CN101813888A - Method for regulating and controlling heat stability and photochemical activity of diazonium photoresists - Google Patents
Method for regulating and controlling heat stability and photochemical activity of diazonium photoresists Download PDFInfo
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- CN101813888A CN101813888A CN 201010152116 CN201010152116A CN101813888A CN 101813888 A CN101813888 A CN 101813888A CN 201010152116 CN201010152116 CN 201010152116 CN 201010152116 A CN201010152116 A CN 201010152116A CN 101813888 A CN101813888 A CN 101813888A
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Abstract
The invention relates to a method for regulating and controlling the heat stability and photochemical activity of diazonium photoresists, which is characterized in that: in colloid emulsion which is used for manufacturing screen printing halftone and takes polyving akohol as a photosensitive reaction component, before diazonium resin photosensitizer is added into the colloid emulsion, acid liquor or alkali liquor is added into the colloid emulsion first, so that the pH value of the colloid emulsion is adjusted between 3.0 and 5.0; and by the regulation and control, the diazonium photoresists with different degrees of heat stability and photochemical activity can be obtained according to requirements, and have the advantages of low cost and easy implementation.
Description
Technical field
The present invention relates to a kind of thermal stability of diazo photosensitive emulsion and photochemically reactive regulate and control method, belong to the screen printing technique field.
Background technology
Diazo photosensitive emulsion is easy to use, and price is suitable, and than environmental protection, is widely used in the production of plate-making, metal etch and printed circuit board (PCB) in the silk-screen printing technique etc.The diazo photosensitive emulsion preparation method of prior art generally is to be that the colloid emulsion of photosensitized reaction component adds a certain proportion of diazo resin photosensitizer with the polyvinyl alcohol (PVA).But general diazo resin is stable inadequately to heat, and after colloid emulsion added diazo resin, even preserve under no optical condition, the performance owing to the effect of dark reaction to photoresists produced adverse influence.The dark reaction essence of diazo photosensitive emulsion is that wherein diazo resin decomposes because of the effect of heat, producing in diazo resin free radical and the photoresists polyvinyl alcohol (PVA) reacts and makes it crosslinked, therefore, the diazo photosensitive emulsion storage temperature is high more, the time of placing is long more, serious more to the diazo photosensitive emulsion Effect on Performance, cause finally that its viscosity increases, photochemical activity descends, water development fastness difference and can not using.
At present, improve or prolong the diazo photosensitive emulsion holding time and keep its photochemically reactive method and mainly contain: after (1) colloid emulsion adds the diazo resin photosensitizer, preserve under lower temperature, this method can make the storage life of photoresists prolong, but fails to tackle the problem at its root; (2) in diazo photosensitive emulsion, add stabilizing agent such as polyvinylpyridine, do not see practicality but cost is higher; (3) synthetic low molecule diazo salt with special molecular structure is as the diphenylamine diazonium salt 3-methoxyl that replaces-to diphenylamine-4-diazonium salt etc., further synthetic again its polymeric diazo resin.Some research structures show that this type of diazo resin has stability preferably to heat, be to overcome diazo photosensitive emulsion to thermally labile with keep it stronger photochemically reactive better approach is arranged, but because synthetic starting material and the method for using, cost is higher, also is difficult to apply.
Summary of the invention
The object of the present invention is to provide a kind of thermal stability of diazo photosensitive emulsion and photochemically reactive regulate and control method, this method can make diazo photosensitive emulsion have thermal stability and photochemical activity preferably, can obtain desirable effect as required.
For achieving the above object, thermal stability of diazo photosensitive emulsion provided by the invention and photochemically reactive regulate and control method are: to what make that screen printing screens uses is the colloid emulsion of photosensitized reaction component with the polyvinyl alcohol (PVA), before adding the diazo resin photosensitizer, the pH that adds acid solution or alkali lye adjusting colloid emulsion earlier is 3.0～5.0.
When the pH that regulates colloid emulsion is 3.5～4.2, when preferably pH is 3.8～4.0, can makes the diazo salt aqueous sensitizing glue of acquisition have thermal stability and stronger photochemical activity preferably, and there is long storage period.
When the pH that regulates colloid emulsion is 3.0～3.5, preferably pH is 3.2～3.4, can make diazo salt aqueous sensitizing glue have better thermal stability and more weak photochemical activity.
When the pH of alkali lye adjusting colloid emulsion is 4.3～5.0, preferably pH is 4.4～4.6, can make the diazo salt aqueous sensitizing glue of acquisition have general thermal stability and stronger photochemical activity.
The acid solution that the present invention adopts is the acid solution of broad sense, promptly shows acid aqueous solution, and preferred, described acid solution is one or more in sulfuric acid, hydrochloric acid and the phosphate aqueous solution.
The alkali lye that the present invention adopts is the alkali lye of broad sense, promptly shows the aqueous solution of alkalescence, and is preferred, and described alkali lye is one or more in the aqueous solution of sodium acetate, sodium phosphate, sodium hydrogen phosphate.
The diazo resin photosensitizer of diazo resin photosensitizer of the present invention for synthesizing with right-diphenylamine-4-diazonium salt.
The thermal stability of diazo resin in the medium of different pH values is different with photochemical activity.PH value one timing of medium, temperature is high more, the easy more decomposition of diazo resin photosensitizer, the photochemical activity of diazo photosensitive emulsion prolongs with period of storage and weakens.And temperature one is regularly, the pH value of medium within the specific limits, the decomposition rate of diazo resin photosensitizer strengthens with the rising of pH value, the photochemical activity of diazo photosensitive emulsion also can weaken with the period of storage prolongation.Therefore, by being the regulation and control of pH value of colloid emulsion of the component of photosensitized reaction with the polyvinyl alcohol (PVA), can reach the thermal stability and the photochemically reactive purpose of regulation and control diazo photosensitive emulsion to what be used to make the silk-screen half tone.Because after colloid emulsion adds the diazo resin photosensitizer, they can decompose generation diazo resin free radical under the effect of heat, the diazo resin free radical that produces can with the hydroxyl reaction of polyvinyl alcohol (PVA) in the colloid emulsion, the viscosity of colloid emulsion is increased, photochemical reaction weakens.Therefore, generally all require diazo photosensitive emulsion that thermal stability and stronger photochemical activity are preferably arranged.
The present invention has the following advantages:
(1) by being the regulation and control of pH value of colloid emulsion of the component of photosensitized reaction with the polyvinyl alcohol (PVA), can regulate and control the thermal stability and the photochemical activity of diazo photosensitive emulsion as required to what make that screen printing screens uses;
(2) the pH value of adjusting colloid emulsion is 3.5～4.2, preferably 3.8～4.0, in such cases, storage period behind the colloid emulsion adding diazo resin, performance was kept well than growing, bake out temperature can improve after the half tone gluing, drying time can prolong, and half tone oven dry back taking-up can be placed the long period and do not influenced exposure and water developable profermance;
(3) in some occasion, require adding diazo photosensitive emulsion has better thermal stability and more weak photochemical activity, and this moment, scalable colloid emulsion pH was 3.0～3.5, and preferably 3.2～3.4;
(4) if after wish adding the diazo resin photosensitizer general thermal stability and stronger photochemical activity are arranged, normally pH is 4.3～5.0, preferably 4.4～4.6.
Embodiment
Following examples only are used to set forth the present invention, and protection scope of the present invention is not only to be confined to following examples.The those of ordinary skill of described technical field all can be realized purpose of the present invention according to above content disclosed by the invention and scope that each parameter is got.
Embodiment 1
Get 950g what be used to prepare diazo photosensitive emulsion is the colloid emulsion of the component of photosensitized reaction with the polyvinyl alcohol (PVA), measure its pH value with pH meter or precision test paper, if the pH value is higher than 3.9, then carefully regulate its pH value most 3.9 with dilute sulfuric acid; If the pH value is lower than 3.9, be that 20% sodium acetate solution is regulated its pH value to 3.9 with weight percentage.Add the diazo resin that synthesizes with right-diphenylamine-4-diazonium salt with a small amount of water-soluble 6g in advance then, stir 15min, lucifuge is placed 30～60min to froth breaking in room temperature, pour out part in the gluing tank, operate in 100 order nylon mesh gluings by common gluing, the dry 30min of convection oven that puts into then under the uniform temperature takes out, with identical film pattern, the time post-flush identical in the vacuum exposure machine exposure of the uviol lamp that is equipped with 3000kw develops, with the integrality of water development fastness and developing pattern estimate photoresists to thermal stability and photochemical activity.With the pH value is 4.5 colloid emulsion for to do contrast test by same procedure in the same old way.The results are shown in Table 1.
Table 1 is with the thermal stability and the photochemical activity of the diazo photosensitive emulsion of the colloid emulsion of different pH values preparation
The result shows: pH is colloid emulsion baking 30min under 40 ℃, 45 ℃, 50 ℃ of 3.9, its water development fastness and developing pattern are all normal, and in the same old way except that the genus still of 40 ℃ of oven dry normally, the oven dry difficulty that occurred developing under higher temperature, the resolution of developing pattern descends.Illustrate that colloid emulsion is that 3.9 photoresists have thermal stability and photochemical activity preferably, and that the pH value is the thermal stability of 4.5 colloid emulsion is poorer than the former, in the drying course owing to diazo resin decompose comparatively seriously cause with colloid in the polyvinyl alcohol (PVA) generation cross-linking reaction difficulty of developing.
Embodiment 2
Get 950g what be used to prepare diazo photosensitive emulsion is two parts of the colloid emulsions of the component of photosensitized reaction with the polyvinyl alcohol (PVA), measuring its pH value with pH meter or precision test paper is 2.4, is that 20% sodium acetate solution is regulated its pH value to 3.9 with a copy of it with weight percentage.Add the diazo resin that synthesizes with right-diphenylamine-4-diazonium salt with a small amount of water-soluble 6g in advance respectively at two parts of colloid emulsions then, stir 15min, lucifuge is placed 30～60min to froth breaking in room temperature, pour out part in the gluing tank, operate in 100 order nylon mesh gluings by common gluing, the dry 30min of convection oven that puts into then under 45 ℃ takes out, with identical film pattern, the time post-flush identical in the vacuum exposure machine exposure of the uviol lamp that is equipped with 3000kw develops, with the water development fastness and come the integrality of developing pattern estimate photoresists to thermal stability and photochemical activity.The results are shown in Table 2.
Table 2 is with the thermal stability and the photochemical activity of the diazo photosensitive emulsion of the colloid emulsion of different pH values preparation
With pH is the photoresists of 3.9 colloid emulsion allotment, exposure 20～40s, and the water development fastness is normal, and developing pattern is complete, and it is clear, respond well to differentiate, but behind the exposure 65s, apparent over-exposed, the fine structure of developing pattern can not be differentiated.With the photoresists that the colloid emulsion of pH=2.4 is prepared, exposure 20～30s, glued membrane is almost dashed fully and is taken off during development; Behind exposure 65s, the water development fastness is still only inadequate, and pattern is easily by the water shock wave.These are more weak performances of photochemical activity of photoresists.These presentation of results can be regulated and control the photochemical activity of diazo salt photoresists by the pH value of adjusting colloid emulsion.
Embodiment 3
Get 950g what be used to prepare diazo photosensitive emulsion is two parts of the colloid emulsions of the component of photosensitized reaction with the polyvinyl alcohol (PVA), measuring its pH value with pH meter or precision test paper is 2.4, be that 5% disodium phosphate soln is regulated its pH value to 3.9 with a copy of it, a its pH value to 4.6 of regulating with weight percentage.In two parts of colloid emulsions, add the diazo resin that synthesizes with right-diphenylamine-4-diazonium salt with a small amount of water-soluble 6g in advance then respectively, stir 15min, lucifuge is placed 30～60min to froth breaking in room temperature, pour out part in the gluing tank, operate in 100 order nylon mesh gluings by common gluing, the dry 30min of convection oven that puts into then under 45 ℃ takes out, after lucifuge is placed certain hour under the room temperature, with identical film pattern, the time post-flush identical in the vacuum exposure machine exposure of the uviol lamp that is equipped with 3000kw develops, with the water development fastness and come the integrality of developing pattern estimate photoresists to thermal stability and photochemical activity.The results are shown in Table 3.
Table 3 is with the thermal stability of the diazo salt aqueous sensitizing glue of the colloid emulsion of different pH values preparation
The result shows: the photoresists of using the colloid emulsion allotment of pH=3.9, silk screen gluing oven dry back is placed 24h and is still had normal developing performance and development effect, and with the photoresists of the colloid emulsion of pH=4.6 allotment, promptly can not normal development after 8h is placed in silk screen gluing oven dry back.Show that at a certain temperature the former has bin stability preferably, thereby the stronger photochemical activity of its standing time of long still maintenance; And the latter's bin stability is relatively poor, because photosensitizer decomposes the dark reaction enhancing that causes, glued membrane takes place crosslinked and shows the increase of water development fastness, has influenced the resolution of developing pattern between storage period.Essence is the pH value of colloid emulsion when high (pH=4.6), and the thermal stability variation of photoresists, the photochemical activity of photoresists prolong with period of storage and weaken.Therefore, adjust pH value adjustable its stability and photochemical activity of colloid emulsion to heat.
Embodiment 4
Being used to of 950g prepares 3 parts of the colloid emulsions of diazo photosensitive emulsion, measuring its pH value with pH meter or precision test paper is 2.4, be that 5% disodium phosphate soln is regulated its pH value to 3.4 with a copy of it, a its pH value to 4.0 of regulating, a its pH value to 4.6 of adjusting with weight percentage.In 3 parts of colloid emulsions, add the diazo resin that synthesizes with right-diphenylamine-4-diazonium salt with a small amount of water-soluble 6g in advance then respectively, stir 15min, lucifuge is measured their viscosity after room temperature is placed certain hour, estimate the regulating and controlling effect of colloid emulsion pH value to the thermal stability of photoresists with viscosity change (increase) amplitude.
Table 4 is with the thermal stability of the diazo photosensitive emulsion of the colloid emulsion of different pH values preparation
The result shows: during pH value high (4.6), the viscosity of photoresists is with increasing the fastest standing time, and the pH value be the viscosity of photoresists of 3.5～4.0 colloid emulsion with essentially no variation standing time, illustrate that the colloid emulsion in this pH value scope has thermal stability preferably.
Embodiment 5
Get 950g what be used to prepare diazo photosensitive emulsion is 2 parts of the colloid emulsions of the component of photosensitized reaction with the polyvinyl alcohol (PVA), regulating a pH value with acid solution or alkali lye is 3.0, another part pH value is 4.4, add the diazo resin that synthesizes with right-diphenylamine-4-diazonium salt with a small amount of water-soluble 6g in advance then, stir 15min, lucifuge is placed 30～60min to froth breaking in room temperature, pour out part in the gluing tank, operate in 100 order nylon mesh gluings by common gluing, the dry 30min of convection oven that puts into then under the uniform temperature takes out, with identical film pattern, the time post-flush identical in the vacuum exposure machine exposure of the uviol lamp that is equipped with 3000kw develops, with the water development fastness and come the integrality of developing pattern estimate photoresists to thermal stability and photochemical activity.
The result shows, the pH value is that the thermal stability of 3.0 diazo photosensitive emulsion is better, photochemical activity a little less than, though and the pH value to be the thermal stability of 4.4 diazo photosensitive emulsion general, but photochemical activity is stronger.
Embodiment 6
Get 950g what be used to prepare diazo photosensitive emulsion is 2 parts of the colloid emulsions of the component of photosensitized reaction with the polyvinyl alcohol (PVA), regulating a pH value with acid solution or alkali lye is 3.5, another part pH value is 5.0, add the diazo resin that synthesizes with right-diphenylamine-4-diazonium salt with a small amount of water-soluble 6g in advance then, stir 15min, lucifuge is placed 30～60min to froth breaking in room temperature, pour out part in the gluing tank, operate in 100 order nylon mesh gluings by common gluing, the dry 30min of convection oven that puts into then under the uniform temperature takes out, with identical film pattern, the time post-flush identical in the vacuum exposure machine exposure of the uviol lamp that is equipped with 3000kw develops, with the water development fastness and come the integrality of developing pattern estimate photoresists to thermal stability and photochemical activity.
The result shows, the pH value is that 3.5 diazo photosensitive emulsion has better thermal stability, but photochemical activity is general, and that the pH value is the thermal stability of 5.0 diazo photosensitive emulsion is relatively poor, photochemical activity prolongs decay comparatively fast with period of storage at a certain temperature, then shows stronger photochemical activity but use at a lower temperature after the impregnation.
Claims (10)
1. a thermal stability of diazo photosensitive emulsion and photochemically reactive regulate and control method, it is characterized in that: to what make that screen printing screens uses is the colloid emulsion of photosensitized reaction component with the polyvinyl alcohol (PVA), before adding the diazo resin photosensitizer, the pH that adds acid solution or alkali lye adjusting colloid emulsion earlier is 3.0～5.0.
2. thermal stability of diazo photosensitive emulsion according to claim 1 and photochemically reactive regulate and control method is characterized in that: the pH that regulates colloid emulsion is 3.5～4.2.
3. thermal stability of diazo photosensitive emulsion according to claim 2 and photochemically reactive regulate and control method is characterized in that: the pH that regulates colloid emulsion is 3.8～4.0.
4. thermal stability of diazo photosensitive emulsion according to claim 1 and photochemically reactive regulate and control method is characterized in that: the pH that regulates colloid emulsion is 3.0～3.5.
5. thermal stability of diazo photosensitive emulsion according to claim 4 and photochemically reactive regulate and control method is characterized in that: the pH that regulates colloid emulsion is 3.2～3.4.
6. thermal stability of diazo photosensitive emulsion according to claim 1 and photochemically reactive regulate and control method is characterized in that: the pH that regulates colloid emulsion is 4.3～5.0.
7. thermal stability of diazo photosensitive emulsion according to claim 6 and photochemically reactive regulate and control method is characterized in that: the pH that regulates colloid emulsion is 4.4～4.6.
8. thermal stability of diazo photosensitive emulsion according to claim 1 and photochemically reactive regulate and control method is characterized in that: described acid solution is one or more in sulfuric acid, hydrochloric acid and the phosphate aqueous solution.
9. thermal stability of diazo photosensitive emulsion according to claim 1 and photochemically reactive regulate and control method is characterized in that: described alkali lye is one or more in the aqueous solution of sodium acetate, sodium phosphate, sodium hydrogen phosphate.
10. thermal stability of diazo photosensitive emulsion according to claim 1 and photochemically reactive regulate and control method is characterized in that: the diazo resin photosensitizer of described diazo resin photosensitizer for synthesizing with right-diphenylamine-4-diazonium salt.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048877A (en) * | 2011-10-14 | 2013-04-17 | 武汉海蓝生物技术有限公司 | Ink-jet printing silk screen plate making method and photo-sensitive resist ink thereof |
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| JP2008224698A (en) * | 2005-11-03 | 2008-09-25 | Kissel & Wolf Gmbh | Photopolymerizable stencil material for manufacturing screen printing plate |
| CN101281366A (en) * | 2007-04-06 | 2008-10-08 | 村上精密制版（昆山）有限公司 | Light-sensitive polymer composition not easy to change color and application thereof |
| CN101512436A (en) * | 2007-09-07 | 2009-08-19 | 凯昂公司 | Photosensitive composition containing polyvinyl alcohol and purpose thereof for dye printing method |
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2010
- 2010-04-14 CN CN2010101521169A patent/CN101813888B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1041463A (en) * | 1962-04-27 | 1966-09-07 | Minnesota Mining & Mfg | Light-sensitive diazo material |
| US3679419A (en) * | 1969-05-20 | 1972-07-25 | Azoplate Corp | Light-sensitive diazo condensate containing reproduction material |
| US5700619A (en) * | 1995-07-07 | 1997-12-23 | Sun Chemical Corporation | Acetal polymers and use thereof in photosensitive compositions and lithographic printing plates |
| CN1651527A (en) * | 2003-12-13 | 2005-08-10 | 曼·罗兰·德鲁克马辛伦公司 | Gumming medium |
| JP2008224698A (en) * | 2005-11-03 | 2008-09-25 | Kissel & Wolf Gmbh | Photopolymerizable stencil material for manufacturing screen printing plate |
| CN101281366A (en) * | 2007-04-06 | 2008-10-08 | 村上精密制版（昆山）有限公司 | Light-sensitive polymer composition not easy to change color and application thereof |
| CN101512436A (en) * | 2007-09-07 | 2009-08-19 | 凯昂公司 | Photosensitive composition containing polyvinyl alcohol and purpose thereof for dye printing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048877A (en) * | 2011-10-14 | 2013-04-17 | 武汉海蓝生物技术有限公司 | Ink-jet printing silk screen plate making method and photo-sensitive resist ink thereof |
| CN103048877B (en) * | 2011-10-14 | 2014-06-18 | 武汉海蓝生物技术有限公司 | Ink-jet printing silk screen plate making method and photo-sensitive resist ink thereof |
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