CN105693093A - Preparation method of electronic paste for low-temperature leadless encapsulation - Google Patents
Preparation method of electronic paste for low-temperature leadless encapsulation Download PDFInfo
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- CN105693093A CN105693093A CN201410705934.5A CN201410705934A CN105693093A CN 105693093 A CN105693093 A CN 105693093A CN 201410705934 A CN201410705934 A CN 201410705934A CN 105693093 A CN105693093 A CN 105693093A
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Abstract
The invention relates to the field of electronic glass production technology, especially to a preparation method of electronic paste for low-temperature leadless encapsulation. The preparation method of the electronic paste for low-temperature leadless encapsulation comprises the following steps: weighing the following raw materials (by weight): 50.0-96.0 parts of Bi2O3, 2.0-20.0 parts of ZnO, 2.0-30.0 parts of B2O3, 0-2.0 parts of CuO, 0-3.0 parts of Cr2O3, 0-2.0 parts of SrO and 0-3.0 parts of BaO, and uniformly mixing; carrying out thermal insulation at the temperature of 900-1200 DEG C for 1-2 h and melting to form molten glass, pouring the molten glass onto a preheated stainless steel plate, and tabletting to prepare glass sheet; levigating the glass sheet, and sieving to prepare glass fine powder; uniformly mixing a refractory filler and the glass fine powder according to the mass ratio of 0-5:20 so as to obtain sealing powder; and adding the sealing powder into an organic solvent with solid-state mass fraction of the sealing powder being 65-90%, and uniformly mixing the above two substances. Sealing temperature of the electronic paste prepared by the preparation method of the electronic paste for low-temperature leadless encapsulation is within 400-600 DEG C, and expansion coefficient is adjustable within 50-115*10<-7>/DEG C.
Description
Technical field
The present invention relates to electronic glass production technical field, the preparation method of especially a kind of low-temperature lead-free packaging electric slurry。
Background technology
Electric slurry is generally by paste through three-roll rolling mix homogeneously of pressed powder and organic solvent。In tradition, the sintering main body of low-temperature pulp mostly is lead bearing glass, but owing in process of production, human body can be caused very major injury, serious environment pollution by the volatilization of PbO, European Union, the U.S., Japan etc. implement to prohibit the plumbous instruction of lead limit in succession。China has also formulated " electronics and information industry portion pollutes protection management way ", limits and uses the poisonous and harmful substances such as lead, cadmium, hydrargyrum in electronic product, and electric slurry is progressively to low lead, unleaded development。
At present, electric slurry crown glass mainly has phosphate glass, vanadate glass, silicon-boron glass etc. and the vanadium of the argentiferous that sealing temperature is below 300 DEG C-tellurium glass。But, phosphate, vanadate glass chemical stability are not as good as lead glass;Silver-containing glass cost is high, is not suitable for commonly used;Silicon-boron glass melting temperature sealing is all more than 500 DEG C。Further, the coefficient of expansion of electric slurry of the prior art is big, is not suitable for the encapsulation of low-expansion coefficient base material。
Summary of the invention
In order to overcome the deficiency that above-mentioned electric slurry sealing temperature is high and the coefficient of expansion is big, the invention provides a kind of low-temperature lead-free packaging electric slurry, between the sealing temperature of described low-temperature lead-free packaging electric slurry 400 DEG C~600 DEG C, the coefficient of expansion is 50~115 × 10-7/ DEG C between adjustable。
The object of the invention to solve the technical problems realizes by the following technical solutions。
By the preparation method of a kind of low-temperature lead-free packaging electric slurry, comprise the following steps:
(1) raw material that quality share is following ratio is weighed: Bi2O350.0~96.0, ZnO2.0~20.0, B2O32.0~30.0, CuO0~2.0, Cr2O30~3.0, SrO0~2.0, BaO0~3.0, mix homogeneously;
(2) being incubated fusing in 1~2 hour under 900~1200 DEG C of temperature conditions and form vitreous humour, be poured on by vitreous humour on preheated corrosion resistant plate, tabletting prepares sheet glass;
(3) sheet glass step (2) obtained is levigate, prepares glass fine powder after sieving;
(4), after the fire resistant infilling that mass ratio is 0~5:20 being mixed homogeneously with the glass fine powder of step (3) gained, it is seal powder;
(5) joining in organic solvent by the seal powder that step (4) obtains, the solid-state mass fraction 65~90% of described seal powder, by above two material mix homogeneously。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described fire resistant infilling is one or more in fused silica powder, cordierite, tungsten wire array, beta-eucryptite。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, the maximum particle diameter of described fire resistant infilling is less than 25um, and the median particle diameter of described fire resistant infilling is 10um。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described organic solvent includes solvent, adhesive, plasticizer, suspending agent, lubricant and defoamer。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, the volatilization of described solvent, adhesive, plasticizer, suspending agent, lubricant and defoamer and decomposition temperature are below the firing temperature of described seal powder, and do not react with described seal powder。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described solvent is terpineol and/or tributyl citrate (wt%): 75~90%。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described adhesive is ethyl cellulose (wt%): 5~10%。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described plasticizer is Polyethylene Glycol and/or dibutyl phthalate (wt%): 5~15%。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described suspending agent is OP-10 (wt%): 1~5%。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described lubricant is Oleum Ricini (wt%): 0~2%。
Further, in the preparation method of above-mentioned low-temperature lead-free packaging electric slurry, described defoamer is ether (wt%): 0~2%。
Further, the purpose of the present invention can also be achieved through the following technical solutions。
By a kind of low-temperature lead-free packaging electric slurry, described low-temperature lead-free packaging electric slurry is to be prepared by above-mentioned preparation method, and the melting temperature sealing of described low-temperature lead-free packaging electric slurry is between 400~600 DEG C, and the coefficient of expansion is 50~115 × 10-7/℃。
Further, the purpose of the present invention can also be achieved through the following technical solutions。
By a kind of glass sealing method, being uniformly coated with above-mentioned low-temperature lead-free packaging electric slurry by the surface of sealing-in substrate, by heating and heat preservation process, under 400 DEG C~600 DEG C temperature conditions, carry out sealing by fusing 20~60min, then lower the temperature。
Further, above-mentioned glass sealing method, described include extrusion molding or method for printing screen molding in the method being uniformly coated with by the surface of sealing-in substrate。
Further, above-mentioned glass sealing method, described heating and heat preservation process includes: tentatively heat up: through 15~30 minutes, be warming up to 150~200 DEG C, constant temperature 10~30 minutes;Again heat up: be continuously heating to 300~350 DEG C through 10~20 minutes, constant temperature 10~30 minutes。
By technique scheme, the preparation method of a kind of low-temperature lead-free packaging electric slurry that the present invention proposes at least has the advantage that
The electric slurry melting temperature sealing prepared by the preparation method of low-temperature lead-free packaging electric slurry disclosed in this invention is between 400~600 DEG C, and the coefficient of expansion is 50~115 × 10-7/ DEG C between adjustable。
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention, and can be practiced according to the content of description, illustrate as rear with presently preferred embodiments of the present invention below。
Accompanying drawing explanation
Fig. 1 is the DSC curve of the seal powder in embodiment 1 to embodiment 4;
Fig. 2 is the thermal coefficient of expansion curve of electric slurry in embodiment 1 to embodiment 4。
Detailed description of the invention
For further setting forth that the present invention reaches technological means and effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, the preparation method to a kind of low-temperature lead-free packaging electric slurry proposed according to the present invention, describe in detail as after。
The preparation method of a kind of low-temperature lead-free packaging electric slurry provided by the invention, comprises the following steps:
(1) raw material that quality share is following ratio is weighed: Bi2O350.0~96.0, ZnO2.0~20.0, B2O32.0~30.0, CuO0~2.0, Cr2O30~3.0, SrO0~2.0, BaO0~3.0, mix homogeneously;
(2) under 900~1200 DEG C of temperature conditions, insulation is fused into vitreous humour in 1~2 hour, is poured on by vitreous humour on preheated corrosion resistant plate, and tabletting prepares sheet glass;
(3) sheet glass step (2) obtained is levigate, prepares glass fine powder after sieving;
(4), after the fire resistant infilling that mass ratio is 0~5:20 being mixed homogeneously with the glass fine powder of step (3) gained, it is seal powder;
(5) seal powder that step (4) obtains is joined in organic solvent, mix homogeneously。
Wherein: described fire resistant infilling is one or more in fused silica powder, cordierite, tungsten wire array, beta-eucryptite。
When being embodied as, the maximum particle diameter of described fire resistant infilling is less than 25um, and the median particle diameter of described fire resistant infilling is 10um。
When being embodied as, described organic solvent includes solvent, adhesive, plasticizer, suspending agent, lubricant and defoamer。
When being embodied as, described organic solvent adopts consisting of: terpineol (50~75%), tributyl citrate (15~25%), ethyl cellulose (5~10%), dibutyl phthalate (5~10%), Polyethylene Glycol (0~5%) OP-10 (1~3%), Oleum Ricini 0~2%, ether 0~2%。
When being embodied as, the low-temperature lead-free packaging electric slurry prepared is loaded and seals preservation in container。
The preparation method that another embodiment of the present invention proposes a kind of low-temperature lead-free packaging electric slurry, the volatilization of described solvent, adhesive, plasticizer, suspending agent, lubricant and defoamer and decomposition temperature are below the firing temperature of described seal powder, and do not react with described seal powder。It is thus possible to make described electric slurry in seal glass process, before arriving melting temperature sealing, described organic solvent all volatilizees, not only without influence on the composition of seal powder, it is often more important that will not have the residual of described organic solvent in the seal glass that sealing-in completes。
When being embodied as, described solvent is terpineol and/or tributyl citrate;
When being embodied as, described adhesive is ethyl cellulose;
When being embodied as, described plasticizer is Polyethylene Glycol and/or dibutyl phthalate;
When being embodied as, described suspending agent is OP-10;
When being embodied as, described lubricant is Oleum Ricini;
When being embodied as, described defoamer is ether。
Another embodiment of the present invention proposes a kind of low-temperature lead-free packaging electric slurry, described low-temperature lead-free packaging electric slurry is to be prepared by the preparation method in above-described embodiment, the melting temperature sealing of described low-temperature lead-free packaging electric slurry is between 400~600 DEG C, and the coefficient of expansion is 50~115 × 10-7/℃。
The coefficient of expansion of the low-temperature lead-free packaging electric slurry prepared by the described preparation method in the above embodiment of the present invention can be calculated by below equation:
In formula:
α1With α2The thermal coefficient of expansion of glass dust and fire resistant infilling
K1With K2Bulk modulus, if the Poisson's ratio of each component is same, then available young's modulus substituted volume modulus
ρ1And ρ2Density
F1With F2The weight fraction of glass dust and fire resistant infilling
Another embodiment of the present invention proposes a kind of glass sealing method, at the low-temperature lead-free packaging electric slurry being uniformly coated with by the surface of sealing-in substrate in above-described embodiment, by heating and heat preservation process, under 400 DEG C~600 DEG C temperature conditions, carry out sealing by fusing 20~60min, then lower the temperature。
When being embodied as, described include extrusion molding or method for printing screen molding in the method being uniformly coated with by the surface of sealing-in substrate。
When being embodied as, described heating and heat preservation process includes: heats up for the first time: room temperature (25 DEG C), through 15~30 minutes, is warming up to 150~200 DEG C, constant temperature 10~30 minutes, dry out solvent;Again heat up: be continuously heating to 300~350 DEG C through 10~20 minutes, constant temperature 10~30 minutes, make binder decomposed volatilize。
Embodiment 1
Prepared by step 1 seal powder: in 100g, according to the weight ratio shown in table 1, weighs the raw material of respective numbers, is sufficiently mixed uniformly;The raw material mixed is put in corundum crucible, in 900 DEG C of high-temperature electric resistance furnaces, be incubated 2h fusing, vitreous humour is poured on preheated corrosion resistant plate (100~200 DEG C), tabletting;Put into (material: ball=1.5:1), instill 5~10 ethanol such that it is able to make the abrading-ball in described ball grinder more disperse in the ball grinder cleaned up, sheet glass is made not stick on ball grinder and abrading-ball, take out after 2 hours, cross 500 mesh sieves, put into sealing bag standby。
Prepared by step 2 organic solvent: prepare a clean beaker, according to terpineol 70%, tributyl citrate 15%, ethyl cellulose 10%, dibutyl phthalate 5%, OP-101.5%, Oleum Ricini 1.0%, ether 0.5% weight ratio, it is positioned in the water bath with thermostatic control of 80 DEG C, until solids is fully dissolved。
Prepared by step 3 electric slurry: be 85:15 according to solid-liquid weight ratio, weighs glass dust, adds organic solution, stirring, mix homogeneously。
With method for printing screen, the slurry of mix homogeneously is coated on substrate surface;According to temperature below system sealing by fusing:
Embodiment 2
According to the weight ratio shown in table 1, with reference to the preparation process of embodiment 1, prepare low-temperature lead-free packaging electric slurry。Compared with embodiment 1, it is distinctive in that, in step 1, glass smelting temperature is 1200 DEG C of insulation 1h, and according to the ratio of 100:15, mixes cordierite filler in milled glass dust, is sufficiently mixed uniformly。
In the present embodiment, being mixed by cordierite refractory filler in the glass fine powder of milled, mix homogeneously can be standby。Fire resistant infilling can't carry out secondary grinding together with glass dust, and fire resistant infilling is meticulous may result in secondary fusion in sealing-in process, loses the function regulating the coefficient of expansion。
With method for printing screen, the slurry of mix homogeneously is coated on substrate surface;According to temperature below system sealing by fusing:
Embodiment 3
According to the weight ratio shown in table 1, the program with reference to embodiment 1 prepares low-temperature lead-free packaging electric slurry。Compared with embodiment 1, it is distinctive in that, in step 1, glass smelting temperature is 1000 DEG C of insulation 1.5h;Cordierite filler is mixed with the ratio of 100:10。
With method for printing screen, mixed slurry is coated on substrate surface, after slurry levelling, according to temperature below system sealing by fusing:
Embodiment 4
According to the weight ratio shown in table 1, the program with reference to embodiment 1 prepares low-temperature lead-free packaging electric slurry。Compared with embodiment 1, it is distinctive in that, in step 1, glass melting temperature is 1200 DEG C of insulation 1h;Beta-eucryptite filler is mixed with the ratio of 100:5。In step 2, consisting of of organic solvent: terpineol 75%, tributyl citrate 15%, ethyl cellulose 5%, dibutyl phthalate 5%, OP-102.5%, Oleum Ricini 0.5%, ether 1.0% weight ratio, it is positioned in the water bath with thermostatic control of 80 DEG C, until solids is fully dissolved。
With glue rifle, slurry is coated with and on base material, according to temperature below program sealing by fusing:
Embodiment 5
According to the weight ratio shown in table 1, the program with reference to embodiment 1 prepares low-temperature lead-free packaging electric slurry。Compared with embodiment 1, it is distinctive in that, in step 1, glass melting temperature is 1200 DEG C of insulation 1h;Fused silica powder filler is mixed with the ratio of 100:7。In step 2, the composition of organic solvent is identical with embodiment 4。
With glue rifle, slurry is coated with and on base material, according to temperature below program sealing by fusing:
Table 1: low-temperature lead-free packaging electric slurry prepares raw material (wt%) and performance parameter
Transition temperature is the inherent feature temperature of glass, by forming decision。If being only glass fine powder, the height of this temperature directly determines sealing temperature。In the present invention, described transition temperature by differential scanning calorimetry (differentialscanningcalorimetry) measurement, embodiment 1 to the glass fine powder of embodiment 5 transition temperature as shown in Figure 1。General, the liquidization and flow temperature of sealing temperature and glass dust, in the present invention, owing to adding fire resistant infilling, can cause certain impact to sealing temperature。Influence degree depends primarily on the size of addition, and addition affects little at least, meanwhile, also relevant with the kind of fire resistant infilling。。
The above, it it is only presently preferred embodiments of the present invention, not the present invention is done any pro forma restriction, according to any simple modification, equivalent variations and modification that above example is made by the technical spirit of the present invention, all still falls within the scope of technical solution of the present invention。
Claims (10)
1. the preparation method of a low-temperature lead-free packaging electric slurry, it is characterised in that comprise the following steps:
(1) raw material that quality share is following ratio is weighed: Bi2O350.0~96.0, ZnO2.0~20.0, B2O32.0~30.0, CuO0~2.0, Cr2O30~3.0, SrO0~2.0, BaO0~3.0, mix homogeneously;
(2) being incubated fusing in 1~2 hour under 900~1200 DEG C of temperature conditions and form vitreous humour, be poured on by vitreous humour on preheated corrosion resistant plate, tabletting prepares sheet glass;
(3) sheet glass step (2) obtained is levigate, prepares glass fine powder after sieving;
(4), after the fire resistant infilling that mass ratio is 0~5:20 being mixed homogeneously with the glass fine powder of step (3) gained, it is seal powder;
(5) joining in organic solvent by the seal powder that step (4) obtains, the solid-state mass fraction 65~90% of described seal powder, by above two material mix homogeneously。
2. the preparation method of low-temperature lead-free packaging electric slurry according to claim 1, it is characterised in that
Described fire resistant infilling is one or more in fused silica powder, cordierite, tungsten wire array, beta-eucryptite。
3. the preparation method of low-temperature lead-free packaging electric slurry according to claim 1 and 2, it is characterised in that
The maximum particle diameter of described fire resistant infilling is less than 25um, and the median particle diameter of described fire resistant infilling is 10um。
4. the preparation method of low-temperature lead-free packaging electric slurry according to claim 1, it is characterised in that
Described organic solvent includes solvent, adhesive, plasticizer, suspending agent, lubricant and defoamer。
5. the preparation method of low-temperature lead-free packaging electric slurry according to claim 4, it is characterised in that
The volatilization of described solvent, adhesive, plasticizer, suspending agent, lubricant and defoamer and decomposition temperature are below the firing temperature of described seal powder, and do not react with described seal powder。
6. the preparation method of the low-temperature lead-free packaging electric slurry according to claim 4 or 5, it is characterised in that
Described solvent is terpineol and/or tributyl citrate (wt%): 75~90%;
Described adhesive is ethyl cellulose (wt%): 5~10%;
Described plasticizer is Polyethylene Glycol and/or dibutyl phthalate (wt%): 5~15%;
Described suspending agent is OP-10 (wt%): 1~5%;
Described lubricant is Oleum Ricini (wt%): 0~2%;
Described defoamer is ether (wt%): 0~2%。
7. a low-temperature lead-free packaging electric slurry, it is characterized in that, prepared by the described preparation method that described low-temperature lead-free packaging electric slurry is any one of claim 1 to 6, the melting temperature sealing of described low-temperature lead-free packaging electric slurry is between 400~600 DEG C, and the coefficient of expansion is 50~115 × 10-7/℃。
8. a glass sealing method, it is characterized in that, being uniformly coated with the low-temperature lead-free packaging electric slurry described in claim 7 by the surface of sealing-in substrate, by heating and heat preservation process, under 400 DEG C~600 DEG C temperature conditions, carry out sealing by fusing 20~60min, then lower the temperature。
9. glass sealing method according to claim 8, it is characterised in that
Described include extrusion molding or method for printing screen molding in the method being uniformly coated with by the surface of sealing-in substrate。
10. glass sealing method according to claim 8 or claim 9, it is characterised in that
Described heating and heat preservation process includes: tentatively heat up: through 15~30 minutes, be warming up to 150~200 DEG C, constant temperature 10~30 minutes;Again heat up: be continuously heating to 300~350 DEG C through 10~20 minutes, constant temperature 10~30 minutes。
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CN108046605A (en) * | 2017-12-26 | 2018-05-18 | 中国建筑材料科学研究总院有限公司 | bismuth zinc boron glass manufacturing method |
CN110357614A (en) * | 2019-07-25 | 2019-10-22 | 哈尔滨理工大学 | A kind of room temperature para-electric-adjustable ceramic material of ferroelectricity and preparation method thereof |
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Application publication date: 20160622 |