into glass liquid at the temperature of more than 1500 ℃, clarified and homogenized, subjected to water quenching treatment to obtain glass particles, crushed and ball-milled, and sieved by a 325-mesh sieve to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
And uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and doping a binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder.
3. The application of the binder obtained by the preparation method of the cordierite-based microcrystalline glass high-temperature binder in the embodiment is as follows:
the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 1h at 850 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
As shown in FIG. 1, the cordierite-based microcrystalline glass high-temperature binder prepared by the embodiment of the invention has good binding effect as a corundum-mullite ceramic binder, and is tightly bound with a ceramic matrix (see FIG. 1 a), and cordierite micropowder is well bound with glass frit (see FIG. 1 b).
Claims (2)
1. A preparation method of a cordierite-based microcrystalline glass high-temperature binder is characterized by comprising the following steps: the high-temperature binder comprises cordierite micropowder with the particle size of 10-75 mu m, low-temperature glass frit powder with the particle size of 100-325 meshes and a binder; the cordierite micro powder comprises raw materials of 46-54 wt% of clay, 33-37 wt% of talcum and 11-19 wt% of alumina, wherein the clay is kaolin, ball clay or montmorillonite, and the alumina is alpha-alumina or gamma-alumina; the raw materials of the low-temperature glass frit powder comprise 12-15% of MgO and wt% of Al 2 O 3 6～10 wt%、SiO 2 58～60 wt%、B 2 O 3 1～3 wt%、ZrO 2 4～6 wt%、K 2 O 3～5 wt%、Na 2 O3-5 wt%; the mass ratio of the low-temperature glass frit powder to the cordierite micro powder is=2-7:3; the adhesive is one or two of water, PVA water solution with the concentration of 6wt%, dextrin and waste paper slurry, and the dosage of the adhesive is 15-18 wt% of the total amount of cordierite micro powder and low-temperature glass frit powder; the preparation method comprises the following steps:
(1) Synthesis of cordierite micropowder
Mixing the raw materials according to the proportion, firing the mixture at 1200-1350 ℃ and then carrying out crushing and ball milling to obtain micron-sized cordierite micro powder;
(2) Preparation of low-temperature glass frit powder
Proportioning the raw materials of the low-temperature glass frit powder, uniformly mixing, melting to prepare glass liquid, clarifying, homogenizing, performing water quenching treatment to obtain glass particles, crushing, ball milling and sieving to obtain the low-temperature glass frit powder;
(3) Preparation of the adhesive
Uniformly mixing the cordierite micro powder and the low-temperature glass frit powder, and then doping the binder for mixing to obtain a viscous pug, namely the cordierite-based microcrystalline glass high-temperature binder; the adhesive is coated on the surface of a material to be bonded or packaged, and after heat treatment for 1-2 hours at 800-900 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging; the thermal expansion coefficient of the adhesive is less than 4 multiplied by 10 -6 ℃ -1 The firing temperature is less than 900 ℃, the thermal conductivity is more than 10W/(m.K), the shearing strength is more than or equal to 40MPa, and the thermal shock resistance circulation is carried out for 30 times at 800 ℃ without cracking.
2. The use of the binder obtained by the method for preparing cordierite-based glass ceramic high-temperature binder of claim 1, characterized in that: the adhesive in the viscous pug is coated on the surface of a material to be bonded or packaged, and after heat treatment for 1-2 hours at 800-900 ℃, the adhesive is melted to form cordierite-based microcrystalline glass to finish bonding or packaging.
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| US4405722A (en) * | 1979-01-23 | 1983-09-20 | Asahi Glass Company Ltd. | Sealing glass compositions |
| DE3934971C1 (en) * | 1989-10-20 | 1991-01-24 | Schott Glaswerke, 6500 Mainz, De | |
| JP3760455B2 (en) * | 1996-03-05 | 2006-03-29 | 日本電気硝子株式会社 | Adhesive composition |
| ATE314324T1 (en) * | 2001-06-12 | 2006-01-15 | Schott Ag | METHOD FOR PRODUCING BOROSILICATE GLASSES |
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