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CN106673452A - Low-melting-point inorganic adhesive for aluminum materials and preparation method thereof - Google Patents

Low-melting-point inorganic adhesive for aluminum materials and preparation method thereof Download PDF

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Publication number
CN106673452A
CN106673452A CN201611128393.XA CN201611128393A CN106673452A CN 106673452 A CN106673452 A CN 106673452A CN 201611128393 A CN201611128393 A CN 201611128393A CN 106673452 A CN106673452 A CN 106673452A
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China
Prior art keywords
inorganic binder
melting point
low melting
granularity
aluminium base
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CN201611128393.XA
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Chinese (zh)
Inventor
刘建
苏冠贤
张晓飞
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Dongguan Corehelm Electronic Material Technology Co Ltd
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Dongguan Corehelm Electronic Material Technology Co Ltd
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Priority to CN201611128393.XA priority Critical patent/CN106673452A/en
Priority to PCT/CN2016/113349 priority patent/WO2018103165A1/en
Publication of CN106673452A publication Critical patent/CN106673452A/en
Pending legal-status Critical Current

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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
    • C03C12/00—Powdered glass; Bead compositions
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a low-melting-point inorganic adhesive for aluminum materials and a preparation method thereof. The low-melting-point inorganic adhesive is prepared from the following materials in percentage by weight: 1-20 percent of SiO2, 30-50 percent of Bi2O3, 5-40 percent of B2O3, 5-15 percent of CaF2, 0.1-2 percent of SnO2, 0.2-15 percent of Al2O3, 0.1-5 percent of ZnO and 0.1-2 percent of TiO2. The low-melting-point inorganic adhesive has low softening point, proper melting temperature, excellent dielectric performance and physiochemical performance, can effectively meet the requirement for insulating mediums of aluminum materials and inorganic adhesive of electronic paste. The preparation method comprises the following steps of: a, weighing and stirring; b, heating and melting; c, water quenching; d, drying; and e, grinding and performing ball milling. By adopting the design of process steps, the preparation method can be used for effectively producing and preparing the low-melting-point inorganic adhesive.

Description

A kind of low melting point inorganic binder suitable for aluminium base and preparation method thereof
Technical field
The present invention relates to technical field of electronic materials, more particularly to a kind of low melting point inorganic binder suitable for aluminium base And preparation method thereof.
Background technology
Inorganic binder glass transition temperature and fusion temperature are relatively low, and it can be applicable to electronic device and quasiconductor The aspects such as sealing-in, bonding Deng element, it is also possible to used in aspects such as electric slurry, dielectric materials.
Leaded low-melting glass easily causes environmental pollution and the body of direct labor can be damaged, although many low Melting point glass overcomes disadvantages mentioned above, but there is still a need for higher temperature could be soft in terms of low temperature softening and low-temperature working Change, and could only in this way realize welding.
It should further be noted that the glass powder with low melting point for producing in the market is primarily present following defect, specially：1st, it is soft Change temperature higher；3rd, the coefficient of expansion is excessive；3rd, dielectric properties are not good.
The content of the invention
Present invention aims to the deficiencies in the prior art and to provide a kind of low melting point suitable for aluminium base inorganic Binding agent, the low melting point inorganic binder softening point that this is applied to aluminium base is low, fusion temperature is moderate, and with excellent dielectric Performance, physicochemical property, you can effectively to meet aluminium base dielectric, electric slurry inorganic binder requirement.
Another object of the present invention is to a kind of preparation method of the low melting point inorganic binder suitable for aluminium base is provided, The preparation method can effectively be produced and prepare above-mentioned low melting point inorganic binder.
To reach above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of low melting point inorganic binder suitable for aluminium base, includes the material of following weight portion, specially：
SiO2 1%-20%
Bi2O3 30%-50%
B2O3 5%-40%
CaF2 5%-15%
SnO2 0.1%-2%
Al2O3 0.2%-15%
ZnO 0.1%-5%
TiO2 0.1%-2%；
Wherein, the inorganic binder is amorphous inorganic binding agent, crystallite state inorganic binder or amorphous inorganic binding agent The mixing inorganic binder constituted with crystallite state inorganic binder.
Wherein, the SiO2Granularity be 1 μm -20 μm, purity is 99.5%-99.9%.
Wherein, the Bi2O3Granularity be 5 μm -50 μm, purity ＞ 99.9%.
Wherein, the CaF2Granularity be 2 μm -30 μm, purity ＞ 99.9%.
Wherein, the SnO2Granularity be 10 μm -50 μm, purity ＞ 99.9%.
Wherein, the Al2O3Granularity be 1 μm -20 μm, purity 99.5-99.9%.
Wherein, the B2O3Granularity be 5 μm -50 μm, purity ＞ 99.5-%.
Wherein, the granularity of the ZnO is 2 μm -30 μm, purity ＞ 99.5%.
Wherein, the TiO2Granularity be 1 μm -20 μm, purity ＞ 99.5%.
A kind of preparation method of the low melting point inorganic binder suitable for aluminium base, includes following processing step, specifically For：
A, accurately weigh SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2 , then by the SiO for weighing2、 Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2It is placed in batch mixer and is stirred mixing；
B, treat SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2After the compound for being constituted is sufficiently mixed, will be mixed Close material to be poured in platinum crucible, and be slowly warmed up to 400 DEG C with the programming rate of 1-5 DEG C/min and be incubated 60min, then again 1100 DEG C are continuously heating to the programming rate of 10-30 DEG C/min and be incubated 2 hours；
C, the compound to melting carry out Water Quenching, to obtain glass dregs；
D, glass dregs are dried with process；
E, dried glass dregs are placed in ball mill carry out crushing ball-milling treatment, then sieve to obtain low-melting glass Powder, low melting point inorganic binder is prepared and finished.
Beneficial effects of the present invention are：A kind of low melting point inorganic binder suitable for aluminium base of the present invention, its The material of following weight portion is included, specially：SiO2 1%-20%、Bi2O3 30%-50%、B2O3 5%-40%、CaF2 5%-15%、 SnO2 0.1%-2% 、Al2O30.2%-15%、ZnO0.1%-5%、TiO2 0.1%-2%.By above-mentioned material proportion, the present invention's is suitable For aluminium base low melting point inorganic binder softening point is low, fusion temperature is moderate, and with excellent dielectric properties, physics and chemistry Can, you can effectively to meet aluminium base dielectric, electric slurry inorganic binder requirement.
The another of the present invention has the beneficial effect that：A kind of low melting point inorganic binder suitable for aluminium base of the present invention Preparation method, it includes following processing step：A, accurately weigh SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、 TiO2 , then by the SiO for weighing2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2It is placed in batch mixer and is stirred Mix mixing；B, treat SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2After the compound for being constituted is sufficiently mixed, will Compound is poured in platinum crucible, and is slowly warmed up to 400 DEG C with the programming rate of 1-5 DEG C/min and is incubated 60min, then It is continuously heating to 1100 DEG C with the programming rate of 10-30 DEG C/min again and is incubated 2 hours；C, the compound to melting carry out water quenching Process, to obtain glass dregs；D, glass dregs are dried with process；E, dried glass dregs are placed in ball mill carry out powder Broken ball-milling treatment, then sieves to obtain glass powder with low melting point, and low melting point inorganic binder is prepared and finished.Walked by above-mentioned technique Rapid design, the preparation method can effectively be produced and prepare above-mentioned low melting point inorganic binder.
Specific embodiment
With reference to specific embodiment, the present invention will be described.
A kind of embodiment one, low melting point inorganic binder suitable for aluminium base, includes the material of following weight portion, tool Body is：
SiO2 5%
Bi2O3 50%
B2O3 35%
CaF2 5%
SnO2 1%
Al2O3 1%
ZnO 2%
TiO2 1%；
Wherein, the inorganic binder is amorphous inorganic binding agent, crystallite state inorganic binder or amorphous inorganic binding agent The mixing inorganic binder constituted with crystallite state inorganic binder.
It should further be noted that SiO2Granularity be 1 μm -20 μm, purity is 99.5%-99.9%；Bi2O3Granularity be 5 μm -50 μm, purity ＞ 99.9%；CaF2Granularity be 2 μm -30 μm, purity ＞ 99.9%；SnO2Granularity be 10 μm- 50 μm, purity ＞ 99.9%；Al2O3Granularity be 1 μm -20 μm, purity 99.5-99.9%；B2O3Granularity be 5 μm -50 μm, purity ＞ 99.5-%；The granularity of ZnO is 2 μm -30 μm, purity ＞ 99.5%；TiO2Granularity be 1 μm -20 μm, it is pure Degree ＞ 99.5%.
By above-mentioned material proportion, the low melting point inorganic binder softening point suitable for aluminium base of the present embodiment one is low, Fusion temperature is moderate, and with excellent dielectric properties, physicochemical property, you can effectively to meet aluminium base dielectric, electricity Sub- slurry inorganic binder is required.
Need to be explained further, the low melting point inorganic binder of the present embodiment one can be using the preparation of following preparation method Into, specifically, a kind of preparation method of the low melting point inorganic binder suitable for aluminium base, it includes following processing step：
A, accurately weigh SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2 , then by the SiO for weighing2、 Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2It is placed in batch mixer and is stirred mixing；
B, treat SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2After the compound for being constituted is sufficiently mixed, will be mixed Close material to be poured in platinum crucible, and be slowly warmed up to 400 DEG C with the programming rate of 3 DEG C/min and be incubated 60min, then again with The programming rate of 10 DEG C/min is continuously heating to 1100 DEG C and is incubated 2 hours；
C, the compound to melting carry out Water Quenching, to obtain glass dregs；
D, glass dregs are dried with process；
E, dried glass dregs are placed in ball mill carry out crushing ball-milling treatment, then sieve to obtain low-melting glass Powder, low melting point inorganic binder is prepared and finished.
A kind of embodiment two, low melting point inorganic binder suitable for aluminium base, includes the material of following weight portion, specifically For：
SiO2 10%
Bi2O3 30%
B2O3 40%
CaF2 10%
SnO2 2%
Al2O3 5%
ZnO 1%
TiO2 2%；
Wherein, the inorganic binder is amorphous inorganic binding agent, crystallite state inorganic binder or amorphous inorganic binding agent The mixing inorganic binder constituted with crystallite state inorganic binder.
It should further be noted that SiO2Granularity be 1 μm -20 μm, purity is 99.5%-99.9%；Bi2O3Granularity be 5 μm -50 μm, purity ＞ 99.9%；CaF2Granularity be 2 μm -30 μm, purity ＞ 99.9%；SnO2Granularity be 10 μm- 50 μm, purity ＞ 99.9%；Al2O3Granularity be 1 μm -20 μm, purity 99.5-99.9%；B2O3Granularity be 5 μm -50 μm, purity ＞ 99.5-%；The granularity of ZnO is 2 μm -30 μm, purity ＞ 99.5%；TiO2Granularity be 1 μm -20 μm, it is pure Degree ＞ 99.5%.
By above-mentioned material proportion, the low melting point inorganic binder softening point suitable for aluminium base of the present embodiment two is low, Fusion temperature is moderate, and with excellent dielectric properties, physicochemical property, you can effectively to meet aluminium base dielectric, electricity Sub- slurry inorganic binder is required.
Need to be explained further, the low melting point inorganic binder of the present embodiment two can be using the preparation of following preparation method Into, specifically, a kind of preparation method of the low melting point inorganic binder suitable for aluminium base, it includes following processing step：
A, accurately weigh SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2 , then by the SiO for weighing2、 Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2It is placed in batch mixer and is stirred mixing；
B, treat SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2After the compound for being constituted is sufficiently mixed, will be mixed Close material to be poured in platinum crucible, and be slowly warmed up to 400 DEG C with the programming rate of 4 DEG C/min and be incubated 60min, then again with The programming rate of 20 DEG C/min is continuously heating to 1100 DEG C and is incubated 2 hours；
C, the compound to melting carry out Water Quenching, to obtain glass dregs；
D, glass dregs are dried with process；
E, dried glass dregs are placed in ball mill carry out crushing ball-milling treatment, then sieve to obtain low-melting glass Powder, low melting point inorganic binder is prepared and finished.
A kind of embodiment three, low melting point inorganic binder suitable for aluminium base, includes the material of following weight portion, specifically For：
SiO2 20%
Bi2O3 35%
B2O3 20%
CaF2 15%
SnO2 2%
Al2O3 5%
ZnO 2%
TiO2 1%；
Wherein, the inorganic binder is amorphous inorganic binding agent, crystallite state inorganic binder or amorphous inorganic binding agent The mixing inorganic binder constituted with crystallite state inorganic binder.
It should further be noted that SiO2Granularity be 1 μm -20 μm, purity is 99.5%-99.9%；Bi2O3Granularity be 5 μm -50 μm, purity ＞ 99.9%；CaF2Granularity be 2 μm -30 μm, purity ＞ 99.9%；SnO2Granularity be 10 μm- 50 μm, purity ＞ 99.9%；Al2O3Granularity be 1 μm -20 μm, purity 99.5-99.9%；B2O3Granularity be 5 μm -50 μm, purity ＞ 99.5-%；The granularity of ZnO is 2 μm -30 μm, purity ＞ 99.5%；TiO2Granularity be 1 μm -20 μm, it is pure Degree ＞ 99.5%.
By above-mentioned material proportion, the low melting point inorganic binder softening point suitable for aluminium base of the present embodiment three is low, Fusion temperature is moderate, and with excellent dielectric properties, physicochemical property, you can effectively to meet aluminium base dielectric, electricity Sub- slurry inorganic binder is required.
Need to be explained further, the low melting point inorganic binder of the present embodiment three can be using the preparation of following preparation method Into, specifically, a kind of preparation method of the low melting point inorganic binder suitable for aluminium base, it includes following processing step：
A, accurately weigh SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2 , then by the SiO for weighing2、 Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2It is placed in batch mixer and is stirred mixing；
B, treat SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3 、ZnO 、TiO2After the compound for being constituted is sufficiently mixed, will be mixed Close material to be poured in platinum crucible, and be slowly warmed up to 400 DEG C with the programming rate of 5 DEG C/min and be incubated 60min, then again with The programming rate of 30 DEG C/min is continuously heating to 1100 DEG C and is incubated 2 hours；
C, the compound to melting carry out Water Quenching, to obtain glass dregs；
D, glass dregs are dried with process；
E, dried glass dregs are placed in ball mill carry out crushing ball-milling treatment, then sieve to obtain low-melting glass Powder, low melting point inorganic binder is prepared and finished.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to the present invention's Thought, will change in specific embodiments and applications, and this specification content should not be construed as to the present invention Restriction.

Claims (10)

1. a kind of low melting point inorganic binder suitable for aluminium base, it is characterised in that include the material of following weight portion, has Body is：
SiO2 1%-20%
Bi2O3 30%-50%
B2O3 5%-40%
CaF2 5%-15%
SnO2 0.1%-2%
Al2O3 0.2%-15%
ZnO 0.1%-5%
TiO2 0.1%-2%；
Wherein, the inorganic binder is amorphous inorganic binding agent, crystallite state inorganic binder or amorphous inorganic binding agent The mixing inorganic binder constituted with crystallite state inorganic binder.
2. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described SiO2Granularity be 1 μm -20 μm, purity is 99.5%-99.9%.
3. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described Bi2O3Granularity be 5 μm -50 μm, purity ＞ 99.9%.
4. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described CaF2Granularity be 2 μm -30 μm, purity ＞ 99.9%.
5. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described SnO2Granularity be 10 μm -50 μm, purity ＞ 99.9%.
6. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described Al2O3Granularity be 1 μm -20 μm, purity 99.5-99.9%.
7. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described B2O3Granularity be 5 μm -50 μm, purity ＞ 99.5-%.
8. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described The granularity of ZnO is 2 μm -30 μm, purity ＞ 99.5%.
9. a kind of low melting point inorganic binder suitable for aluminium base according to claim 1, it is characterised in that：It is described TiO2Granularity be 1 μm -20 μm, purity ＞ 99.5%.
10. a kind of preparation method of the low melting point inorganic binder suitable for aluminium base, it is characterised in that include following technique Step, specially：
A, accurately weigh SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3、ZnO 、TiO2 , then by the SiO for weighing2、Bi2O3、 B2O3、CaF2、SnO2、Al2O3、ZnO 、TiO2It is placed in batch mixer and is stirred mixing；
B, treat SiO2、Bi2O3、B2O3、CaF2、SnO2、Al2O3、ZnO 、TiO2After the compound for being constituted is sufficiently mixed, will mix Material is poured in platinum crucible, and is slowly warmed up to 400 DEG C with the programming rate of 1-5 DEG C/min and is incubated 60min, then again with The programming rate of 10-30 DEG C/min is continuously heating to 1100 DEG C and is incubated 2 hours；
C, the compound to melting carry out Water Quenching, to obtain glass dregs；
D, glass dregs are dried with process；
E, dried glass dregs are placed in ball mill carry out crushing ball-milling treatment, then sieve to obtain low-melting glass Powder, low melting point inorganic binder is prepared and finished.
CN201611128393.XA 2016-12-09 2016-12-09 Low-melting-point inorganic adhesive for aluminum materials and preparation method thereof Pending CN106673452A (en)

Priority Applications (2)

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CN201611128393.XA CN106673452A (en) 2016-12-09 2016-12-09 Low-melting-point inorganic adhesive for aluminum materials and preparation method thereof
PCT/CN2016/113349 WO2018103165A1 (en) 2016-12-09 2016-12-30 Low-melting-point inorganic binder suitable for aluminum substrate and preparation method therefor

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Application Number Priority Date Filing Date Title
CN201611128393.XA CN106673452A (en) 2016-12-09 2016-12-09 Low-melting-point inorganic adhesive for aluminum materials and preparation method thereof

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US20240167320A1 (en) * 2022-11-23 2024-05-23 LuxWall, Inc. Vacuum insulated panel with edge seal

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CN117486620B (en) * 2023-10-30 2024-05-31 西华大学 Alumina low temperature sintering aid, alumina ceramic material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN112037960A (en) * 2020-09-16 2020-12-04 湖南利德电子浆料股份有限公司 Conductive silver paste, preparation method thereof and 5G ceramic filter
CN112037960B (en) * 2020-09-16 2022-03-15 湖南利德电子浆料股份有限公司 A conductive silver paste and its preparation method and 5G ceramic filter
US20240167320A1 (en) * 2022-11-23 2024-05-23 LuxWall, Inc. Vacuum insulated panel with edge seal
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Application publication date: 20170517