CN114049986A - Lead-free and bismuth-free high-performance dielectric slurry - Google Patents
Lead-free and bismuth-free high-performance dielectric slurry Download PDFInfo
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- CN114049986A CN114049986A CN202111619720.2A CN202111619720A CN114049986A CN 114049986 A CN114049986 A CN 114049986A CN 202111619720 A CN202111619720 A CN 202111619720A CN 114049986 A CN114049986 A CN 114049986A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/008—Other insulating material
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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
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Abstract
The invention discloses a lead-free and bismuth-free high-performance dielectric paste, which consists of modified glass powder and an organic carrier; the modified glass powder is obtained by mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol and then vibrating through a vibration mill; the organic carrier is composed of ethyl cellulose, lecithin and methallyl alcohol. Compared with the traditional high-bismuth glass powder used for the dielectric paste, the glass powder used for the dielectric paste has the advantages that the pollution is low, the particle size of glass powder particles is more concentrated, and the glass powder has a lower softening point and stronger chemical stability; the organic carrier uses methallyl alcohol to replace the traditional terpineol, and further improves the chemical stability of the carrier and the dispersibility of the carrier to powder. The prepared medium slurry has high chemical stability, high compactness, high homogeneity, low pollution and capacity of being used in low temperature section.
Description
Technical Field
The invention belongs to the technical field of dielectric paste, and particularly relates to a lead-free bismuth-free dielectric paste with excellent performance.
Background
With the development of the times, the importance and the demand of the dielectric paste in the industries of thick film integrated circuits, electronic components, semiconductors and the like are increasing due to the excellent chemical stability, corrosion resistance, higher breakdown voltage and simpler preparation process of the dielectric paste; as protective slurry, various performance requirements for media slurry are also increasing.
The glass powder adopted in the traditional dielectric paste is high-bismuth system glass powder, and although the lead-free performance is realized, along with the development of times, the requirement of people on environmental protection is further improved, the higher pollution performance of bismuth is increasingly emphasized, and the bismuth-free performance is gradually brought into the required range by the electronic manufacturing industry of various countries; meanwhile, the disadvantage of higher cost of the high bismuth system glass powder is gradually exposed, and a more suitable glass powder needs to be found to replace the high bismuth glass powder. Meanwhile, with the continuous improvement of the demand, the performances of the traditional medium slurry, such as chemical stability, corrosion resistance, compactness after sintering and the like, are probably improved in time, so that the medium slurry meeting the requirements is needed at present.
Disclosure of Invention
In order to solve the problems, the invention provides a lead-free and bismuth-free high-performance medium slurry, which aims to solve the problems of pollution, chemical stability, compactness and the like of the medium slurry.
Aiming at the purposes, the lead-free and bismuth-free high-performance dielectric paste provided by the invention comprises 60-85% of modified glass powder and 15-40% of organic carrier by weight of 100%; the modified glass powder is obtained by mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol and then performing modification treatment through a vibration mill; the organic carrier is composed of ethyl cellulose, lecithin and methallyl alcohol.
The Ba-Si-Zn-Al-Pt glass powder comprises the following components in percentage by weight: 27-40% of barium oxide, 18-30% of silicon dioxide, 5-10% of aluminum oxide, 20-40% of zinc oxide, 2-10% of boron trioxide and 0.5-1.5% of platinum powder.
The preparation method of the Ba-Si-Zn-Al-Pt glass powder comprises the following steps: the method comprises the steps of fully and uniformly mixing barium oxide, silicon dioxide, aluminum oxide, zinc oxide, boron trioxide and platinum powder according to weight percentage, putting the obtained mixture into a high-temperature resistance furnace at 1100-1200 ℃ for smelting for 1-2 hours, then carrying out water quenching on molten glass liquid to obtain glass slag, refining the glass slag until the granularity D50 is less than or equal to 1.5 mu m, then carrying out ball material separation by using a 325-mesh stainless steel screen, drying and sieving to obtain Ba-Si-Zn-Al-Pt glass powder.
The modified glass powder is obtained by mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol according to the weight ratio of 7: 1-5.5: 1, adding the mixture into a vibration mill, and vibrating for 0.5-2 hours.
The organic carrier comprises the following components in percentage by weight: 7-15% of ethyl cellulose, 7-15% of lecithin and 75-85% of methallyl alcohol.
The invention has the following beneficial effects:
1. the modified glass powder used by the dielectric paste is Ba-Si-Zn-Al-Pt glass powder, the Ba-Si-Zn-Al-Pt glass powder is lead-free and bismuth-free, the pollution of materials is reduced, the chemical stability is good, the softening point is lower, and the prepared paste can be used in a low-temperature section.
2. The glass powder can enable the particle size of powder particles to be more concentrated through vibration mill treatment, but the vibration mill has larger energy, so that the appearance of the glass powder is easy to destroy on a large scale, and the condition can be effectively avoided by adding methallyl alcohol as a coating agent; and the heating condition is serious in the using process of the vibration mill, and the heat stability of the methyl allyl alcohol is good.
3. The solvent of the organic carrier used by the medium slurry is methyl allyl alcohol, and new impurities cannot be introduced when the modified glass powder is used; compared with the traditional terpineol solvent, the dispersibility and the dispersion retentivity of the methallyl alcohol are better, the dispersibility of the slurry can be better, the compactness is higher, and the sedimentation and delamination can not occur for a long time.
Drawings
FIG. 1 is a photomicrograph of the sintered surface film of the media slurry prepared in example 1.
Figure 2 is a photomicrograph of the sintered surface film of the media slurry prepared in example 2.
FIG. 3 is a photomicrograph of the sintered surface film of the media slurry prepared in example 3.
Fig. 4 is a photomicrograph of the sintered surface film of the media slurry prepared in comparative example 1.
Fig. 5 is a photomicrograph of the sintered surface film of the media slurry prepared in comparative example 2.
Fig. 6 is a photomicrograph of the sintered surface film of the media slurry prepared in comparative example 3.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
Preparing modified glass powder: the preparation method comprises the following steps of preparing 1kg of materials in a 3L polyethylene tank according to the weight percentage of 30% of barium oxide, 25% of silicon dioxide, 6% of aluminum oxide, 35% of zinc oxide, 3.5% of boron trioxide and 0.5% of platinum powder, sealing the opening of the polyethylene tank, and mixing the materials on an eight-roller ball mill for 1 hour; after the mixing is finished, pouring the mixed glass material into a 2L quartz crucible, putting the quartz crucible into a high-temperature resistance furnace at 1200 ℃ for smelting for 2 hours, and quenching the completely molten glass liquid to obtain glass slag; adding glass slag and deionized water in a weight ratio of 1:0.73 into a 5L corundum ball milling tank, placing the 5L corundum ball milling tank on an eight-roller ball mill for ball milling until the particle size D50 is less than or equal to 1.5 mu m, then using a 325-mesh stainless steel screen mesh for ball material separation, placing the separated glass liquid in a 120 ℃ oven for drying for 18 hours, and using a 60-mesh stainless steel screen mesh for dry powder screening of the dried glass powder to obtain Ba-Si-Zn-Al-Pt glass powder; mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol according to the weight ratio of 6.5:1, pouring the mixture into a vibration mill, starting the vibration mill to vibrate for 0.5 hour, and discharging to obtain the modified glass powder.
Preparation of organic vehicle: the organic carrier consists of 10 percent of ethyl cellulose, 10 percent of lecithin and 80 percent of methallyl alcohol by weight percentage, and the total amount of the ingredients is 2 kg; firstly, adding methallyl alcohol into a 3L stainless steel barrel, then adding ethyl cellulose, starting stirring, heating the solution to 55 ℃ after the ethyl cellulose begins to be dissolved in a large amount and the solution begins to change color, then adding lecithin, carrying out melt processing for 2 hours, and sieving by using a 200-mesh stainless steel sieve mesh to obtain the organic carrier.
Preparing medium slurry: mixing 85% of modified glass powder and 15% of organic carrier according to the weight percentage of the medium slurry to obtain 1kg in total, mixing the materials by using a three-roll mill, and then rolling to obtain the medium slurry with the fineness of 8 mu m.
Example 2
Preparing modified glass powder: the preparation method comprises the following steps of preparing 1kg of barium oxide, 20% of silicon dioxide, 8% of aluminum oxide, 30% of zinc oxide, 7% of boron trioxide and 1% of platinum powder in a 3L polyethylene tank according to the weight percentage, sealing the opening of the polyethylene tank, and mixing materials on an eight-roller ball mill for 1 hour; after the mixing is finished, pouring the mixed glass material into a 2L quartz crucible, putting the quartz crucible into a high-temperature resistance furnace at 1150 ℃ for smelting for 2 hours, and quenching the completely molten glass liquid to obtain glass slag; adding glass slag and deionized water in a weight ratio of 1:0.73 into a 5L corundum ball milling tank, placing the 5L corundum ball milling tank on an eight-roller ball mill for ball milling until the particle size D50 is less than or equal to 1.5 mu m, then using a 325-mesh stainless steel screen mesh for ball material separation, placing the separated glass liquid in a 120 ℃ oven for drying for 18 hours, and using a 60-mesh stainless steel screen mesh for dry powder screening of the dried glass powder to obtain Ba-Si-Zn-Al-Pt glass powder; mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol according to the weight ratio of 6:1, pouring the mixture into a vibration mill, starting the vibration mill to vibrate for 1 hour, and discharging to obtain the modified glass powder.
Preparation of organic vehicle: the organic carrier is composed of 7% of ethyl cellulose, 8% of lecithin and 85% of methallyl alcohol by weight percentage, and the total amount of the ingredients is 2 kg; firstly, adding methallyl alcohol into a 3L stainless steel barrel, then adding ethyl cellulose, starting stirring, heating the solution to 55 ℃ after the ethyl cellulose begins to be dissolved in a large amount and the solution begins to change color, then adding lecithin, carrying out melt processing for 2 hours, and sieving by using a 200-mesh stainless steel sieve mesh to obtain the organic carrier.
Preparing medium slurry: 75% of modified glass powder and 25% of organic carrier are mixed according to the weight percentage of the medium slurry to be 1kg in total, a three-roll mill is used for mixing materials, and then rolling is carried out to obtain the medium slurry with the fineness of 8 mu m.
Example 3
Preparing modified glass powder: the preparation method comprises the following steps of preparing 1kg of materials according to the weight percentage of 40% of barium oxide, 18% of silicon dioxide, 10% of aluminum oxide, 22% of zinc oxide, 8.5% of boron trioxide and 1.5% of platinum powder in a 3L polyethylene tank, sealing the opening of the polyethylene tank, and mixing the materials on an eight-roller ball mill for 1 hour; after the mixing is finished, pouring the mixed glass material into a 2L quartz crucible, putting the quartz crucible into a high-temperature resistance furnace at 1100 ℃ for smelting for 1 hour, and quenching the completely molten glass liquid to obtain glass slag; adding glass slag and deionized water in a weight ratio of 1:0.73 into a 5L corundum ball milling tank, placing the 5L corundum ball milling tank on an eight-roller ball mill for ball milling until the particle size D50 is less than or equal to 1.5 mu m, then using a 325-mesh stainless steel screen mesh for ball material separation, placing the separated glass liquid in a 120 ℃ oven for drying for 18 hours, and using a 60-mesh stainless steel screen mesh for dry powder screening of the dried glass powder to obtain Ba-Si-Zn-Al-Pt glass powder; mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol according to the weight ratio of 5.5:1, pouring the mixture into a vibration mill, starting the vibration mill to vibrate for 3 hours, and discharging to obtain the modified glass powder.
Preparation of organic vehicle: the organic carrier consists of 15 percent of ethyl cellulose, 10 percent of lecithin and 75 percent of methallyl alcohol by weight percentage, and the total amount of the ingredients is 2 kg; firstly, adding methallyl alcohol into a 3L stainless steel barrel, then adding ethyl cellulose, starting stirring, heating the solution to 55 ℃ after the ethyl cellulose begins to be dissolved in a large amount and the solution begins to change color, then adding lecithin, carrying out melt processing for 2 hours, and sieving by using a 200-mesh stainless steel sieve mesh to obtain the organic carrier.
Preparing medium slurry: mixing 65% of modified glass powder and 35% of organic carrier according to the weight percentage of the medium slurry to obtain 1kg in total, mixing the materials by using a three-roll mill, and then rolling to obtain the medium slurry with the fineness of 8 mu m.
Comparative example 1
In example 1, methallyl alcohol used in the preparation of the organic vehicle was replaced with terpineol of the same weight, and the other steps were the same as in example 1, to obtain a medium slurry with a fineness of 8 μm.
Comparative example 2
In example 1, the Ba-Si-Zn-Al-Pt glass powder was not subjected to vibration treatment by a vibration mill, and the remaining steps were the same as in example 1, thereby obtaining a medium slurry with a fineness of 8 μm.
Comparative example 3
In example 1, Ba-Si-Zn-Al-Pt glass powder was not subjected to vibration treatment by a vibration mill, methallyl alcohol used in the preparation of the organic vehicle was replaced with terpineol of equal weight, and other steps were the same as in example 1, thereby obtaining a medium slurry having a fineness of 8 μm.
The dielectric paste prepared in the above examples 1 to 3 and comparative examples 1 to 3 was printed on alumina substrates 10mm long × 10mm wide × 1mm thick by using an automatic printing machine, the film thickness was 50 μm, 6 substrates were printed, all substrates were sintered by using a 550 ℃ sintering furnace, and the results were detected by using a 50-fold microscope, and are shown in fig. 1 to 6.
Placing the sintered sheet into a dilute sulfuric acid water solution with the mass concentration of 5% to be soaked for 72 hours, observing the falling condition of a sintered film, and evaluating the acid resistance; and the sintered substrate was subjected to dielectric loss, insulation resistance and breakdown voltage tests in sequence, the test results are shown in table 1.
TABLE 1
| Surface sintered film state | Sintered film state after soaking dilute sulfuric acid | Dielectric loss (%) | Insulation resistance (omega) | Breakdown voltage (V/50μm) | |
| Example 1 | Is flat and compact | Can not fall off | 0.10 | 7.41×1012 | 1520 |
| Example 2 | Is flat and compact | Can not fall off | 0.14 | 4.01×1012 | 1370 |
| Example 3 | Is smooth and compact | Can not fall off | 0.19 | 9.27×1011 | 1145 |
| Comparative example 1 | Is flat and compact with a small amount of bubbles | Can not fall off | 0.16 | 1.64×109 | 753 |
| Comparative example 2 | Concave-convex bubble | Begin to fall off | 0.26 | 5.73×1010 | 1090 |
| Comparative example 3 | Concave-convex with obvious bubbles | The falling-off condition is obvious | 0.31 | 1.04×108 | 523 |
As can be seen from table 1, by comparing example 1, example 2 and example 3, the higher the content of glass frit in the dielectric paste, the better each property of the dielectric paste prepared therefrom; comparing example 1 with comparative example 1, the organic carrier solvent is changed into terpineol, and the insulation resistance and breakdown voltage of the prepared dielectric paste are greatly reduced; comparing the embodiment 1 with the comparative embodiment 2, the glass powder is not modified, and all performances of the obtained dielectric paste are obviously reduced; comparing example 1 with comparative example 3, it can be seen that the glass frit is not modified, the organic vehicle is terpineol, and the properties of the obtained dielectric paste are sharply reduced.
Claims (5)
1. A lead-free and bismuth-free high-performance dielectric paste is characterized in that: the medium slurry consists of 60-85% of modified glass powder and 15-40% of organic carrier by weight of 100%;
the modified glass powder is obtained by mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol and then performing modification treatment through a vibration mill;
the organic carrier is composed of ethyl cellulose, lecithin and methallyl alcohol.
2. The lead-free and bismuth-free high performance dielectric paste as claimed in claim 1, wherein the Ba-Si-Zn-Al-Pt based glass powder comprises, in weight percent: 27-40% of barium oxide, 18-30% of silicon dioxide, 5-10% of aluminum oxide, 20-40% of zinc oxide, 2-10% of boron trioxide and 0.5-1.5% of platinum powder.
3. The lead-free and bismuth-free high performance dielectric paste according to claim 2, wherein the preparation method of the Ba-Si-Zn-Al-Pt series glass powder comprises: the method comprises the steps of fully and uniformly mixing barium oxide, silicon dioxide, aluminum oxide, zinc oxide, boron trioxide and platinum powder according to weight percentage, putting the obtained mixture into a high-temperature resistance furnace at 1100-1200 ℃ for smelting for 1-2 hours, then carrying out water quenching on molten glass liquid to obtain glass slag, refining the glass slag until the granularity D50 is less than or equal to 1.5 mu m, then carrying out ball material separation by using a 325-mesh stainless steel screen, drying and sieving to obtain Ba-Si-Zn-Al-Pt glass powder.
4. The lead-free and bismuth-free high performance dielectric paste according to any one of claims 1 to 3, wherein: mixing Ba-Si-Zn-Al-Pt glass powder and methallyl alcohol according to the weight ratio of 7: 1-5.5: 1, adding the mixture into a vibration mill, and vibrating for 0.5-2 hours to obtain the modified glass powder.
5. The lead-free bismuth-free high performance media paste of claim 1 wherein the organic vehicle comprises in weight percent: 7-15% of ethyl cellulose, 7-15% of lecithin and 75-85% of methallyl alcohol.
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