CN103910536A - 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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- CN103910536A CN103910536A CN201410094332.0A CN201410094332A CN103910536A CN 103910536 A CN103910536 A CN 103910536A CN 201410094332 A CN201410094332 A CN 201410094332A CN 103910536 A CN103910536 A CN 103910536A
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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, particularly a kind of method of stamp mark under glazing ceramic metallization pipe glaze.
Background technology
Ceramic-to-metal seal technology is widely used in manufacturing electron tube, vacuum switch tube equal vacuum electron device.At present, the metallized ceramic pipe that sealing-in producer is used mostly adopts outsourcing, and has the phenomenon of same cast from different manufacturers buying.Due to from being difficult in appearance distinguish manufacturer or production batch, therefore, also cannot batch producing by product.When sealing-in producer is in sealing-in production process or when user in use goes wrong, determine that with regard to being difficult to the product going wrong is the metallized ceramic pipe of which producer, which batch.Not yet investigate thoroughly and do not have before corresponding improvement solution in reason, conventionally can only take the mode of stopping production isolation, further expanding to avoid damage.
The sealing-in quality of metallized ceramic pipe is except being subject to the many factors such as technique, the scolder of sealing-in, the material of 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.Once and occur that quality problems cannot understand fully reason being improved conventionally at short notice.Like this, just all cause very big loss 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 this batch of metallized ceramic pipe of isolation, greatly reduce both sides' loss.By lot number, metallized ceramic pipe manufacturer can trace the condition of production of this batch products fast, finds rapidly problem reason and implements preventative quality control method.
At present, domestic there is no is specifically designed to the ink of metallized ceramic pipe stamp mark use and the method for stamp mark, and conventional under glazed pigment is the highest can only bear 1300 ℃ of following temperature, can not meet the requirement of metallized ceramic pipe following process.Because after stamp mark, also need through gloss firing, once to metallize 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 is to carry out sintering at strong reducing property atmosphere is hydrogen nitrogen mixed gas and high temperature 1450-1520 ℃, the inorganic color in color under glaze in high temp pigment is reduced or decomposes, and the handwriting is blurred after causing sintering, and color differs, and is beyond recognition.In the time containing too much solubility salt under glazed pigment or contain more crystal water, also there will be due to problems such as scarce glaze that glaze has more gas to discharge to produce in sintering process, foaming, pin holes.And the purposes of metallized ceramic pipe requires it must possess good electric and mechanical property, therefore, stamp mark can not affect the overall performance of product, and will have good operation and stability.Meanwhile, require the writing of stamp mark clear, color and luster is stable, 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, after the aluminium oxide powder of getting ferric oxide powder, the 40-80% of manganese powder, the 1-5% of chromium sesquioxide powder, the 2-5% of 10-55% according to weight percent mixes, put into baking oven, at the temperature of 100-110 ℃, 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 percent of alumina balls and above-mentioned material is 1-2:1, grind 8-10 hour, make its mean particle size reach 1-5 μ m, screen out alumina balls, obtaining mean particle size is the mixed powder of the above-mentioned material of 1-5 μ m;
3, by ethyl cellulose by weight percentage 1:15-25 join in Terpineol 350, be heated to 100-120 ℃, insulation 12-24 hour, ethyl cellulose dissolve after, the 16-24 hour that rolls on roller bottle machine, fully dissolves ethyl cellulose;
4,1-2:1 joins mixed powder and the terpineol solution that is dissolved with ethyl cellulose in ball mill by weight percentage, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight percent of alumina balls and above-mentioned material is 1-2:1, grind 2-4 hour, make its mean particle size reach 1-5 μ m, 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, alumina ceramic tube is carried out to stamp mark by pad printer;
7, by the alumina ceramic tube after bat printing stamp at the temperature of 140-200 ℃, insulation 2-3 hour, thoroughly solidifies printing-ink, obtains the alumina ceramic tube with stamp mark, after normal glaze spraying, gloss firing, the production of can metallizing.
The invention has the advantages that:
1, in printing-ink of the present invention, introduce chromium element, form and the aluminum oxide formation Solid solution of metallic element and chromium beautiful with chromium steel in spinel type chromic salt mineral make to develop the color, reduce because the corrosion to pigment in glaze melting process causes that the handwriting is blurred and color and luster differs, utilize the affinity that chromic oxide and aluminum oxide are stronger, mark under glaze is not spread to glaze with ceramic surface close contact, the contained metal oxide of pigment can not be reduced under the protection of glaze layer like this, after sintering, glaze is smooth, writing is clear, color and luster is stable, in use procedure, there will not be wire drawing, fluffing, poor adhesive force or the not first-class problem of seal, there is good operability, in addition, can also adjust as required the ratio between four kinds of powders in printing-ink formula, thereby after sintering, obtain from pale red to grayish green different colours, method of the present invention can also be printed trade mark except mark product batch number, there is antiforge function, simultaneously, mark of the present invention can not affect the electric and mechanical property of metallized ceramic pipe entirety.
2, use method of the present invention stamp on every alumina ceramic tube, identify product batch number or date manufactured, can only this batch of product be isolated or be recalled once go wrong, fast processing faulty goods problem, greatly reduce the financial loss of metallized ceramic pipe and sealing-in factory, the perfect trackability of product, improves and preventive measures provide powerful guarantee targetedly to implementing after going wrong, and is conducive to Improving The Quality of Products and the use producer degree of belief to product.
Embodiment:
Embodiment 1:
1.1, get 550g chromium sesquioxide powder, 20g manganese powder, 30g ferric oxide powder, 400g aluminium oxide powder and put into baking oven after mixing, at the temperature of 110 ℃, dry 1 hour;
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 percent of alumina balls and above-mentioned material is 1:1, grind 10 hours, make its mean particle size reach 1-5 μ m, screen out alumina balls, obtaining mean particle size is the mixed powder of the above-mentioned material of 1-5 μ m;
1.3, by ethyl cellulose by weight percentage 1:25 join in Terpineol 350, be heated to 110 ℃, be incubated 20 hours, ethyl cellulose dissolve after, on roller bottle machine, roll 16 hours, ethyl cellulose is fully dissolved;
1.4,1.5:1 joins mixed powder and the terpineol solution that is dissolved with ethyl cellulose in ball mill by weight percentage, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight percent of alumina balls and above-mentioned material is 1:1, grind 3 hours, make its mean particle size reach 1-5 μ m, 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, glaze layer thickness can be controlled by the etching depth of oily steel letters plate, after assurance metallization sintering, on stamp font or pattern, there are enough glaze layer thicknesses, make glaze smooth;
1.6, printing-ink is added in pad printer, alumina ceramic tube is carried out to stamp mark by pad printer;
1.7, by the alumina ceramic tube after bat printing stamp at the temperature of 140 ℃, be incubated 2.5 hours, printing-ink is thoroughly solidified, obtain the alumina ceramic tube with stamp mark, after normal glaze spraying, gloss firing, the production of can metallizing.
Embodiment 2:
2.1, get 100g chromium sesquioxide powder, 50g manganese powder, 50g ferric oxide powder, 800g aluminium oxide powder and put into baking oven after mixing, at the temperature of 100 ℃, dry 1.3 hours;
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 percent of alumina balls and above-mentioned material is 1.5:1, grind 8 hours, make its mean particle size reach 1-5 μ m, screen out alumina balls, obtaining mean particle size is the mixed powder of the above-mentioned material of 1-5 μ m;
2.3, by ethyl cellulose by weight percentage 1:15 join in Terpineol 350, be heated to 120 ℃, be incubated 12 hours, ethyl cellulose dissolve after, on roller bottle machine, roll 24 hours, ethyl cellulose is fully dissolved;
2.4,2:1 joins mixed powder and the terpineol solution that is dissolved with ethyl cellulose in ball mill by weight percentage, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight percent of alumina balls and above-mentioned material is 2:1, grind 2 hours, make its mean particle size reach 1-5 μ m, 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, glaze layer thickness can be controlled by the etching depth of oily steel letters plate, after assurance metallization sintering, on stamp font or pattern, there are enough glaze layer thicknesses, make glaze smooth;
2.6, printing-ink is added in pad printer, alumina ceramic tube is carried out to stamp mark by pad printer;
2.7, by the alumina ceramic tube after bat printing stamp at the temperature of 200 ℃, be incubated 3 hours, printing-ink is thoroughly solidified, obtain the alumina ceramic tube with stamp mark, after normal glaze spraying, gloss firing, the production of can metallizing.
Embodiment 3:
3.1, get 410g chromium sesquioxide powder, 30g manganese powder, 10g ferric oxide powder, 550g aluminium oxide powder and put into baking oven after mixing, at the temperature of 106 ℃, dry 2 hours;
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 percent of alumina balls and above-mentioned material is 2:1, grind 9 hours, make its mean particle size reach 1-5 μ m, screen out alumina balls, obtaining mean particle size is the mixed powder of the above-mentioned material of 1-5 μ m;
3.3, by ethyl cellulose by weight percentage 1:20 join in Terpineol 350, be heated to 100 ℃, be incubated 24 hours, ethyl cellulose dissolve after, on roller bottle machine, roll 20 hours, ethyl cellulose is fully dissolved;
3.4,1:1 joins mixed powder and the terpineol solution that is dissolved with ethyl cellulose in ball mill by weight percentage, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight percent of alumina balls and above-mentioned material is 1.5:1, grind 4 hours, make its mean particle size reach 1-5 μ m, 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, glaze layer thickness can be controlled by the etching depth of oily steel letters plate, after assurance metallization sintering, on stamp font or pattern, there are enough glaze layer thicknesses, make glaze smooth;
3.6, printing-ink is added in pad printer, alumina ceramic tube is carried out to stamp mark by pad printer;
3.7, by the alumina ceramic tube after bat printing stamp at the temperature of 160 ℃, be incubated 2 hours, printing-ink is thoroughly solidified, obtain the alumina ceramic tube with stamp mark, after normal glaze spraying, gloss firing, the production of can metallizing.
Claims (1)
1. a method for stamp mark under glazing ceramic metallization pipe glaze, is characterized in that, it carries out in the steps below:
(1) after the aluminium oxide powder of getting ferric oxide powder, the 40-80% of manganese powder, the 1-5% of chromium sesquioxide powder, the 2-5% of 10-55% according to weight percent mixes, put into baking oven, at the temperature of 100-110 ℃, 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 percent of alumina balls and above-mentioned material is 1-2:1, grind 8-10 hour, make its mean particle size reach 1-5 μ m, screen out alumina balls, obtaining mean particle size is the mixed powder of the above-mentioned material of 1-5 μ m;
(3) by ethyl cellulose by weight percentage 1:15-25 join in Terpineol 350, be heated to 100-120 ℃, insulation 12-24 hour, ethyl cellulose dissolve after, the 16-24 hour that rolls on roller bottle machine, fully dissolves ethyl cellulose;
(4) 1-2:1 joins mixed powder and the terpineol solution that is dissolved with ethyl cellulose in ball mill by weight percentage, add alumina balls, the diameter of alumina balls is Φ 6-Φ 10mm, the weight percent of alumina balls and above-mentioned material is 1-2:1, grind 2-4 hour, make its mean particle size reach 1-5 μ m, cross 200 mesh sieves, obtain printing-ink;
(5) on the oily steel of pad printer, etch font or the pattern that stamp identifies, make bat printing steel plate, etching depth is 0.1-0.4mm;
(6) printing-ink is added in pad printer, alumina ceramic tube is carried out to stamp mark by pad printer;
(7) by the alumina ceramic tube after bat printing stamp at the temperature of 140-200 ℃, insulation 2-3 hour, thoroughly solidifies printing-ink, obtains the alumina ceramic tube with stamp mark.
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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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106910417A (en) * | 2015-12-22 | 2017-06-30 | 德国贺利氏公司 | For carrying out separately encoded method to cermet substrate |
| 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 |
| CN110171981A (en) * | 2019-05-31 | 2019-08-27 | 景德镇景华特种陶瓷有限公司 | A kind of ceramic metallizing paste, preparation method and applications |
| CN111320814A (en) * | 2020-03-16 | 2020-06-23 | 山东成锋医药包装材料有限公司 | Packaging bottle and preparation method thereof |
| CN113149600A (en) * | 2021-04-12 | 2021-07-23 | 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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| CN101353251A (en) * | 2008-09-08 | 2009-01-28 | 苏州大学 | Blackened ceramic infrared radiation material |
| EP1306412B1 (en) * | 2001-10-24 | 2012-05-02 | Merck Patent GmbH | Coloured interference pigments |
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1306412B1 (en) * | 2001-10-24 | 2012-05-02 | Merck Patent GmbH | Coloured interference pigments |
| CN101353251A (en) * | 2008-09-08 | 2009-01-28 | 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 |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106910417A (en) * | 2015-12-22 | 2017-06-30 | 德国贺利氏公司 | For carrying out separately encoded method to cermet substrate |
| CN106910417B (en) * | 2015-12-22 | 2022-10-25 | 德国贺利氏公司 | Method for individually coding a metal-ceramic substrate |
| 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 |
| CN110171981A (en) * | 2019-05-31 | 2019-08-27 | 景德镇景华特种陶瓷有限公司 | A kind of ceramic metallizing paste, preparation method and applications |
| 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 |
| CN111320814A (en) * | 2020-03-16 | 2020-06-23 | 山东成锋医药包装材料有限公司 | Packaging bottle and preparation method 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 |
| CN113149600A (en) * | 2021-04-12 | 2021-07-23 | 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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| CN103910536B (en) | 2015-06-03 |
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