CN106396409A - Low-temperature lead-free glass binder for electronic paste and preparation method thereof - Google Patents
Low-temperature lead-free glass binder for electronic paste and preparation method thereof Download PDFInfo
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- CN106396409A CN106396409A CN201510445096.7A CN201510445096A CN106396409A CN 106396409 A CN106396409 A CN 106396409A CN 201510445096 A CN201510445096 A CN 201510445096A CN 106396409 A CN106396409 A CN 106396409A
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- 239000011521 glass Substances 0.000 title claims abstract description 98
- 239000011230 binding agent Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 59
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 238000010791 quenching Methods 0.000 claims abstract description 7
- 230000000171 quenching effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 239000004065 semiconductor Substances 0.000 claims abstract description 3
- 239000000428 dust Substances 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 13
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000292 calcium oxide Substances 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- WJEIYVAPNMUNIU-UHFFFAOYSA-N [Na].OC(O)=O Chemical compound [Na].OC(O)=O WJEIYVAPNMUNIU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 6
- 235000013312 flour Nutrition 0.000 claims description 6
- 239000010436 fluorite Substances 0.000 claims description 6
- 235000012054 meals Nutrition 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- -1 pottery Substances 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000005331 crown glasses (windows) Substances 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 229910052845 zircon Inorganic materials 0.000 claims 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 14
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 2
- 239000002893 slag Substances 0.000 abstract 3
- 239000000919 ceramic Substances 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 20
- 239000011787 zinc oxide Substances 0.000 description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 7
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 7
- 235000013350 formula milk Nutrition 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 239000004020 conductor Substances 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 229910052810 boron oxide Inorganic materials 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 235000020610 powder formula Nutrition 0.000 description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 3
- 229910000416 bismuth oxide Inorganic materials 0.000 description 3
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000005308 flint glass Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000007613 slurry method Methods 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- GEZAUFNYMZVOFV-UHFFFAOYSA-J 2-[(2-oxo-1,3,2$l^{5},4$l^{2}-dioxaphosphastannetan-2-yl)oxy]-1,3,2$l^{5},4$l^{2}-dioxaphosphastannetane 2-oxide Chemical compound [Sn+2].[Sn+2].[O-]P([O-])(=O)OP([O-])([O-])=O GEZAUFNYMZVOFV-UHFFFAOYSA-J 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229960004643 cupric oxide Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000005394 sealing glass Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Abstract
The invention relates to a low-temperature lead-free glass binder for electronic paste and a preparation method thereof, wherein the low-temperature lead-free glass binder comprises 20-30% of SiO (silicon dioxide) by mass2、30～65%Bi2O3、0.3～1.5%Na2O、1.5～3.0%K2O、1.5～2.5%ZnO、0.8～1.8%Al2O3、10～16%B2O3、0.5~1.5%CaO、0.4～1.7%F2、1.8～6.0%ZrO2. The preparation method comprises the following steps: (1) accurately weighing the raw materials according to the formula, and mixing for 60 minutes by using a mixer to obtain a uniform mixture; (2) adding the mixture into a frit furnace at 1200-1300 ℃ for heat preservation for 40-60 minutes, after the mixture is completely melted, performing water quenching to obtain glass slag, and mixing the glass slag with the glass slagPutting the glass slag into a ball milling tank, and ball milling for 15-24 hours in a vibration ball mill; (3) and (3) screening the mixture by a 400-mesh screen after ball milling, drying the mixture in a drying box, and finally dispersing the dried glass powder in a dispersion machine to obtain the low-temperature lead-free glass powder. The glass binder prepared by the method has low softening temperature, proper expansion coefficient, good chemical stability and good adhesive force. The low-temperature lead-free glass powder can also be suitable for sealing between glass, ceramics, metal and semiconductors.
Description
Technical field
The invention belongs to chemical industry, field of electronic materials, specifically a kind of electric slurry low-temperature lead-free glass binder and preparation method thereof.
Background technology
Electrocondution slurry is the basis of development electronic devices and components, is the critical material of encapsulation, electrode and interconnection.Electrocondution slurry can be divided into thick film conductor paste and conducting resinl two big class.Thick film conductor paste is used for the high temperature insulated substrate such as pottery, glass.At present, thick film circuit has become one of electronics industry growth rate kind the fastest.Thick film conductor paste consumption based on noble metal for the European and American developed countries substantially exceeds thin film of conductive material.Thick film conductor paste is generally by conductive filler（As silver, gold, copper etc.）, glass powder and organic carrier composition.Wherein glass powder plays binding agent and acts on it is desirable to its softening temperature is at 500 DEG C～600 DEG C or lower.
Traditional glass powder with low melting point is generally flint glass powder, removes or reduces the lead content in glass, the fusing point of glass can increase.Constantly strengthen the enforcement with environmental regulation with various countries' environmental consciousness, electronic product is unleaded to be the Main way that electronic product develops.Develop the lead-less glasses material of low melting point, be the key of exploitation leadless electronic slurry.
In recent years, the research and development of lead-free glass powder gradually cause the attention of researcher.Relevant patent application has：《Barium crown glass powder for electronic slurry and preparation method》The Chinese patent of application number 200710043183.5 discloses the lead-free glass powder formula with bismuth oxide, boron oxide, zinc oxide, aluminum oxide, silica, magnesia and manganese oxide as raw material；《A kind of preparation method of leadless glass powder for electronic slurry》The Chinese patent of application number 200710307708.1 discloses the lead-free glass powder formula with silica, barium monoxide, boron oxide, bismuth oxide, aluminum oxide, zinc oxide, sodium oxide molybdena, potassium oxide and titanium dioxide as raw material.《A kind of no-lead RE doped sealing glass powder with low smelting point and its manufacture method》Application number 200710111386.3；《One kind and metal or alloy lead-free glass powder with low melting point for sealing and preparation method thereof》Application number 200710043182.0；《A kind of low-melting point leadless borophosphate seal glass powder and preparation method thereof》Application number 200810060990.2；《Low-melting point lead-less glasses powder for frit slurry and preparation method thereof and purposes》Application number 200810200747.6；《A kind of lead-free glass powder adhesive and its preparation method and application》The Chinese patent of application number 200910102943.4 discloses the lead-free glass powder formula with zinc oxide, boron oxide, barium monoxide, vanadium oxide and calcium oxide as raw material；《A kind of lead-free glass powder for electronic device connection and preparation method thereof》The Chinese patent of application number 200910102945.3 discloses the lead-free glass powder formula with stannous pyrophosphate, silica, alchlor, cupric oxide, calcium oxide, strontium oxide strontia, vanadium oxide and barium monoxide as raw material；《A kind of low-temperature lead-free glass dust and preparation method thereof》The Chinese patent of application number 201310259302.6 discloses with bismuth oxide, boron oxide, zinc oxide.
The present invention is different according to application purpose, develops a kind of electrocondution slurry low-temperature lead-free glass dust, performance is suitable with low melting point flint glass powder, can be used for the connection between glass, pottery, metal and semiconductor.At aspects such as formula materials unlike the prior art.
Content of the invention
It is an object of the present invention to provide a kind of electric slurry low-temperature lead-free glass binder and preparation method thereof.This low-temperature lead-free glass binder does not contain the harmful element of health risk, and its softening temperature is low, and the coefficient of expansion is suitable, chemical stability and adhesive force is good, preparation method is simple.
The present invention provides a kind of electric slurry low-temperature lead-free glass binder, comprises following component and weight/mass percentage composition：25～35% SiO2, 30～65% Bi2O3, 0.3～1.5% Na2O, 1.5～3.0% K2O, 1.5～2.5% ZnO, 0.8～1.8% Al2O3, 10～16% B2O3, 0.5 ~ 1.5% CaO, 0.4～1.7%F2, 1.8～6.0% ZrO2.
The raw material preparing low-temperature lead-free glass binder is silica flour, oxidation bismuth meal, carbonic acid sodium powder, potassium carbonate powder, oxide powder and zinc, alumina powder, boric acid powder, calcium carbonate, Fluorspar Powder and zirconia powder.
SiO in the present invention2Add for improving mechanical strength, hardness, chemical stability and the heat endurance of glass, but SiO2Too high levels can lead to glass dust softening temperature to raise, and thermal coefficient of expansion increases, SiO2Content is too low, then chemical stability and heat endurance can be led to decline.Pass through in the present invention to introduce and regulation and control ZrO2Content, improves SiO2Too low led to problem.Bi2O3Addition can reduce softening temperature, expand sealing temperature scope, adjust thermal expansion coefficient of glass, but Bi2O3Content can increase cost too much, content very little then softening temperature decline inconspicuous.Na2O and K2O is used for reducing fusion temperature, chemical stability, improves the gloss of glass.ZnO and Al2O3Softening temperature and the thermal coefficient of expansion of glass can be reduced, improve chemical stability and the heat endurance of glass.B2O3The coefficient of expansion of glass can be reduced, improve heat endurance and the chemical stability of glass. CaF2Glass smelting temperature can be reduced, improve chemical stability.ZrO2Chemical stability and mechanical strength and the hardness of glass can be improved.
A kind of sealing temperature of electric slurry low-temperature lead-free glass binder that the present invention provides is 520～680 DEG C, and the coefficient of expansion is 50～76 × 10-7/℃.
The present invention also provides a kind of preparation method of electric slurry low-temperature lead-free glass binder, comprises the steps：
(1) mix 60 minutes according to formula precise raw material, using batch mixer, obtain uniform compound；
(2) compound is poured in Cinker clew furnace, be incubated 40～60 minutes in 1200～1300 DEG C of conditions, after compound is completely melt, water quenching obtains glass dregs, glass dregs are loaded in ball grinder ball milling 15～24 hours in vibrator；
(3) cross 400 mesh mesh screens after ball milling, dry in drying box, finally the glass dust being dried is disperseed in dispersion machine, just obtain low-temperature lead-free glass dust.
Specific embodiment：
In order that the object, technical solutions and advantages of the present invention are clearer, with reference to the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.Described embodiment is a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, broadly fall into the scope of protection of the invention.
Embodiment 1：
The mass percentage content of the low-temperature lead-free glass binder component that the present embodiment provides is respectively 25.7% SiO2、51.0% Bi2O3、0.4% Na2O、2.1% K2O、2.2% ZnO、1.4% Al2O3、11.9% B2O3、0.9% CaO、0.5%F2、3.9% ZrO2.Weigh raw material according to this recipe ingredient mass percentage content to be respectively：Silica flour 232 g, aoxidizes bismuth meal 460g, carbonic acid sodium powder 6 g, potassium carbonate powder 32 g, oxide powder and zinc 20 g, alumina powder 13 g, boric acid powder 191 g, Paris white 3 g, Fluorspar Powder 9g, zirconia powder 35 g, 1000 g altogether.Then according to the following step prepares low-temperature lead-free glass binder：
（1）Mix 60 minutes according to formula precise raw material, using batch mixer, obtain uniform compound；（2）Add mixture in 1200 DEG C of Cinker clew furnace be incubated 50 minutes, after compound is completely melt, water quenching obtains glass dregs, by glass dregs load ball grinder in vibrator ball milling 16 hours；（3）Cross 400 mesh mesh screens after ball milling, dry in drying box, finally the glass dust being dried is disperseed in dispersion machine, just obtain low-temperature lead-free glass dust.530 DEG C of the sealing temperature of the low-temperature lead-free glass binder of the present embodiment, the coefficient of expansion is 72 × 10-7/ DEG C, chemical stability and adhesive force good.
Embodiment 2：The mass percentage content of the low-temperature lead-free glass binder component that the present embodiment provides is respectively 28.0% SiO2、48.0% Bi2O3、0.4% Na2O、2.5% K2O、2.2% ZnO、1.4% Al2O3、12.3% B2O3、1.4% CaO、0.8%F2、3.0% ZrO2.Weigh raw material according to this recipe ingredient mass percentage content to be respectively：Silica flour 251 g, aoxidizes bismuth meal 431g, carbonic acid sodium powder 6 g, potassium carbonate powder 38 g, oxide powder and zinc 20 g, alumina powder 13 g, boric acid powder 196 g, Paris white 3 g, Fluorspar Powder 15g, zirconia powder 27 g, 1000 g altogether.Then according to the following step prepares low-temperature lead-free glass binder：
（1）Mix 60 minutes according to formula precise raw material, using batch mixer, obtain uniform compound；
（2）Add mixture in 1200 DEG C of Cinker clew furnace be incubated 50 minutes, after compound is completely melt, water quenching obtains glass dregs, by glass dregs load ball grinder in vibrator ball milling 16 hours；
（3）Cross 400 mesh mesh screens after ball milling, dry in drying box, finally the glass dust being dried is disperseed in dispersion machine, just obtain low-temperature lead-free glass dust.560 DEG C of the sealing temperature of the low-temperature lead-free glass binder of the present embodiment, the coefficient of expansion is 69 × 10-7/ DEG C, chemical stability and adhesive force good.
Embodiment 3：The mass percentage content of the low-temperature lead-free glass binder component that the present embodiment provides is respectively 30.8% SiO2、45.7% Bi2O3、0.4% Na2O、2.5% K2O、2.0% ZnO、1.2% Al2O3、12.2% B2O3、1.8% CaO、1.1%F2、2.0% ZrO2.Weigh raw material according to this recipe ingredient mass percentage content to be respectively：Silica flour 276 g, aoxidizes bismuth meal 410g, carbonic acid sodium powder 11 g, potassium carbonate powder 38 g, oxide powder and zinc 18 g, alumina powder 11 g, boric acid powder 195 g, Paris white 3 g, Fluorspar Powder 21g, zirconia powder 18 g, 1000 g altogether.Then according to the following step prepares low-temperature lead-free glass binder：
（1）Mix 60 minutes according to formula precise raw material, using batch mixer, obtain uniform compound；
（2）Add mixture in 1250 DEG C of Cinker clew furnace be incubated 50 minutes, after compound is completely melt, water quenching obtains glass dregs, by glass dregs load ball grinder in vibrator ball milling 16 hours；
（3）Cross 400 mesh mesh screens after ball milling, dry in drying box, finally the glass dust being dried is disperseed in dispersion machine, just obtain low-temperature lead-free glass dust.560 DEG C of the sealing temperature of the low-temperature lead-free glass binder of the present embodiment, the coefficient of expansion is 67 × 10-7/ DEG C, chemical stability and adhesive force good.
Embodiment 4：The mass percentage content of the low-temperature lead-free glass binder component that the present embodiment provides is respectively 33.0% SiO2、46.4% Bi2O3、0.7% Na2O、2.9% K2O、1.9% ZnO、1.2% Al2O3、10.5% B2O3、0.9% CaO、0.5%F2、2.0% ZrO2.Weigh raw material according to this recipe ingredient mass percentage content to be respectively：Silica flour 298 g, aoxidizes bismuth meal 419g, carbonic acid sodium powder 11 g, potassium carbonate powder 44 g, oxide powder and zinc 17 g, alumina powder 11 g, boric acid powder 169 g, Paris white 3 g, Fluorspar Powder 9g, zirconia powder 18 g, 1000 g altogether.Then according to the following step prepares low-temperature lead-free glass binder：
（1）Mix 60 minutes according to formula precise raw material, using batch mixer, obtain uniform compound；
（2）Add mixture in 1250 DEG C of Cinker clew furnace be incubated 50 minutes, after compound is completely melt, water quenching obtains glass dregs, by glass dregs load ball grinder in vibrator ball milling 16 hours；
（3）Cross 400 mesh mesh screens after ball milling, dry in drying box, finally the glass dust being dried is disperseed in dispersion machine, just obtain low-temperature lead-free glass dust.
570 DEG C of the sealing temperature of the low-temperature lead-free glass binder of the present embodiment, the coefficient of expansion is 63 × 10-7/ DEG C, chemical stability and adhesive force good.
Certainly; the present invention also can have other various embodiments; in the case of without departing substantially from present invention spirit and its essence, those of ordinary skill in the art can make various corresponding changes according to the present invention and deform, but these corresponding changes and deformation all should belong to the protection domain of the claims in the present invention.
Claims (6)
1. a kind of electric slurry low-temperature lead-free glass binder is it is characterised in that described low-temperature lead-free glass binder comprises following component and weight/mass percentage composition：25～35% SiO2, 30～65% Bi2O3, 0.3～1.5% Na2O, 1.5～3.0% K2O, 1.5～2.5% ZnO, 0.8～1.8% Al2O3, 10～16% B2O3, 0.5 ~ 1.5% CaO, 0.4～1.7%F2, 1.8～6.0% ZrO2.
2. low-temperature lead-free glass binder according to claim 1 is it is characterised in that the raw material of described low-temperature lead-free glass binder is silica flour, oxidation bismuth meal, carbonic acid sodium powder, potassium carbonate powder, oxide powder and zinc, boric acid powder, calcium carbonate, Fluorspar Powder and zircon powder.
3. it is characterised in that the sealing temperature of described crown glass binding agent is 520～680 DEG C, the coefficient of expansion is 50～76 × 10 to low-temperature lead-free glass binder according to claim 1-7/℃.
4. the preparation method of low-temperature lead-free glass dust according to claim 1, comprises the following steps：
（1）Mix 60 minutes according to formula precise raw material, using batch mixer, obtain uniform compound；
（2）Add mixture in 1200～1280 DEG C of Cinker clew furnace be incubated 40～60 minutes, after compound is completely melt, water quenching obtains glass dregs, by glass dregs load ball grinder in vibrator ball milling 15～24 hours；
（3）Cross 400 mesh mesh screens after ball milling, dry in drying box, finally the glass dust being dried is disperseed in dispersion machine, just obtain obtaining lead-free glass powder.
5. the preparation method of low-temperature lead-free glass binder according to claim 2 is it is characterised in that glass dust particle diameter is at 1～5 micron.
6. according to claim 1 low-temperature lead-free glass binder application it is characterised in that described crown glass binding agent can be used for the glass binder in electric slurry and can be used for the sealing-in between glass, pottery, metal and semiconductor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN107021635A (en) * | 2017-04-26 | 2017-08-08 | 苏州融睿电子科技有限公司 | Glass solder and preparation method thereof |
| CN107880786A (en) * | 2017-11-30 | 2018-04-06 | 上海穗杉实业股份有限公司 | A kind of inorganic sealant and preparation method thereof and application method |
| CN110683764A (en) * | 2019-11-15 | 2020-01-14 | 黄山市晶特美新材料有限公司 | Glass powder for environment-friendly high-acid-resistance automobile glass slurry and preparation method thereof |
| CN111675490A (en) * | 2020-06-20 | 2020-09-18 | 厦门翰森达电子科技有限公司 | Lead-free and cadmium-free glass powder and preparation method thereof, and conductive silver paste and preparation method thereof |
| CN112358191A (en) * | 2020-11-11 | 2021-02-12 | 上海大洲电子材料有限公司 | Formula, preparation and surface modification methods of lead-free low-melting-point glass powder for conductive paste |
| CN113087399A (en) * | 2021-04-07 | 2021-07-09 | 淄博宝晶新材料股份有限公司 | Environment-friendly low-expansion high-covering-power glass powder for electrical appliance |
| CN113286419A (en) * | 2021-07-22 | 2021-08-20 | 西安宏星电子浆料科技股份有限公司 | Multilayer isolation medium slurry for thick film circuit |
| CN114315160A (en) * | 2021-12-20 | 2022-04-12 | 西安赛尔电子材料科技有限公司 | Low dielectric sealing glass granulation powder and preparation method thereof |
| CN116217246A (en) * | 2023-02-27 | 2023-06-06 | 合肥水泥研究设计院有限公司 | Inorganic binder and preparation method of inorganic binder/TiC composite material |
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| CN107021635A (en) * | 2017-04-26 | 2017-08-08 | 苏州融睿电子科技有限公司 | Glass solder and preparation method thereof |
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| CN110683764A (en) * | 2019-11-15 | 2020-01-14 | 黄山市晶特美新材料有限公司 | Glass powder for environment-friendly high-acid-resistance automobile glass slurry and preparation method thereof |
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| CN113087399A (en) * | 2021-04-07 | 2021-07-09 | 淄博宝晶新材料股份有限公司 | Environment-friendly low-expansion high-covering-power glass powder for electrical appliance |
| CN113286419A (en) * | 2021-07-22 | 2021-08-20 | 西安宏星电子浆料科技股份有限公司 | Multilayer isolation medium slurry for thick film circuit |
| CN114315160A (en) * | 2021-12-20 | 2022-04-12 | 西安赛尔电子材料科技有限公司 | Low dielectric sealing glass granulation powder and preparation method thereof |
| CN116217246A (en) * | 2023-02-27 | 2023-06-06 | 合肥水泥研究设计院有限公司 | Inorganic binder and preparation method of inorganic binder/TiC composite material |
| CN116217246B (en) * | 2023-02-27 | 2023-12-19 | 合肥水泥研究设计院有限公司 | Inorganic binder and preparation method of inorganic binder/TiC composite material |
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