CN104658707A - Method for preparing photo-curing copper electronic paste - Google Patents
Method for preparing photo-curing copper electronic paste Download PDFInfo
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- CN104658707A CN104658707A CN201510066529.8A CN201510066529A CN104658707A CN 104658707 A CN104658707 A CN 104658707A CN 201510066529 A CN201510066529 A CN 201510066529A CN 104658707 A CN104658707 A CN 104658707A
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Abstract
The invention discloses a method for preparing a photo-curing copper electronic paste. The method specifically comprises the following steps: weighing hydrazine hydrate, PVP and copper powder respectively; preparing a mixed solvent from the hydrazine hydrate, the PVP and the copper powder, and heating the mixed solvent for reaction to prepare pre-treated copper powder; weighing epoxy acrylate, dipentaerythritol pentaacrylate, acyl phosphorus oxide TPO, silane coupling agent KH550 and a defoamer respectively, and mixing the five weighed materials to prepare a photo-curing solvent; mixing the pre-treated copper powder and the photo-curing solvent to obtain a mixture, and printing the mixture on a glass substrate through a silk screen; performing photo-curing treatment on the glass substrate to prepare the photo-curing copper electronic paste. The method for preparing the photo-curing copper electronic paste is simple in process, capable of carrying out production without special equipment, efficient, and energy-saving, and causes less pollution to the environment; the prepared electronic paste is excellent in conductivity and long in shelf life.
Description
Technical field
The invention belongs to electronic package material preparation method technical field, be specifically related to a kind of preparation method of photocuring copper electric slurry.
Background technology
In recent years, along with the high speed development of electronic technology, people become electronic product and more and more rely on, and electric slurry is one of basic material preparing electronic devices and components.Nowadays, along with the progressively enhancing of people's environmental protection and awareness of saving energy, develop environmental protection (Ecology), efficient (Efficiency), energy-conservation (Energy), low cost (Economy) electric slurry become study hotspot and the emphasis of people.
The preparation process of existing electric slurry mainly by raw material after silk screen printing, be positioned in baking oven and dry, whole preparation process required time is longer, and has certain requirement to used equipment in preparation process.
UV-curing technology is that liquid is rapidly converted into the most effective technology of solid, UV-curing technology is applied to the emphasis that electric slurry preparation becomes Recent study.UV-curing technology has following advantage: (1) environmental protection: substantially not containing solvent in photo-curing material, non-volatile, environmentally safe; (2) efficient: curing time is shorter; (3) energy-conservation: without the need to heating in ultraviolet light polymerization process, institute's energy requirement is only about 1/5 of hot curing; (4) low cost: consume energy low and efficiency is high, can reduce production cost to greatest extent.
In addition, in the process preparing electric slurry, the selection of conductive filler is also very important, this is because conductive filler is the key factor affecting electric slurry conductivity.Although noble metal (as: Au, Ag etc.) has excellent conductivity, costly, particularly Ag in use, Ag for its price
+can transport phenomena be there is, thus reduce its useful life, reduce the scope of application; Cu in base metal becomes the study hotspot of people in recent years, its main cause is: the source of Cu is comparatively extensive, and conductivity is only lower than Ag, and higher than Au, performance can meet the requirement preparing electric slurry, but but there is oxidizable, easy reunion and the problem low with substrate combinating strength in fine copper powder.
For these reasons, be necessary that very much seeking one can improve the oxidation resistant modified technique of Copper Powder Surface, prepare a kind ofly carry out suitability for industrialized production, there is good electric conductivity, can the environment-friendly type photocuring electric slurry of long term storage.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of photocuring copper electric slurry, utilize the Cu in base metal to prepare in conjunction with UV-curing technology and there is superior electrical conductivity and can the electric slurry of long term storage.
The technical solution adopted in the present invention is, the preparation method of photocuring copper electric slurry, specifically implements according to following steps:
Step 1, take hydrazine hydrate, polyvinylpyrrolidone PVP and copper powder respectively; Utilize hydrazine hydrate, polyvinylpyrrolidone PVP and copper powder to make mixed solvent, thermal response is added to mixed solvent, prepares preliminary treatment copper powder;
Step 2, prepare preliminary treatment copper powder through step 1 after, take epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer respectively, then prepare photocuring solvent by after take five kinds of material mixing;
Step 3, by prepare through step 1 to preliminary treatment copper powder with after the photocuring solvent that step 2 prepares, obtain mixture, by mixture through screen printing on glass substrate;
Step 4, photocuring process is carried out to the glass substrate obtained through step 3, prepare photocuring copper electric slurry.
Feature of the present invention is also,
Step 1 is specifically implemented according to following steps:
Step 1.1, be that 2 ~ 4:1 ~ 3:5 ~ 8 take hydrazine hydrate, polyvinylpyrrolidone PVP, copper powder respectively according to mass ratio;
Step 1.2, first the hydrazine hydrate taken in step 1.1, polyvinylpyrrolidone PVP and copper powder are mixed formation mixed solvent, then use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 60 DEG C ~ 80 DEG C under the state stirred, the supernatant in the process of agitating heating in mixed solvent becomes black;
Step 1.3, through step 1.2, after the supernatant in solvent to be mixed becomes black, first leave standstill 10min ~ 20min, then outwell supernatant, obtain compounding substances A;
Step 1.4, the compounding substances A absolute ethyl alcohol obtained through step 1.3 and deionized water are cleaned 2 times ~ 3 times respectively, obtain compounding substances B; Then compounding substances B is put into vacuum drying box to dry.
In step 1.4, baking temperature is 80 DEG C ~ 100 DEG C, and drying time is 2h ~ 3h.
Step 2 is specifically implemented according to following steps:
Step 2.1, prepare preliminary treatment copper powder through step 1 after, be that 65 ~ 80:8 ~ 15:4 ~ 10:3 ~ 10:3 ~ 5 take epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer respectively in mass ratio;
Step 2.2, the epoxy acrylate taken in step 2.1, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer to be mixed, prepare photocuring solvent.
Step 3 is specifically implemented according to following steps:
Step 3.1, be that 65 ~ 85:35 ~ 15 take the preliminary treatment copper powder prepared through step 1, the photocuring solvent prepared through step 2 respectively in mass ratio;
Step 3.2, by the preliminary treatment copper powder that takes through step 3.1 and photocuring solvent even, prepare mixture;
Step 3.3, by the mixture that obtains through step 3.2 through screen printing on glass substrate.
In step 4, photocuring processing procedure is specially:
What adopt is that ultraviolet medium pressure mercury lamp irradiates the glass substrate obtained through step 3, and the time of irradiation is 40s ~ 100s.
Beneficial effect of the present invention is:
1. in the preparation method of photocuring copper electric slurry of the present invention, utilize hydrazine hydrate to make reducing agent, PVP does dispersant, in order to remove the oxide layer of Copper Powder Surface, through magnetic agitation, leave standstill acquisition copper powder pre-coated body, then dry and obtain preliminary treatment copper powder; Adopt epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer as photocuring solvent; Preliminary treatment copper powder is prepared photocuring electric slurry as conductive phase; By the copper slurry for preparing through silk screen printing on a glass substrate, adopt curing molding under middle-ultraviolet lamp medium pressure mercury lamp of suitable time, namely obtain the conductive copper slurry that can be used for Electronic Packaging coating.
2., in the preparation method of photocuring copper electric slurry of the present invention, utilize copper base metal as conductive filler, cheap due to copper wide material sources, effectively can reduce production cost.
3. have employed photocuring technology in the preparation method of photocuring copper electric slurry of the present invention, there is efficient, energy-conservation, environmentally friendly and cheap feature, be highly suitable for suitability for industrialized production.
4. the preparation method of photocuring copper electric slurry of the present invention has simple, lower to the equipment requirement advantage of preparation flow, and the not leaded cadmium composition of the conductive copper films prepared is pollution-free, and electric conductivity is excellent, and can long-term storage.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The preparation method of photocuring copper electric slurry of the present invention, specifically implements according to following steps:
Step 1, take hydrazine hydrate, PVP and copper powder respectively; Utilize hydrazine hydrate, PVP and copper powder to make mixed solvent, thermal response added to mixed solvent, prepare preliminary treatment copper powder, specifically implement according to following steps:
Step 1.1, be that 2 ~ 4:1 ~ 3:5 ~ 8 take hydrazine hydrate, polyvinylpyrrolidone PVP, copper powder respectively according to mass ratio;
Step 1.2, first the hydrazine hydrate taken in step 1.1, polyvinylpyrrolidone PVP and copper powder are mixed formation mixed solvent, then use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 60 DEG C ~ 80 DEG C under the state stirred, the supernatant in the process of agitating heating in mixed solvent becomes black;
Step 1.3, through step 1.2, after the supernatant in solvent to be mixed becomes black, first leave standstill 10min ~ 20min, then outwell supernatant, obtain compounding substances A;
Step 1.4, the compounding substances A absolute ethyl alcohol obtained through step 1.3 and deionized water are cleaned 2 times ~ 3 times respectively, obtain compounding substances B; Then compounding substances B is put into vacuum drying box to dry;
Wherein, it is 80 DEG C ~ 100 DEG C that baking temperature controls, and drying time is 2h ~ 3h, obtains preliminary treatment copper powder.
Step 2, prepare preliminary treatment copper powder through step 1 after; take epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer respectively; then prepare photocuring solvent by after take five kinds of material mixing, specifically implement according to following steps:
Step 2.1, prepare preliminary treatment copper powder through step 1 after, be that 65 ~ 80:8 ~ 15:4 ~ 10:3 ~ 10:3 ~ 5 take epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer respectively in mass ratio;
Step 2.2, the epoxy acrylate taken in step 2.1, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer to be mixed, prepare photocuring solvent.
Step 3, by prepare through step 1 to preliminary treatment copper powder with after the photocuring solvent that step 2 prepares, obtain mixture, by mixture through screen printing on glass substrate, specifically implement according to following steps:
Step 3.1, be that 65 ~ 85:35 ~ 15 take the preliminary treatment copper powder prepared through step 1, the photocuring solvent prepared through step 2 respectively in mass ratio;
Step 3.2, by the preliminary treatment copper powder that takes through step 3.1 and photocuring solvent even, prepare mixture;
Step 3.3, by the mixture that obtains through step 3.2 through screen printing on glass substrate.
Step 4, photocuring process is carried out to the glass substrate obtained through step 3, prepares photocuring copper electric slurry of the present invention, specifically implement in accordance with the following methods:
In the photocuring processing procedure of step 4, employing be that ultraviolet medium pressure mercury lamp irradiates the glass substrate obtained through step 3, the time of irradiation is 40s ~ 100s.
In the preparation method of photocuring copper electric slurry of the present invention:
(1) utilize hydrazine hydrate to make reducing agent, PVP does dispersant, effectively can remove the oxide layer of Copper Powder Surface, through magnetic agitation, leaves standstill acquisition copper powder pre-coated body, then dries and obtain preliminary treatment copper powder;
(2) adopt epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer as photocuring solvent, pretreated copper powder prepares photocuring electric slurry as conductive phase;
(3) by the copper slurry for preparing through silk screen printing on a glass substrate, adopt curing molding under middle-ultraviolet lamp medium pressure mercury lamp of suitable time, obtain the conductive copper slurry that can be used for Electronic Packaging coating.
Embodiment 1
Be that 2:3:8 takes hydrazine hydrate, PVP, copper powder respectively according to mass ratio; Be mixed the hydrazine hydrate taken, PVP, copper powder formation mixed solvent, use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 60 DEG C under stirring, supernatant in the process adding thermal agitation in mixed solvent becomes black, leave standstill 10min afterwards, outwell supernatant again, obtain compounding substances A; Compounding substances A absolute ethyl alcohol and deionized water are cleaned 2 times respectively, obtains compounding substances B; Then compounding substances B is put into vacuum drying box, under 80 DEG C of conditions, drying 3h, obtains preliminary treatment copper powder;
Epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer is taken respectively in mass ratio for 65:8:10:10:5; The epoxy acrylate taken, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer are mixed, prepares photocuring solvent;
Preliminary treatment copper powder, photocuring solvent is taken respectively in mass ratio for 65:30; By the preliminary treatment copper powder that takes and photocuring solvent evenly after, obtain mixture; By mixture through screen printing on glass substrate;
Adopt ultraviolet medium pressure mercury lamp to irradiate glass substrate, carry out photocuring process, the time of irradiation is 50s, prepares photocuring copper electric slurry of the present invention.
Embodiment 2
Be that 2:1:5 takes hydrazine hydrate, PVP, copper powder respectively according to mass ratio; Be mixed the hydrazine hydrate taken, PVP, copper powder formation mixed solvent, use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 70 DEG C under stirring, supernatant in the process adding thermal agitation in mixed solvent becomes black, leave standstill 15min afterwards, outwell supernatant again, obtain compounding substances A; Compounding substances A absolute ethyl alcohol and deionized water are cleaned 2 times respectively, obtains compounding substances B; Then compounding substances B is put into vacuum drying box, under 85 DEG C of conditions, drying 160min, obtains preliminary treatment copper powder;
Epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer is taken respectively in mass ratio for 65:8:4:3:3; The epoxy acrylate taken, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer are mixed, prepares photocuring solvent;
Preliminary treatment copper powder, photocuring solvent is taken respectively in mass ratio for 75:25; By the preliminary treatment copper powder that takes and photocuring solvent evenly after, obtain mixture; By mixture through screen printing on glass substrate;
Adopt ultraviolet medium pressure mercury lamp to irradiate glass substrate, carry out photocuring process, the time of irradiation is 65s, prepares photocuring copper electric slurry of the present invention.
Embodiment 3
Be that 3:1.5:7 takes hydrazine hydrate, PVP, copper powder respectively according to mass ratio; Be mixed the hydrazine hydrate taken, PVP, copper powder formation mixed solvent, use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 75 DEG C under stirring, supernatant in this course in mixed solvent becomes black, leave standstill 18min afterwards, outwell supernatant again, obtain compounding substances A; Compounding substances A absolute ethyl alcohol and deionized water are cleaned 3 times respectively, obtains compounding substances B; Then compounding substances B is put into vacuum drying box, under 90 DEG C of conditions, drying 140min, obtains preliminary treatment copper powder;
Epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550, defoamer is taken respectively in mass ratio for 75:10:8:8:4; The epoxy acrylate taken, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer are mixed, prepares photocuring solvent;
Preliminary treatment copper powder, photocuring solvent is taken respectively in mass ratio for 80:20; By the preliminary treatment copper powder that takes and photocuring solvent evenly after, obtain mixture; By mixture through screen printing on glass substrate;
Adopt ultraviolet medium pressure mercury lamp to irradiate glass substrate, carry out photocuring process, the time of irradiation is 75s, prepares photocuring copper electric slurry of the present invention.
Embodiment 4
Be that 4:3:8 takes hydrazine hydrate, PVP, copper powder respectively according to mass ratio; Be mixed the hydrazine hydrate taken, PVP, copper powder formation mixed solvent, use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 80 DEG C under stirring, supernatant in this course in mixed solvent becomes black, leave standstill 20min afterwards, outwell supernatant again, obtain compounding substances A; Compounding substances A absolute ethyl alcohol and deionized water are cleaned 3 times respectively, obtains compounding substances B; Then compounding substances B is put into vacuum drying box, under 100 DEG C of conditions, drying 120min, obtains preliminary treatment copper powder;
Epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550, defoamer is taken respectively in mass ratio for 80:15:10:10:5; The epoxy acrylate taken, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer are mixed, prepares photocuring solvent;
Preliminary treatment copper powder, photocuring solvent is taken respectively in mass ratio for 85:15; By the preliminary treatment copper powder that takes and photocuring solvent evenly after, obtain mixture; By mixture through screen printing on glass substrate;
Adopt ultraviolet medium pressure mercury lamp to irradiate glass substrate, carry out photocuring process, the time of irradiation is 100s, prepares photocuring copper electric slurry of the present invention.
Test according to four kinds of photocuring copper electric slurry four-point probe prepared by above-mentioned four embodiments (embodiment 1 ~ embodiment 4), gained resistance is as shown in table 1, after can finding out the copper slurry solidification prepared by four embodiments, its resistance is all in m Ω level, shows good electric conductivity.
Table 1
| Example number | Sheet resistance |
| 1 | 30.24 |
| 2 | 28.97 |
| 3 | 18.23 |
| 4 | 25.14 |
In the preparation method of photocuring copper electric slurry of the present invention, using copper base metal as conductive filler, wide material sources, cheap; Coordinate photocuring technology, there is efficient, energy-conservation, environmentally friendly and cheap advantage, suitable very for suitability for industrialized production; In addition, whole preparation process is simple, lower to equipment requirement, the electrocondution slurry prepared, and not leaded cadmium composition is pollution-free, and electric conductivity is excellent, and can long-term storage.
Claims (6)
1. the preparation method of photocuring copper electric slurry, is characterized in that, concrete steps are:
Step 1, take hydrazine hydrate, polyvinylpyrrolidone PVP and copper powder respectively; Utilize hydrazine hydrate, polyvinylpyrrolidone PVP and copper powder to make mixed solvent, thermal response is added to mixed solvent, prepares preliminary treatment copper powder;
Step 2, prepare preliminary treatment copper powder through step 1 after, take epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer respectively, then prepare photocuring solvent by after take five kinds of material mixing;
Step 3, by prepare through step 1 to preliminary treatment copper powder with after the photocuring solvent that step 2 prepares, obtain mixture, by mixture through screen printing on glass substrate;
Step 4, photocuring process is carried out to the glass substrate obtained through step 3, prepare photocuring copper electric slurry.
2. the preparation method of photocuring copper electric slurry according to claim 1, it is characterized in that, described step 1 is specifically implemented according to following steps:
Step 1.1, be that 2 ~ 4:1 ~ 3:5 ~ 8 take hydrazine hydrate, polyvinylpyrrolidone PVP, copper powder respectively according to mass ratio;
Step 1.2, first the hydrazine hydrate taken in step 1.1, polyvinylpyrrolidone PVP and copper powder are mixed formation mixed solvent, then use constant temperature blender with magnetic force that the mixed solvent of formation is heated to 60 DEG C ~ 80 DEG C under the state stirred, the supernatant in the process of agitating heating in mixed solvent becomes black;
Step 1.3, through step 1.2, after the supernatant in solvent to be mixed becomes black, first leave standstill 10min ~ 20min, then outwell supernatant, obtain compounding substances A;
Step 1.4, the compounding substances A absolute ethyl alcohol obtained through step 1.3 and deionized water are cleaned 2 times ~ 3 times respectively, obtain compounding substances B; Then compounding substances B is put into vacuum drying box to dry.
3. the preparation method of photocuring copper electric slurry according to claim 2, is characterized in that, in described step 1.4, baking temperature is 80 DEG C ~ 100 DEG C, and drying time is 2h ~ 3h.
4. the preparation method of photocuring copper electric slurry according to claim 1, it is characterized in that, described step 2 is specifically implemented according to following steps:
Step 2.1, prepare preliminary treatment copper powder through step 1 after, be that 65 ~ 80:8 ~ 15:4 ~ 10:3 ~ 10:3 ~ 5 take epoxy acrylate, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer respectively in mass ratio;
Step 2.2, the epoxy acrylate taken in step 2.1, double pentaerythritol C5 methacrylate, acyl group phosphorous oxides TPO, Silane coupling agent KH550 and defoamer to be mixed, prepare photocuring solvent.
5. the preparation method of photocuring copper electric slurry according to claim 1, it is characterized in that, described step 3 is specifically implemented according to following steps:
Step 3.1, be that 65 ~ 85:35 ~ 15 take the preliminary treatment copper powder prepared through step 1, the photocuring solvent prepared through step 2 respectively in mass ratio;
Step 3.2, by the preliminary treatment copper powder that takes through step 3.1 and photocuring solvent even, prepare mixture;
Step 3.3, by the mixture that obtains through step 3.2 through screen printing on glass substrate.
6. the preparation method of photocuring copper electric slurry according to claim 1, it is characterized in that, in described step 4, photocuring processing procedure is specially:
What adopt is that ultraviolet medium pressure mercury lamp irradiates the glass substrate obtained through step 3, and the time of irradiation is 40s ~ 100s.
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| CN105161219A (en) * | 2015-09-28 | 2015-12-16 | 西安工程大学 | Preparation method for UV light-cured silver-coated nickel conductive slurry |
| CN105722254A (en) * | 2016-02-24 | 2016-06-29 | 东莞珂洛赫慕电子材料科技有限公司 | Photo-curable resistance paste for flexible electrothermal film and preparation method of photo-curable resistance paste |
| CN106041122A (en) * | 2016-07-13 | 2016-10-26 | 许勤峰 | Method for preparing nanometre copper-catalyzed slurry by virtue of PCB acidic waste liquid |
| CN106077700A (en) * | 2016-07-13 | 2016-11-09 | 许勤峰 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
| CN113327721A (en) * | 2021-08-04 | 2021-08-31 | 西安宏星电子浆料科技股份有限公司 | Preparation method of low-temperature cured conductive copper paste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105161219A (en) * | 2015-09-28 | 2015-12-16 | 西安工程大学 | Preparation method for UV light-cured silver-coated nickel conductive slurry |
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| CN106041122A (en) * | 2016-07-13 | 2016-10-26 | 许勤峰 | Method for preparing nanometre copper-catalyzed slurry by virtue of PCB acidic waste liquid |
| CN106077700A (en) * | 2016-07-13 | 2016-11-09 | 许勤峰 | A kind of method utilizing circuit board waste liquid to prepare Nanometer Copper catalysis slurry |
| CN113327721A (en) * | 2021-08-04 | 2021-08-31 | 西安宏星电子浆料科技股份有限公司 | Preparation method of low-temperature cured conductive copper paste |
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Application publication date: 20150527 |