CN101544470A - High-bismuth-oxide dielectric material for electrode coating - Google Patents
High-bismuth-oxide dielectric material for electrode coating Download PDFInfo
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- CN101544470A CN101544470A CN200910102521A CN200910102521A CN101544470A CN 101544470 A CN101544470 A CN 101544470A CN 200910102521 A CN200910102521 A CN 200910102521A CN 200910102521 A CN200910102521 A CN 200910102521A CN 101544470 A CN101544470 A CN 101544470A
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Abstract
The invention provides a high-bismuth-oxide dielectric material for electrode coating, which consists of low-melting-point glass powder and high-temperature ceramic pigment by mass percentage: 80 to 90 percent of the low-melting-point glass powder and 1 to 20 percent of the high-temperature ceramic pigment; BaO and TiO2 are added to a formulation of the low-melting-point glass powder; the compositions of the low-melting-point glass powder by mass percentage are: 50 to 80 percent of Bi2O3, 5 to 20 percent of B2O3, 2 to 20 percent of Al2O3, 1 to 20 percent of SiO2, 0.1 to 20 percent of BaO, 0.01 to 10 percent of TiO2, and 0 to 10 percent of R2O; the R2O is an alkali metal oxide; and the high-temperature ceramic pigment is selected from at least one of TiO2, Al2O3, SiO2, ZrO2, cordierite, mullite, silica, willemite, tin oxide and ZnO. The material has the advantages that the material is small in dielectric constant, excellent in expansion coefficient and the matching property of back substrate glass, high in pressure resistance, incapable of warping after the dielectric material and the substrate glass are sintered, incapable of yellowing after the dielectric material and an electrode are sintered and excellent in compactness, alkali resistance and the strength of diaphragms after sintering, and the manufacture of the material is simple in process, stable in batch production, easy to control and suitable for industrial production.
Description
Technical field
The present invention relates to glass and form, also relate to beramic color, furthermore, relate to the dielectric substance that is used for covering electrodes.
Background technology
Plasmia indicating panel enjoys people to pay close attention to as realizing slim light-weighted indicating meter.The requirement of making material is also more and more become more meticulous.Plasmia indicating panel comprises the front panel and the backplate of glass substrate and configuration integrant thereon.And front panel and backplate dispose in mutual opposed mode, and peripheral part is sealed.Front panel comprises the front glass substrate, is formed with the show electrode of striped shape in its surface, and, be formed with dielectric medium and protective layer in the above; Backplate comprises back side glass substrate, is formed with the address electrode of striped shape in its surface, forms dielectric layer in the above, and, form barrier each other at adjacent address electrode, between the adjacent barrier that forms, form luminescent coating.Front panel and backplate under electrode quadrature that is configured to both and state opposite each other, sealing outer rim, filling inertia discharge gas in being formed at inner enclosed space.Two formations of show electrode are a pair of, and the show electrode that it is a pair of and an addressing electrode become the lattice that helps pictorial display across the clover leaf zone of discharge space.
Because dielectric layer is formed on the electrode, so will have high insulativity; To have low specific inductivity in order to suppress power consumption; For do not peel off and rupture will with the matched coefficients of thermal expansion of base plate glass.Dielectric layer and covering electrodes can not react.And the dielectric layer on formation and the back base plate glass requires its dielectric reflecting rate height usually for display brightness reaches optimum.Chemistry, thermostability to glass require also strict, if the glass that chemical durability is weak, surface after the pulverizing, because the mechanical energy when pulverizing becomes apt to deteriorate, so, just becoming when burning till is easy to generate small bubble, cause resistance to pressure to reduce, in addition, at the big powder of specific area, react with regard to easy and airborne moisture; And the surface takes place to go bad, and steeps from the rotten generation that is present in the powder crystal boundary easily when burning till.Use in the dielectric medium purposes in the address electrode protection, making under the situation of barrier by sand-blast, glass exposure is in basic solution.Use basic solution in the development of dry film photoresist or when peeling off.Therefore,, just produce dielectric layer and be subjected to the basic solution erosion, become not fine and close as making ionogen with the glass a little less than the chemical durability.Dielectric layer is to mix by powder, solvent, tackiness agent, by screen printing technique, is printed onto on the base plate glass, so the affinity of powder and solvent and tackiness agent is the key factor of dielectric layer compactness.
In relevant prior art, No. 200710041637.5 " a kind of lead-free glass powder and preparation methods that are used for covering electrodes " and No. 200710046055.6 " barium crown glass powder for electrode superposition and preparation method thereof " of Donghua University's application, the prepared material of these patented technologies is all undesirable: the specific refractory power of glass and stability are not high, and glass and silver electrode have yellowing phenomenon when burning till.Someone proposes to add a small amount of WO or MnO in glass
2Or both, can suppress the diaphragm jaundice; But cause the glass manufacture difficulty to increase like this.
Summary of the invention
The purpose of this invention is to provide a kind of high-bismuth-oxide dielectric material that is used for covering electrodes, burn till the back warpage or problems such as crackle, diaphragm jaundice occur to solve with base plate glass, provide a kind of and sticking power glass substrate excellent, can improve the material reflecting rate, suppress the material of diaphragm jaundice, improve the chemical stability of material, improve the electrical property and the resistance to pressure of material.
To achieve the above object of the invention, the contriver is through experimental study, and the high-bismuth-oxide dielectric material that is used for covering electrodes that provides is made up of glass powder with low melting point and pyroceramic pigment, and both in the proportioning of massfraction are: glass powder with low melting point 80%～99%; Pyroceramic pigment 1%～20%; Be added with BaO and TiO in the described glass powder with low melting point prescription
2, each component of low melting glass in the composition of massfraction is: Bi
2O
350%～80%, B
2O
35%～20%, Al
2O
32%～20%, SiO
21%～20%, BaO 0.1%～20%, TiO
20.01%～10%, R
2O 0%～10%, wherein R
2O is a kind of in the oxide compound of Li, Na, K; Described pyroceramic pigment is TiO
2, Al
2O
3, SiO
2, ZrO
2, at least a in the trichroite, mullite, silica, willemite, stannic oxide, ZnO.
The contriver points out that prescription characteristics of the present invention are that bismuth oxide is higher relatively, add BaO and TiO simultaneously
2, BaO can improve the specific refractory power of glass, makes the reflecting rate height of material, TiO
2The stability of glass is improved, turn to be yellow in the time of can also suppressing glass and silver electrode and burn till.
The effect of each component is as follows in the prescription of this glass powder:
B
2O
3Can improve thermostability, the chemical stability of glass, increase the specific refractory power of glass, improve the gloss of glass, improve the mechanical property of glass.B
2O
3Also play the effect of fluxing, quicken the clarification of glass and the crystallizing power of reduction glass.TiO
2Can improve the thermostability of glass, increase the chemical stability of glass, can also suppress with the electrode sintering after turn to be yellow.TiO
2Also be the nucleator of glass, make devitrification of glass easily,, add and fashionablely will make each component and TiO so can not add
2Ratio is fit to, and not so milky white can appear in glass.Thereby lose some performances of glass.Bi
2O
3When keeping stability, glass, also have the reduction glass softening point, make glass when fusing, have suitable flowability and the thermal expansivity of regulating glass, increase the proportion of glass.SiO
2Can reduce the thermal expansivity of glass, improve thermostability, chemical stability, softening temperature, resistance to pressure, the physical strength of glass, be network former, the necessary composition of composition.Al
2O
3Belong to intermediate oxide, can reduce the crystallization tendency of glass, improve thermostability, chemical stability, the physical strength of glass.BaO has the phase-splitting of inhibition, increases thermal expansivity, increases stability, glass.R
2Viscosity when O can reduce glass smelting is the good fusing assistant of glass, increases the thermal expansivity of glass, but can not add, and thermostability, chemical stability, the physical strength of glass are reduced, and glass is had a negative impact on the contrary.
Preparing the method that is used for the high-bismuth-oxide dielectric material of covering electrodes of the present invention is: according to after the accurate weighing of each component of formula rate with frit, dry mixed is evenly put into crucible and founded, and rolls sheet, pulverizing, makes glass powder with low melting point, and is standby; Mix according to the pyroceramic pigment of formula rate again, promptly obtain being used for the high-bismuth-oxide dielectric material of covering electrodes with the process weighing.
Glass melting temperature described in the aforesaid method is 1100 ℃～1350 ℃, and melting time is 10～180 minutes.
The high-bismuth-oxide dielectric material that is used for covering electrodes of the present invention does not contain the material to environment and human body harmful, meets China, America and Europe, Japan etc. and has issued the rules that must not contain the content of lead, mercury, cadmium, sexavalent chrome, polymerization bromination biphenyl (PPB), polymerization bromination biphenyl ether (PBDE) and other hazardous and noxious substances from July 1st, 2006 in the electronics product.Material of the present invention burns till that the back is stable, physical strength is excellent, reflecting rate is high (more than 90%); Glass powder in this material is unleaded, stability is excellent, and after the pyroceramic pigment combinations, the matching of specific inductivity little (specific inductivity is smaller or equal to 14 under the 1MHz), the coefficient of expansion and metacoxa glass is excellent, resistance to pressure is high; After burning till with base plate glass, warpage can not take place, after burning till with electrode, can not turn to be yellow; Compactness is excellent, and alkali resistance is excellent.The coefficient of expansion is in the time of 50 ℃～350 ℃ 65～85 * 10
-7, softening temperature is at 450 ℃-660 ℃; It is excellent to burn till rear film intensity; The manufacture craft of material is simple; Mass production is stable, and is easy to control, suitability for industrialized production.This dielectric substance mainly is used in the coating material of addressing electrode on the metacoxa of plasma display system, can also be under the situation that does not increase temperature filler, be used in transparency electrode on the prebasal plate of plasma display system, be used for the sealing-in of other all glass that conform to the coefficient of expansion in this temperature, pottery, metal.
Embodiment
Embodiment:, further set forth the present invention below in conjunction with specific embodiment.
The accurate weighing of the composition of according to the form below massfraction, dry mixed is even, with the glass raw material that mix, be placed in 1300 ℃ of platinum pots in the electric furnace and founded 30 minutes, the glass metal material is drained into roll sheet on the milling train, will roll sheet stock and pulverize, obtain glass powder with low melting point, standby; Take by weighing pyroceramic pigment and glass powder with low melting point uniform mixing more in proportion and promptly get required dielectric medium powder.Tg, Tf point is by the test of DT-40 differential thermal tester in the following table parameter, and thermal expansivity is by the test of ZNO-11 coefficient of expansion determinator, and specific inductivity is by the test of HIOKI 3532-50 LCR tester, and reflecting rate is by the portable reflectance test instrument test of JFB-1 type.
The contriver has carried out 3 batches of tests, below is the test result of 3 batches of tests:
First test-results of table 1
| Example | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Bi 2O 3 | 52.7 | 60 | 57.71 | 68.71 | 62.99 | 68.5 | 60.5 | 63.3 | 66.5 |
| SiO 2 | 11.7 | 5.71 | 6.71 | 6.71 | 6.7 | 2.6 | 1.65 | 1.65 | 1.65 |
| B 2O 3 | 16.5 | 15.05 | 18.07 | 10.07 | 12.96 | 15.65 | 12.8 | 13.2 | 12.32 |
| Al 2O 3 | 4.5 | 3.5 | 3.27 | 5 | 4.95 | 8.35 | 11.35 | 7.35 | 9.33 |
| BaO | 10.4 | 12.24 | 12.24 | 7.24 | 10.4 | 1.5 | 11.5 | 10.5 | 6.5 |
| TiO 2 | 2.2 | 2 | 0.2 | 1.77 | 2 | 2.1 | 1 | 1.6 | 2.3 |
| Na 2O | 1 | 1.5 | / | / | / | 0.8 | 0.8 | 2.4 | 1.4 |
| Li 2O | / | 1 | 0.5 | / | 0.5 | 0.2 | / | / | |
| K 2O | 1 | / | 0.8 | / | / | / | 0.2 | / | / |
| Filler % | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 |
| Tg | 465 | 460 | 463 | 462 | 460 | 465 | 460 | 460 | 462 |
| Tf | 559 | 560 | .556 | 560 | 559 | 556 | 556 | 550 | 575 |
| α | 70 | 70 | 73 | 72 | 73 | 72 | 70 | 72 | 73 |
| p | 5.1 | 5.1 | 5.2 | 5.2 | 5.1 | 5.2 | 5.1 | 5.2 | 5.1 |
| ε | 10 | 10 | 11 | 10 | 10 | 11 | 10 | 11 | 10 |
| Reflecting rate | 91.5 | 93.2 | 90.1 | 92.4 | 92.5 | 93.5 | 90 | 91.2 | 90.4 |
Second batch of test-results of table 2
| Example | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Bi 2O 3 | 65 | 62.4 | 61.25 | 55.71 | 62.25 | 70.5 | 78.05 | 73.3 | 78.09 |
| SiO 2 | 7.4 | 7.5 | 10.5 | 2.4 | 9.54 | 6.8 | 1.65 | 1.65 | 2.85 |
| B 2O 3 | 13.35 | 13.5 | 11.65 | 16.07 | 12.42 | 12 | 15.15 | 11 | 10.56 |
| Al 2O 3 | 7.6 | 8 | 7.4 | 9.7 | 7.26 | 5 | 1.35 | 1.35 | 3.6 |
| Ba0 | 2.2 | 4.2 | 3.6 | 10.42 | 2.6 | 1.4 | 2.5 | 10.5 | 2 |
| TiO 2 | 1.6 | 2 | 5.6 | 2.6 | 4.5 | 2.1 | 1 | 1.6 | 2.3 |
| Na 2O | 1.08 | 2.4 | / | 2.6 | 0.6 | 0.9 | 0.3 | 0.6 | 0.4 |
| Li 2O | 0.8 | / | / | / | 0.83 | 0.8 | / | / | 0.2 |
| K 2O | 0.97 | / | / | 0.5 | / | 0.5 | / | / | / |
| Filler % | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 |
| Tg | 460 | 464 | 466 | 477 | 470 | 460 | 470 | 462 | 460 |
| Tf | 554 | 550 | 558 | 560 | 559 | 556 | 556 | 551 | 554 |
| α | 77 | 78 | 74 | 71 | 79 | 76 | 77 | 75 | 78 |
| p | 5.1 | 5.3 | 5.1 | 5.2 | 5.2 | 5.2 | 5.3 | 5.3 | 5.3 |
| ε | 10 | 11 | 10 | 10 | 11 | 11 | 10 | 10 | 11 |
| Reflecting rate | 94.7 | 94.2 | 94.2 | 94.2 | 94.7 | 93 | 92.2 | 94.2 | 94.7 |
The 3rd batch of test-results of table 3
| Example | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Bi 2O 3 | 56 | 70 | 62 | 60.56 | 71.75 | 60.5 | 58.05 | 60.5 | 66.25 |
| SiO 2 | 10.4 | 8.5 | 2.5 | 6.71 | 9.54 | 3.8 | 1.65 | 5.15 | 7.02 |
| B 2O 3 | 15.35 | 13.1 | 12.65 | 12.07 | 12.42 | 18 | 17.8 | 13 | 10.56 |
| Al 2O 3 | 9 | 2.51 | 11.4 | 2.7 | 4.26 | 3.35 | 1.35 | 1.85 | 5.6 |
| BaO | 2.2 | 4.2 | 5.6 | 8.26 | 0.6 | 5.4 | 18 | 15.5 | 6 |
| TiO 2 | 5.17 | 1 | 4.43 | 8.6 | 0.5 | 7.1 | 1.5 | 1.6 | 2.3 |
| Na 2O | 1.08 | 0.5 | 0.2 | 0.6 | 0.6 | 0.9 | 0.8 | 2.4 | 1.4 |
| Li 2O | 0.8 | 0.19 | 0.22 | / | 0.33 | 0.8 | / | / | 0.87 |
| K 2O | / | / | 1 | 0.5 | / | 0.15 | 0.85 | / | / |
| Filler % | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 |
| Tg | 465 | 460 | 461 | 462 | 464 | 462 | 466 | 462 | 462 |
| Tf | 563 | 559 | 558 | 560 | 559 | 558 | 566 | 565 | 560 |
| α | 71 | 72 | 71 | 73 | 72 | 71 | 73 | 72 | 70 |
| p | 5.1 | 5.3 | 5.2 | 5.2 | 5.3 | 5.2 | 5.1 | 5.2 | 5.2 |
| ε | 11 | 10 | 11 | 11 | 10 | 11 | 11 | 11 | 11 |
| Reflecting rate | 91.7 | 93 | 92.2 | 92.7 | 94.5 | 91.2 | 91.3 | 92 | 92.2 |
More than each the table in, Tg is the softening temperature of glass, Tf is the transition point of glass, α is a thermal expansivity, p is a glass density, ε is a specific inductivity.
Claims (3)
1 one kinds of high-bismuth-oxide dielectric materials that are used for covering electrodes are made up of glass powder with low melting point and pyroceramic pigment, it is characterized in that glass powder with low melting point and pyroceramic pigment in the proportioning of massfraction are: glass powder with low melting point 80%～99%; Pyroceramic pigment 1%～20%; Be added with BaO and TiO in the described glass powder with low melting point prescription
2, each component of low melting glass in the composition of massfraction is: Bi
2O
350%～80%, B
2O
35%～20%, Al
2O
32%～20%, SiO
21%～20%, BaO 0.1%～20%, TiO
20.01%～10%, R
2O 0%～10%, wherein R
2O is a kind of in the oxide compound of Li, Na, K; Described pyroceramic pigment is TiO
2, Al
2O
3, SiO
2, ZrO
2, at least a in the trichroite, mullite, silica, willemite, stannic oxide, ZnO.
2 high-bismuth-oxide dielectric materials that are used for covering electrodes as claimed in claim 1, it is characterized in that this dielectric substance makes in accordance with the following methods: according to after the accurate weighing of each component of formula rate with frit, dry mixed is evenly put into crucible and is founded, roll sheet, pulverizing, make glass powder with low melting point, standby; Mix according to the pyroceramic pigment of formula rate again, promptly obtain being used for the dielectric substance of covering electrodes with the process weighing.
3 a kind of high-bismuth-oxide dielectric materials that are used for covering electrodes as claimed in claim 2 is characterized in that in the manufacturing processed that described glass melting temperature is 1100 ℃～1350 ℃; Described melting time is 10～180 minutes.
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|---|---|---|---|
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2009
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| CN102643023A (en) * | 2012-05-04 | 2012-08-22 | 台州市定向反光材料有限公司 | Environmental-friendly black glaze for automotive glass and preparation method of black glaze |
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| CN102992633B (en) * | 2012-11-10 | 2014-09-10 | 江苏瑞德新能源科技有限公司 | Lead-free and silicon-free glass powder with wide sintering process window and adaptive to back silver paste |
| CN103894694A (en) * | 2014-04-17 | 2014-07-02 | 哈尔滨工业大学 | Method for connection between composite type green low-melting solder glass and silicon carbide reinforced aluminum matrix composites |
| CN105364245A (en) * | 2015-12-17 | 2016-03-02 | 哈尔滨工业大学 | Low-temperature welding method for sapphires |
| CN108298823A (en) * | 2018-04-09 | 2018-07-20 | 东华大学 | A kind of unleaded bismuthic acid salt system glass powder with low melting point and preparation method thereof |
| CN110950537A (en) * | 2018-09-27 | 2020-04-03 | 湖南嘉业达电子有限公司 | Preparation method of low-expansion low-temperature environment-friendly glass glaze |
| CN110217993A (en) * | 2019-06-26 | 2019-09-10 | 鲁米星特种玻璃科技股份有限公司 | A kind of Environment-friendlylow-temperature low-temperature seal glass and preparation method thereof |
| CN110217993B (en) * | 2019-06-26 | 2022-05-27 | 鲁米星特种玻璃科技股份有限公司 | Environment-friendly low-temperature sealing glass and preparation method thereof |
| CN115772005A (en) * | 2021-09-06 | 2023-03-10 | 长春理工大学 | Preparation method of lead-free glass powder for silver paste of solar cell |
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