CN103910536B - Underglaze code printing method for glazed and metalized ceramic pipe - Google Patents
Underglaze code printing method for glazed and metalized ceramic pipe Download PDFInfo
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Abstract
The invention relates to an underglaze code printing method for a glazed and metalized ceramic pipe. The method includes: a step of uniformly mixing 10-55% by weight of chromic oxide powder, 2-5% by weight of manganese powder, 1-5% by weight of ferric oxide powder and 40-80% by weight of aluminium oxide powder, drying at 100-110 DEG C for 1-2 h, and grinding the material mixture for 8-10 h; a step of adding ethyecellulose into terpilenol according to a weight ratio of 1:15-25, heating to 100-120 DEG C, maintaining the temperature for 12-24 h, and rolling on a bottle turning machine for 16-24 h; a step of grinding the powder mixture and the terpilenol solution containing the ethyecellulose according to a weight ratio of 1-2:1 for 2-4 h, and sieving with a sieve having a size of 200 meshes to obtain printing ink; a step of etching fonts or patterns for code printing in oil steel of a pad printer and subjecting an aluminum oxide ceramic pipe to code printing; and a step of maintaining the temperature of the aluminum oxide ceramic pipe at 140-200 DEG C for 2-3 h to obtain the aluminum oxide ceramic pipe with the code printing.
Description
Technical field:
The invention belongs to vacuum electronic components and parts production technical field, a kind of method that particularly under glazing ceramic metallization pipe glaze, stamp identifies.
Background technology
Ceramic-to-metal seal technology is widely used in manufacturing the vacuum electron device such as electron tube, vacuum switch tube.At present, the metallized ceramic pipe that sealing-in producer uses mostly adopts outsourcing, and there is the phenomenon that same cast purchases from different manufacturers.Due to from being difficult in appearance distinguish manufacturer or production batch, therefore, also cannot batch to produce by product.When sealing-in producer is in sealing-in production process or when user in use goes wrong, the product with regard to being difficult to determine to go wrong is the metallized ceramic pipe of which producer, which batch.Before reason is not yet investigated thoroughly and do not had corresponding improvement solution, usually can only take the mode of isolating that stops production, expand further to avoid damage.
The sealing-in quality of metallized ceramic pipe is except the many factors such as the material by the technique of sealing-in, solder, hardware, and the quality of metallized ceramic pipe itself also plays very large impact.Because preparation technology's cycle of metallized ceramic pipe is long, stability is bad, poor anti jamming capability, shortage effectively detect and performance analysis, meanwhile, the metallized ceramic pipe manufacturer automation level of enterprises is low, so, often there will be quality problems.And once occur that quality problems usually cannot be understood fully reason at short notice and be improved.Like this, just all extreme loss is caused to metallized ceramic pipe and sealing-in manufacturer.
In view of above problem, if all stamp product batch number on every metallized ceramic pipe, after going wrong like this, only need isolate this batch of metallized ceramic pipe, greatly reduce both sides' loss.By lot number, metallized ceramic pipe manufacturer can trace the condition of production of this batch products fast, finds questions and prospect rapidly and implements preventative quality control method.
At present, the domestic method that there is no ink and the stamp mark being specifically designed to metallized ceramic pipe stamp mark, the conventional the highest temperature can only bearing less than 1300 DEG C of under glazed pigment, can not meet the requirement of metallized ceramic pipe following process.Because after stamp mark, also need through gloss firing, once metallization and second metallization sintering, glaze also has second melting and solidification process.Therefore, adopt general under glazed pigment to there will be diffusion phenomena, the problem such as make that the handwriting is blurred unclear.And once metallization sinters at strong reducing property atmosphere and hydrogen nitrogen mixed gas and high temperature 1450-1520 DEG C, and the inorganic color in color under glaze in high temp pigment is reduced or decomposes, cause after sintering that the handwriting is blurred, color differs, and is beyond recognition.When containing too much solubility salt under glazed pigment or containing more crystal water, also there will be the problem such as scarce glaze, foaming, pin hole produced because glaze has more gas to discharge in sintering process.And the purposes of metallized ceramic pipe requires that it must possess good electric and mechanical property, and therefore, stamp mark can not affect the overall performance of product, and will have well operation and stability.Meanwhile, the writing requiring stamp to identify is clear, color stability, can not destroy the smooth finish of glaze layer.
Summary of the invention:
The object of the invention is to solve the problem of stamp mark under metallized ceramic pipe glaze, the method for stamp mark under a kind of glazing ceramic metallization pipe glaze is provided.
Production method of the present invention is:
1, get the chromium sesquioxide powder of 10-55% according to weight percent, the manganese powder of 2-5%, the ferric oxide powder of 1-5%, the aluminium oxide powder of 40-80% put into baking oven after mixing, at the temperature of 100-110 DEG C, dry 1-2 hour;
2, above-mentioned material is put into ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1-2:1, grinding 8-10 hour, make its mean particle size reach 1-5 μm, screen out alumina balls, obtain the mixed powder that mean particle size is the above-mentioned material of 1-5 μm;
3, join in Terpineol 350 by ethyl cellulose by weight 1:15-25, be heated to 100-120 DEG C, insulation 12-24 hour, after ethyl cellulose is dissolved, roller bottle machine rolls 16-24 hour, and ethyl cellulose is fully dissolved;
4, by weight 1-2:1, mixed powder and the terpineol solution that is dissolved with ethyl cellulose are joined in ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1-2:1, grinding 2-4 hour, make its mean particle size reach 1-5 μm, cross 200 mesh sieves, obtain printing-ink;
5, on the oily steel of pad printer, etch font or the pattern of stamp mark, make bat printing steel plate, etching depth is 0.1-0.4mm;
6, printing-ink is added in pad printer, by pad printer, stamp mark is carried out to alumina ceramic tube;
7, by the alumina ceramic tube after bat printing stamp at the temperature of 140-200 DEG C, insulation 2-3 hour, printing-ink is thoroughly solidified, namely obtain with stamp mark alumina ceramic tube, after normal glaze spraying, gloss firing, can carry out metallization production.
The invention has the advantages that:
1, chromium element is introduced in printing-ink of the present invention, the form of colour developing metallic element and chromium beautiful with chromium steel in spinel type chromic salt mineral and aluminum oxide is made to form Solid solution, decrease owing to causing the corrosion of pigment in glaze melting process that the handwriting is blurred and color and luster differs, utilize chromic oxide and the stronger affinity of aluminum oxide, make mark and ceramic surface close contact under glaze and do not spread to glaze paint, metal oxide contained by such pigment can not be reduced under the protection of glaze layer, after sintering, glaze paint is smooth, writing is clear, color stability, wire drawing is there will not be in use procedure, fluffing, poor adhesive force or the not first-class problem of print, there is good operability, in addition, the ratio between four kinds of powders in printing-ink formula can also be adjusted as required, thus obtain from pale red to grayish green different colours after sintering, method of the present invention can also print trade mark except mark product batch number, there is antiforge function, simultaneously, mark of the present invention can not affect the electric of metallized ceramic pipe entirety and mechanical property.
2, method of the present invention stamp on every alumina ceramic tube is used, identify product batch number or date manufactured, can only isolate this batch of product once go wrong or recall, fast processing faulty goods problem, greatly reduce the financial loss of metallized ceramic pipe and sealing-in factory, the perfect trackability of product, to improve targetedly and preventive measures provide powerful guarantee implementing after going wrong, being conducive to Improving The Quality of Products and using producer to the degree of belief of product.
Embodiment:
Embodiment 1:
1.1, get 550g chromium sesquioxide powder, 20g manganese powder, 30g ferric oxide powder, 400g aluminium oxide powder put into baking oven after mixing, dry 1 hour at the temperature of 110 DEG C;
1.2, above-mentioned material is put into ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1:1, grind 10 hours, make its mean particle size reach 1-5 μm, screen out alumina balls, obtain the mixed powder that mean particle size is the above-mentioned material of 1-5 μm;
1.3, ethyl cellulose is joined in Terpineol 350 by weight 1:25, be heated to 110 DEG C, be incubated 20 hours, after ethyl cellulose is dissolved, roller bottle machine rolls 16 hours, ethyl cellulose is fully dissolved;
1.4, by weight 1.5:1, mixed powder and the terpineol solution that is dissolved with ethyl cellulose are joined in ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1:1, grind 3 hours, make its mean particle size reach 1-5 μm, cross 200 mesh sieves, obtain printing-ink;
1.5, on the oily steel of pad printer, etch font or the pattern of stamp mark, make bat printing steel plate, etching depth is 0.1mm, glazed thickness is controlled by the etching depth of oily steel letters plate, after ensureing metallization sintering, stamp font or pattern there are enough glazed thickness, make glaze paint smooth;
1.6, printing-ink is added in pad printer, by pad printer, stamp mark is carried out to alumina ceramic tube;
1.7, by the alumina ceramic tube after bat printing stamp at the temperature of 140 DEG C, be incubated 2.5 hours, printing-ink thoroughly solidified, namely obtain with stamp mark alumina ceramic tube, after normal glaze spraying, gloss firing, can carry out metallization production.
Embodiment 2:
2.1, get 100g chromium sesquioxide powder, 50g manganese powder, 50g ferric oxide powder, 800g aluminium oxide powder put into baking oven after mixing, dry 1.3 hours at the temperature of 100 DEG C;
2.2, above-mentioned material is put into ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1.5:1, grind 8 hours, make its mean particle size reach 1-5 μm, screen out alumina balls, obtain the mixed powder that mean particle size is the above-mentioned material of 1-5 μm;
2.3, ethyl cellulose is joined in Terpineol 350 by weight 1:15, be heated to 120 DEG C, be incubated 12 hours, after ethyl cellulose is dissolved, roller bottle machine rolls 24 hours, ethyl cellulose is fully dissolved;
2.4, by weight 2:1, mixed powder and the terpineol solution that is dissolved with ethyl cellulose are joined in ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 2:1, grind 2 hours, make its mean particle size reach 1-5 μm, cross 200 mesh sieves, obtain printing-ink;
2.5, on the oily steel of pad printer, etch font or the pattern of stamp mark, make bat printing steel plate, etching depth is 0.3mm, glazed thickness is controlled by the etching depth of oily steel letters plate, after ensureing metallization sintering, stamp font or pattern there are enough glazed thickness, make glaze paint smooth;
2.6, printing-ink is added in pad printer, by pad printer, stamp mark is carried out to alumina ceramic tube;
2.7, by the alumina ceramic tube after bat printing stamp at the temperature of 200 DEG C, be incubated 3 hours, printing-ink thoroughly solidified, namely obtain with stamp mark alumina ceramic tube, after normal glaze spraying, gloss firing, can carry out metallization production.
Embodiment 3:
3.1, get 410g chromium sesquioxide powder, 30g manganese powder, 10g ferric oxide powder, 550g aluminium oxide powder put into baking oven after mixing, dry 2 hours at the temperature of 106 DEG C;
3.2, above-mentioned material is put into ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 2:1, grind 9 hours, make its mean particle size reach 1-5 μm, screen out alumina balls, obtain the mixed powder that mean particle size is the above-mentioned material of 1-5 μm;
3.3, ethyl cellulose is joined in Terpineol 350 by weight 1:20, be heated to 100 DEG C, be incubated 24 hours, after ethyl cellulose is dissolved, roller bottle machine rolls 20 hours, ethyl cellulose is fully dissolved;
3.4, by weight 1:1, mixed powder and the terpineol solution that is dissolved with ethyl cellulose are joined in ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1.5:1, grind 4 hours, make its mean particle size reach 1-5 μm, cross 200 mesh sieves, obtain printing-ink;
3.5, on the oily steel of pad printer, etch font or the pattern of stamp mark, make bat printing steel plate, etching depth is 0.4mm, glazed thickness is controlled by the etching depth of oily steel letters plate, after ensureing metallization sintering, stamp font or pattern there are enough glazed thickness, make glaze paint smooth;
3.6, printing-ink is added in pad printer, by pad printer, stamp mark is carried out to alumina ceramic tube;
3.7, by the alumina ceramic tube after bat printing stamp at the temperature of 160 DEG C, be incubated 2 hours, printing-ink thoroughly solidified, namely obtain with stamp mark alumina ceramic tube, after normal glaze spraying, gloss firing, can carry out metallization production.
Claims (1)
1. the method that under glazing ceramic metallization pipe glaze, stamp identifies, it is characterized in that, it carries out in the steps below:
(1) get the chromium sesquioxide powder of 10-55% according to weight percent, the manganese powder of 2-5%, the ferric oxide powder of 1-5%, the aluminium oxide powder of 40-80% put into baking oven after mixing, at the temperature of 100-110 DEG C, dry 1-2 hour;
(2) above-mentioned material is put into ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1-2:1, grinding 8-10 hour, make its mean particle size reach 1-5 μm, screen out alumina balls, obtain the mixed powder that mean particle size is the above-mentioned material of 1-5 μm;
(3) join in Terpineol 350 by ethyl cellulose by weight 1:15-25, be heated to 100-120 DEG C, insulation 12-24 hour, after ethyl cellulose is dissolved, roller bottle machine rolls 16-24 hour, and ethyl cellulose is fully dissolved;
(4) by weight 1-2:1, mixed powder and the terpineol solution being dissolved with ethyl cellulose are joined in ball mill, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight ratio of alumina balls and above-mentioned material is 1-2:1, grinding 2-4 hour, make its mean particle size reach 1-5 μm, cross 200 mesh sieves, obtain printing-ink;
(5) on the oily steel of pad printer, etch font or the pattern of stamp mark, make bat printing steel plate, etching depth is 0.1-0.4mm;
(6) printing-ink is added in pad printer, by pad printer, stamp mark is carried out to alumina ceramic tube;
(7) by the alumina ceramic tube after bat printing stamp at the temperature of 140-200 DEG C, insulation 2-3 hour, printing-ink is thoroughly solidified, namely obtain with stamp mark alumina ceramic tube.
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| CN201410094332.0A CN103910536B (en) | 2014-03-14 | 2014-03-14 | Underglaze code printing method for glazed and metalized ceramic pipe |
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| CN201410094332.0A CN103910536B (en) | 2014-03-14 | 2014-03-14 | Underglaze code printing method for glazed and metalized ceramic pipe |
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| EP3185655B8 (en) * | 2015-12-22 | 2024-01-03 | Heraeus Electronics GmbH & Co. KG | Method for the individual encoding of metal-ceramic substrates |
| CN109627036A (en) * | 2018-12-26 | 2019-04-16 | 常熟市银洋陶瓷器件有限公司 | A kind of metallizing paste and preparation method thereof suitable for 99% aluminium oxide ceramics |
| CN110171981B (en) * | 2019-05-31 | 2021-09-03 | 景德镇景华特种陶瓷有限公司 | Ceramic metallization paste, preparation method and application thereof |
| CN111320814B (en) * | 2020-03-16 | 2023-01-06 | 山东成锋医药包装材料有限公司 | Packaging bottle and preparation method thereof |
| CN113149600B (en) * | 2021-04-12 | 2022-10-25 | 佛山市东鹏陶瓷有限公司 | Rock plate with anti-counterfeiting mark and preparation method thereof |
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| DE10151844A1 (en) * | 2001-10-24 | 2003-05-08 | Merck Patent Gmbh | Colored interference pigments |
| CN101353251B (en) * | 2008-09-08 | 2011-09-14 | 苏州大学 | Blackened ceramic infrared radiation material |
| CN103172408A (en) * | 2013-04-12 | 2013-06-26 | 锦州金属陶瓷有限公司 | High-strength aluminum oxide ceramic metalized paste and preparation method thereof |
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