CN100579929C - Method for preparing nano composite low melting point glass insulation coating - Google Patents
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- CN100579929C CN100579929C CN200510041144A CN200510041144A CN100579929C CN 100579929 C CN100579929 C CN 100579929C CN 200510041144 A CN200510041144 A CN 200510041144A CN 200510041144 A CN200510041144 A CN 200510041144A CN 100579929 C CN100579929 C CN 100579929C
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- powder
- melting point
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
- C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
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Abstract
The process of preparing nanometer composite insulating low smelting point glass coating includes the following steps: 1. preparing mixed slurry through mixing low smelting point SiO2-B2O3 glass powder, nanometer ceramic powder, two or more of sodium silicate, silica sol, methyl cellulose and polyethylene glycol, and water in the weight ratio of 100 to 5-60 to 1-30 to 200-400 and ball milling for 5-10hr; 2. coating the slurry onto substrate, drying at 80-120 deg.c for 10-30 min, and heat treatment first at 350-450 deg.c for 30-60 and then at 500-700 deg.c for 5-30 min; and 3. repeating the step 2 by 3-10 times to prepare the nanometer composite insulating low smelting point glass coating. The preparation process has low cost and no environmental pollution, and the coating has relatively high heat expansion coefficient matching the metal substrate and excellent high temperature insulating performance.
Description
Technical field
The present invention relates to a kind of method for making of insulating coating, especially the preparation method of nano composite low melting point glass insulation coating.
Background technology
Has inorganic insulation coated material high temperature resistant, the insulation strength advantages of higher, plant and instrument has a wide range of applications in various fields such as nuclear energy, metallurgy, mines to the requirement of high insulating property under high temperature (～400 ℃) condition to satisfy can to substitute the organic polymer insulating material.As the low melting glass of one of inorganic insulation coated material, fusing point is low, thermal expansivity is higher (greater than 10 * 10 though have
-6/ ℃), make it can under lower temperature, prepare fine and close insulating coating, and can alleviate and the base material thermal expansivity does not match and causes the advantage of coating cracking; Yet but have because of its high thermal expansion coefficient and low-melting acquisition be by increasing alkalimetal oxide R in the glass system
2The content of O (R is Li, Na, K etc.) obtains, and the diffusion of these alkalimetal ions is accelerated under hot environment, produces ionic conductance, seriously undermines the defective of the insulating property of coating.For the way of avoiding this defective, have taking the component of glass is adjusted, as a kind of " the thick film circuit dielectric slurry " that discloses among the disclosed Chinese invention patent ublic specification of application CN1508812A on June 30th, 2004.It is intended to provide a kind of slurry, with reach make multilayer thick film circuit middle level with layer between insulation layer and the individual layer circuit in the purpose of insulation layer.The preparation method of this slurry contains TiO for preparing earlier
2And ZrO
2The glass powder of composition is dispersed in this glass powder and forms slurry in the organic medium, afterwards, slurry is used for Al
2O
3Make wet film with methods such as silk screen printing, sprayings on ceramic substrate or the common electropane substrate, last, behind super-dry, 540～600 ℃ sintering, form the insulation layer in the thick film circuit.But this inorganic insulation layer and preparation method thereof all exists weak point, and at first, the formation of slurry needs with an organic solvent, not only costs an arm and a leg, and also very easily environment is polluted; Secondly, formed glass dielectric layer material coefficient of thermal expansion coefficient has only 7.3 * 10
-6/ ℃, be lower than the thermal expansivity of common metal base material, because not matching between the two very easily causes the cracking in the use, influence the insulating property of final coating.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming weak point of the prior art, provide that a kind of cost is low, simple, the environmentally safe of preparation, the goods of being made can keep the higher thermal expansivity that is complementary with metal base, can have the preparation method than the nano composite low melting point glass insulation coating of high insulating property again under hot conditions.
The preparation method of nano composite low melting point glass insulation coating comprises and being coated in the substrate after glass powder made slurry, drying, sintering again, and particularly it is finished according to the following steps: (1), with SiO
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass or silicon sol or methylcellulose gum or polyoxyethylene glycol or aforementioned in two or morely mix mutually according to 100: 5～60: 1～30: 200～400 ratio with water, again its ball milling was obtained mixed slurry in 5～10 hours; (2), use the mixed slurry coated substrate, again with its in 80～120 ℃ dry 10～30 minutes down, afterwards, with it successively in 350～450 ℃ of following thermal treatments 30～60 minutes, 500～700 ℃ of following thermal treatment 5～30 minutes; (3), repeat step 3～10 time of (2), make nano composite low melting point glass insulation coating.
As the preparation method's of nano composite low melting point glass insulation coating further improvement, described SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
220～60wt%, B
2O
35～30wt%, ZnO3～25wt%, CaO0.5～10wt%, MgO0.5～7wt%, BaO0.5～5wt%, Na
2O5～20wt%, K
2O5～20wt% and Al
2O
3Get raw material 0.1 the ratio of～2wt% is joined, it was mixed back ball milling 5～10 hours, under 1000～1300 ℃, founded 30～80 minutes again, then, ball milling 5～10 hours and the solid powder that obtains behind the quenching in water; Described nano-ceramic powder be alumina powder jointed or magnesium oxide powder or beta-silicon nitride powder or aluminium nitride powder or aforementioned powder in two or more, its particle diameter is 20～150nm; Described water is deionized water or distilled water; Described ball milling is to place ball grinder to mix on planetary ball mill and grinding mixture; Described spin coating or spraying or the dipping of being applied to; Described substrate is metal base or the semiconductor-based end or superconductor substrate; Described before coated substrate, earlier it is polished, deoils and cleans.
Beneficial effect with respect to prior art is that one is respectively to using pure SiO
2-B
2O
3Be the low melting glass powder, at SiO
2-B
2O
3Be that the surface topography that adds the sample that makes behind 5～60% the nano-ceramic powder in the low melting glass powder uses field emission scanning electron microscope to characterize, from the stereoscan photograph that obtains as can be known, only use pure SiO
2-B
2O
3The structure that is the insulating coating that makes of glass powder with low melting point body is not fine and close, and many holes are arranged in the coating, and at SiO
2-B
2O
3Be that to have added the structure of the insulating coating that makes behind 5～60% the nano-ceramic powder in the low melting glass powder tight, fine and smooth, its surface is solidifies shape, can find out thus, because the particle diameter of nano-ceramic powder is 20～150nm, and itself and SiO
2-B
2O
3Be that wetting property between the matrix that forms after the fusion of low melting glass powder is better, therefore in heat treatment process, help the discharge of pore, finally reduced the porosity of insulating coating inside, help to promote the insulation strength of coating; Its two, respectively to using pure SiO
2-B
2O
3Be the low melting glass powder, at SiO
2-B
2O
3Be to add the sample that makes behind 5～60% the nano-ceramic powder in the low melting glass powder to carry out the test of thermal expansivity, can find out that by its thermal expansion graphic representation in the time of 90～400 ℃, sample has more uniform thermal expansion, can calculate SiO according to this figure
2-B
2O
3Be that low melting glass and the thermal expansivity that adds 20% nano alumina powder jointed composite low melting point glass are respectively 12.3 * 10
-6/ ℃, 11.8 * 10
-6/ ℃, these all are close with the thermal expansivity of common metal matrix.In addition, from figure, also can find out because the softening temperature that the interpolation of nano-ceramic powder makes sample rises to 583 ℃ from 530 ℃, so nano composite low melting point glass insulation coating in 400 ℃ of environment trouble-free service without any problem; Its three, respectively to using pure SiO
2-B
2O
3Be the low melting glass powder, at SiO
2-B
2O
3Be to add the sample that makes behind 5～60% the nano-ceramic powder in the low melting glass powder to carry out the measurement of insulation resistance, the result shows that the sample volume resistivity of adding nano-ceramic powder under 400 ℃ of conditions is 7.38 * 10
8Ω cm is far above pure SiO
2-B
2O
3It is 2 * 10 of low melting glass
6The volume specific resistance of Ω cm, the interpolation of this explanation nano-ceramic powder have reduced the electricity of glass intermediate ion leads, and this mainly is because nano-ceramic powder is dispersed in the matrix of glass equably, and both things are different mutually, cause number of grain boundaries to increase, and hindered Na
+Deng the motion of conductive ion, thereby increased the high temperature insulation characteristic of coating, though after adding nano-ceramic powder SiO
2-B
2O
3The thermal expansivity that is low melting glass can slightly reduce, but the raising of insulating property is significant under high temperature (400 ℃) environment; Its four, coating is carried out insulation strength test, the result shows that the interpolation of nano ceramics particle has also improved the dielectric breakdown strength of glass coating, this is to come from the lifting of coating density and the reduction of ionic conductance; Its five, production cost is low, preparation is easy, environmentally safe.
Description of drawings
Below in conjunction with accompanying drawing optimal way of the present invention is described in further detail.
Fig. 1 observes the photo of taking behind the pattern of coatingsurface to insulating coating with the Sirion 200FEG of U.S. FEI Co. type field emission scanning electron microscope, and wherein, (a) figure uses pure SiO
2-B
2O
3Be the surface topography map of the insulating coating that is equipped with of glass powder with low melting point system, (b) figure is at SiO
2-B
2O
3It is the surface topography map that adds the insulating coating that makes behind 20% the nano aluminium oxide in the low melting glass powder;
Fig. 2 is the graphic representation that the anti-DIL402C of the company type thermal dilatometer of speeding of sample utilization Germany that makes is carried out thermal expansivity test back gained, and wherein, X-coordinate is a temperature, and ordinate zou is a sample length, and the curve among the figure (a) is for using pure SiO
2-B
2O
3Be the thermal expansion curve of the sample of glass powder with low melting point system one-tenth, curve (b) is at SiO
2-B
2O
3It is the thermal expansion curve that has added the sample that makes behind 20% the nano aluminium oxide in the low melting glass powder;
Fig. 3 utilizes LK2679A type Insulation Resistance Tester and LK2672A type Hi-pot Tester to carry out the graph of a relation of the test of insulation resistance and voltage breakdown and the resistivity that obtains and disruptive strength and temperature respectively after calculation of correlation to the sample that makes, wherein, X-coordinate is a temperature, left side ordinate zou is a resistivity, and right ordinate zou is a disruptive strength.Curve among the figure (a) is for using pure SiO
2-B
2O
3Be the resistivity of the sample that becomes of glass powder with low melting point system and the graph of a relation of disruptive strength and temperature, curve (b) is at SiO
2-B
2O
3It is the graph of a relation that has added resistivity and the disruptive strength and the temperature of the sample that makes behind 20% the nano aluminium oxide in the low melting glass powder.
Embodiment
At first make or buy particle diameter and be alumina powder jointed, magnesium oxide powder, beta-silicon nitride powder and the aluminium nitride powder of 20～150nm from market with ordinary method, and water glass, silicon sol, methylcellulose gum and polyoxyethylene glycol.Then:
1), earlier with SiO embodiment 1: finish preparation according to the following steps:
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass and deionized water (or distilled water) according to 100: 5: 30: 200 ratio is mixed mutually; Wherein, SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
225wt%, B
2O
310wt%, ZnO20wt%, CaO7wt%, MgO5wt%, BaO4wt%, Na
2O15wt%, K
2O13.4wt% and Al
2O
3The ratio of 0.6wt% is joined and is got raw material, and it was mixed back ball milling 5 hours, under 1000 ℃, founded 80 minutes again, then, and ball milling 5 hours and the solid powder that obtains behind the quenching in water, nano-ceramic powder is selected for use alumina powder jointed.Again mixture is placed ball grinder on planetary ball mill, to mix and obtained mixed slurry in 10 hours with grinding.2) use mixed slurry spin coating (or spraying or dipping) in the surface of metal base copper (or the semiconductor-based end or superconductor substrate), earlier, wherein, before spin coating metal base copper, earlier it is polished, deoils and cleans; Again with its in 80 ℃ dry 30 minutes down, afterwards, with it successively in 350 ℃ of following thermal treatments 60 minutes, 500 ℃ of following thermal treatment 30 minutes.3), repeat 2) step 3 time, make and be similar to the nano composite low melting point glass insulation coating shown in Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b).
1), earlier with SiO embodiment 2: finish preparation according to the following steps:
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass and deionized water (or distilled water) according to 100: 20: 23: 250 ratio is mixed mutually; Wherein, SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
230wt%, B
2O
325wt%, ZnO12wt%, CaO4wt%, MgO1wt%, BaO5wt%, Na
2O13wt%, K
2O9.7wt% and Al
2O
3The ratio of 0.3wt% is joined and is got raw material, and it was mixed back ball milling 6.3 hours, under 1100 ℃, founded 68 minutes again, then, and ball milling 6.3 hours and the solid powder that obtains behind the quenching in water, nano-ceramic powder is selected for use alumina powder jointed.Again mixture is placed ball grinder on planetary ball mill, to mix and obtained mixed slurry in 8.3 hours with grinding.2) use mixed slurry spin coating (or spraying or dipping) in the surface of metal base copper (or the semiconductor-based end or superconductor substrate), earlier, wherein, before spin coating metal base copper, earlier it is polished, deoils and cleans; Again with its in 90 ℃ dry 25 minutes down, afterwards, with it successively in 380 ℃ of following thermal treatments 55 minutes, 550 ℃ of following thermal treatment 25 minutes.3), repeat 2) step 4 time, make the nano composite low melting point glass insulation coating shown in Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b).
1), earlier with SiO embodiment 3: finish preparation according to the following steps:
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass and deionized water (or distilled water) according to 100: 35: 15: 300 ratio is mixed mutually; Wherein, SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
235wt%, B
2O
320wt%, ZnO8wt%, CaO9wt%, MgO6wt%, BaO3wt%, Na
210wt%, K
2O7.8wt% and Al
2O
3The ratio of 1.2wt% is joined and is got raw material, and it was mixed back ball milling 7.5 hours, under 12O0 ℃, founded 55 minutes again, then, and ball milling 7.5 hours and the solid powder that obtains behind the quenching in water, nano-ceramic powder is selected for use alumina powder jointed.Again mixture is placed ball grinder on planetary ball mill, to mix and obtained mixed slurry in 7.5 hours with grinding.2) use mixed slurry spin coating (or spraying or dipping) in the surface of metal base copper (or the semiconductor-based end or superconductor substrate), earlier, wherein, before spin coating metal base copper, earlier it is polished, deoils and cleans; Again with its in 100 ℃ dry 20 minutes down, afterwards, with it successively in 400 ℃ of following thermal treatments 45 minutes, 600 ℃ of following thermal treatment 18 minutes.3), repeat 2) step 6 time, make and be similar to the nano composite low melting point glass insulation coating shown in Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b).
1), earlier with SiO embodiment 4: finish preparation according to the following steps:
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass and deionized water (or distilled water) according to 100: 48: 8: 350 ratio is mixed mutually; Wherein, SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
240wt%, B
2O
320wt%, ZnO10wt%, CaO5wt%, MgO4wt%, BaO2wt%, Na
2O11wt%, K
2O7wt% and Al
2O
3The ratio of 1wt% is joined and is got raw material, and it was mixed back ball milling 8.3 hours, under 1250 ℃, founded 44 minutes again, then, and ball milling 8.3 hours and the solid powder that obtains behind the quenching in water, nano-ceramic powder is selected for use alumina powder jointed.Again mixture is placed ball grinder on planetary ball mill, to mix and obtained mixed slurry in 6.3 hours with grinding.2) use mixed slurry spin coating (or spraying or dipping) in the surface of metal base copper (or the semiconductor-based end or superconductor substrate), earlier, wherein, before spin coating metal base copper, earlier it is polished, deoils and cleans; Again with its in 110 ℃ dry 15 minutes down, afterwards, with it successively in 430 ℃ of following thermal treatments 38 minutes, 650 ℃ of following thermal treatment 13 minutes.3), repeat 2) step 8 time, make and be similar to the nano composite low melting point glass insulation coating shown in Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b).
1), earlier with SiO embodiment 5: finish preparation according to the following steps:
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass and deionized water (or distilled water) according to 100: 60: 1: 400 ratio is mixed mutually; Wherein, SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
250wt%, B
2O
315wt%, ZnO7wt%, CaO2wt%, MgO 3wt%, BaO3wt%, Na
2O10wt%, K
2O8.8wt% and Al
2O
3The ratio of 1.2wt% is joined and is got raw material, and it was mixed back ball milling 10 hours, under 1300 ℃, founded 30 minutes again, then, and ball milling 10 hours and the solid powder that obtains behind the quenching in water, nano-ceramic powder is selected for use alumina powder jointed.Again mixture is placed ball grinder on planetary ball mill, to mix and obtained mixed slurry in 5 hours with grinding.2) use mixed slurry spin coating (or spraying or dipping) in the surface of metal base copper (or the semiconductor-based end or superconductor substrate), earlier, wherein, before spin coating metal base copper, earlier it is polished, deoils and cleans; Again with its in 120 ℃ dry 10 minutes down, afterwards, with it successively in 450 ℃ of following thermal treatments 30 minutes, 700 ℃ of following thermal treatment 5 minutes.3), repeat 2) step 10 time, make and be similar to the nano composite low melting point glass insulation coating shown in Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b).
Select for use respectively again in magnesium oxide powder in the nano-ceramic powder or beta-silicon nitride powder or aluminium nitride powder or the aforementioned powder two or more, water glass with silicon sol or methylcellulose gum or polyoxyethylene glycol or aforementioned in two or morely replace, metal base copper replaces with stainless steel or nickel or silver or aluminium, repeat the foregoing description 1～5, make equally and be similar to the nano composite low melting point glass insulation coating shown in Fig. 1 (b), Fig. 2 (b) and Fig. 3 (b).
Obviously, those skilled in the art can carry out various changes and modification to the preparation method of nano composite low melting point glass insulation coating of the present invention and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (8)
1, a kind of preparation method of nano composite low melting point glass insulation coating comprises being coated in the substrate after glass powder made slurry, and drying, sintering again is characterized in that finishing according to the following steps:
1.1, with SiO
2-B
2O
3Be the low melting glass powder with nano-ceramic powder and water glass or silicon sol or methylcellulose gum or polyoxyethylene glycol or aforementioned in two or morely mix mutually according to 100: 5～60: 1～30: 200～400 ratio with water, again its ball milling was obtained mixed slurry in 5～10 hours, wherein, two or more in aforementioned are two or more in water glass or silicon sol or methylcellulose gum or the polyoxyethylene glycol;
1.2, use the mixed slurry coated substrate, again with its in 80～120 ℃ dry 10～30 minutes down, afterwards, with it successively in 350～450 ℃ of following thermal treatments 30～60 minutes, 500～700 ℃ of following thermal treatment 5～30 minutes;
1.3, repeat 1.2 step 3～10 time, make nano composite low melting point glass insulation coating.
2, the preparation method of nano composite low melting point glass insulation coating according to claim 1 is characterized in that SiO
2-B
2O
3Be that the low melting glass powder is served as reasons earlier according to SiO
220～60wt%, B
2O
35～30wt%, ZnO3～25wt%, CaO0.5～10wt%, MgO0.5～7wt%, BaO0.5～5wt%, Na
2O5～20wt%, K
2O5～20wt% and Al
2O
3Get raw material 0.1 the ratio of～2wt% is joined, it was mixed back ball milling 5～10 hours, under 1000～1300 ℃, founded 30～80 minutes again, then, ball milling 5～10 hours and the solid powder that obtains behind the quenching in water.
3, the preparation method of nano composite low melting point glass insulation coating according to claim 1, it is characterized in that nano-ceramic powder be alumina powder jointed or magnesium oxide powder or beta-silicon nitride powder or aluminium nitride powder or aforementioned powder in two or more, its particle diameter is 20～150nm.
4, the preparation method of nano composite low melting point glass insulation coating according to claim 1 is characterized in that water is deionized water or distilled water.
5, the preparation method of nano composite low melting point glass insulation coating according to claim 1 is characterized in that ball milling is to place ball grinder to mix and grinding mixture on planetary ball mill.
6, the preparation method of nano composite low melting point glass insulation coating according to claim 1 is characterized in that being applied to spin coating or spraying or dipping.
7, the preparation method of nano composite low melting point glass insulation coating according to claim 1 is characterized in that substrate is metal base or the semiconductor-based end or superconductor substrate.
8, the preparation method of nano composite low melting point glass insulation coating according to claim 1 is characterized in that before coated substrate, earlier it is polished, deoils and cleans.
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2005
- 2005-07-19 CN CN200510041144A patent/CN100579929C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
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| Ceramic sol-gel composite coatings for electrial insulation. Tim Olding et al.Thin solid films,No.398-399. 2001 |
| Ceramic sol-gel composite coatings for electrial insulation. Tim Olding et al.Thin solid films,No.398-399. 2001 * |
| 电绝缘玻璃材料的研制. 高淑雅等.陕西科技大学学报，第21卷第3期. 2003 |
| 电绝缘玻璃材料的研制. 高淑雅等.陕西科技大学学报，第21卷第3期. 2003 * |
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| CN1899999A (en) | 2007-01-24 |
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