CN105127435A - Low-temperature sintering nano-silver paste and preparation process thereof - Google Patents
Low-temperature sintering nano-silver paste and preparation process thereof Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000009766 low-temperature sintering Methods 0.000 title abstract description 4
- 239000004094 surface-active agent Substances 0.000 claims abstract description 93
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 75
- 239000002245 particle Substances 0.000 claims abstract description 49
- 239000012071 phase Substances 0.000 claims abstract description 43
- 239000005416 organic matter Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010587 phase diagram Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000008346 aqueous phase Substances 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims description 65
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical group CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 58
- 239000004064 cosurfactant Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000003921 oil Substances 0.000 claims description 40
- NWGKJDSIEKMTRX-MDZDMXLPSA-N Sorbitan oleate Chemical group CCCCCCCC\C=C\CCCCCCCC(=O)OCC(O)C1OCC(O)C1O NWGKJDSIEKMTRX-MDZDMXLPSA-N 0.000 claims description 35
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 35
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 26
- 239000012153 distilled water Substances 0.000 claims description 25
- 239000003638 chemical reducing agent Substances 0.000 claims description 20
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 18
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 18
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 18
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 238000005119 centrifugation Methods 0.000 claims description 10
- 230000007928 solubilization Effects 0.000 claims description 10
- 238000005063 solubilization Methods 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002002 slurry Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 2
- 239000000969 carrier Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000006911 nucleation Effects 0.000 abstract 1
- 238000010899 nucleation Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000693 micelle Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a process for preparing low-temperature sintering nano-silver paste. The process comprises the following steps: 1) preparing blank reverse microemulsion and making a pseudoternary phase diagram; 2) preparing the reverse microemulsion containing nano-silver particles; 3) performing centrifugal separation: performing centrifugal separation on the reverse microemulsion containing the nano-silver particles 2-4 times, separating oil phase organic matter and aqueous phase solution, and obtaining the nano-silver particles adsorbed by mixed surfactants; 4) causing the nano-silver particles adsorbed by the mixed surfactants obtained in the step 3) to be mixed with organic carriers, adjusting the viscosity, and preparing the low-temperature sintering nano-silver paste. The process has the advantages that the nano-silver particles are wrapped with the surfactants from nucleation growth to the formation of final slurry, the hard aggregation of the nano-silver particles is greatly reduced, the nano-silver particles prepared through the process are controllable in size, and the preparation process is simplified.
Description
Technical field
The present invention relates to material preparation technology, specifically a kind of low temperature-sintered nano silver paste and preparation technology.
Background technology
Take carborundum as the third generation semiconductor of representative, compared with the first generation, second generation semi-conducting material, there is wider energy gap, high breakdown voltage, high thermal conductivity, the capability of resistance to radiation that high electronics is saturated and higher.These features make third generation semiconductor energy bear higher power density, but this it is also proposed higher challenge to its encapsulation, and the interconnection material of chip and substrate, as the material closest to chip, produces extremely important impact to the performance of chip performance.
Interconnection material-the solder of traditional die and substrate and conducting resinl are difficult to satisfy the demands owing to there is fatal defect.Solder is in the not high shortcoming of condition of high temperature reliability, and solder thermal stress under devices function state is comparatively large simultaneously, easily causes chip to lose efficacy because thermal coefficient of expansion does not mate; The thermal conductivity of conducting resinl is lower, is usually in 10-25W/mK, and the glass transition temperature of conducting resinl is lower, along with the growth of service time, the resin-based of conducting resinl knows from experience the situation engendering fatigue failure, and thermal resistance raises, for the heat radiation of chip and physical property totally unfavorable.In the face of the growth requirement of high power density components and parts, be badly in need of the new chip of research and development and substrate interconnect material.Low temperature-sintered nano silver paste adopts nano-Ag particles as function phase, it has the highest metallic thermal conductivity and electrical conductivity, and sintering temperature is low even can reach less than 200 DEG C, can bear high operating temperature after sintering, there is good reliability, the growth requirement of present high performance components can be met.
The preparation of nano-Ag particles and follow-up silver are starched preparation and are separated by the preparation process of current low temperature-sintered nano silver paste.Usual employing physical method or chemical method (mainly adopting liquid phase reduction) prepare nano-Ag particles, after these methods obtain pure nano-Ag particles, joined containing in the formula mixed solution such as surfactant again, viscosity is regulated to obtain silver slurry, but in this preparation process, nano-Ag particles does not have surfactant to wrap up, because nano-Ag particles has very high interfacial energy, easy generation hard aggregation, decreases the advantage of Argent grain sintering of nano-material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, and a kind of low temperature-sintered nano silver paste and preparation technology are provided.This low temperature-sintered nano silver paste can reduce the impact of impurity on low temperature-sintered nano silver paste sintering character, improves the sintering character of low temperature-sintered nano silver paste, can reduce sintering temperature simultaneously; This technique can greatly reduce the phenomenon of nano-Ag particles generation hard aggregation, and the granular size of Nano Silver prepared by this technique is controlled, can simplify preparation technology simultaneously.
The technical scheme realizing the object of the invention is:
A kind of low temperature-sintered nano silver paste preparation technology, comprises the steps:
1) blank reverse micro emulsion is prepared, do pseudoternary phase diagram: in compound surfactant, different ratios got by two kinds of surfactants, compound surfactant: the mass ratio of cosurfactant is 2:1, the gross mass of compound surfactant and cosurfactant: the organic mass ratio of oil phase is 1:1, by each for compound surfactant composition, cosurfactant and oil phase organic matter add in different colorimetric cylinders successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to two kinds of surfactant optimum quality ratio K1 in maximum water solubilization determination compound surfactant,
The compound surfactant of K1 ratio composition gets different mass ratioes from cosurfactant, the gross mass of compound surfactant and cosurfactant: the organic mass ratio of oil phase is 1:1, each for compound surfactant composition, cosurfactant are added in different colorimetric cylinders from oil phase organic matter successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to the optimum quality ratio K2 of maximum water solubilization determination compound surfactant and cosurfactant;
Compound surfactant and cosurfactant ratio are K2, wherein in compound surfactant, the mass ratio of two kinds of surfactants is K1, gross mass and the oil phase organic matter of compound surfactant and cosurfactant get different ratios, by each for compound surfactant composition, cosurfactant and oil phase organic matter add in different colorimetric cylinders successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to the surfactant in reverse micro emulsion blank during solubilising maximum amount of water, cosurfactant, oil phase organic matter, the mass ratio of distilled water, make pseudoternary phase diagram,
2) preparation is containing the reverse micro emulsion of nano-Ag particles: by silver-colored source, reducing agent replaces distilled water, according to the compound surfactant in the pseudoternary phase diagram that step 1) obtains, cosurfactant, the organic optimum proportioning of oil phase, prepare silver-colored source reverse micro emulsion respectively, reducing agent reverse micro emulsion, reducing agent reverse micro emulsion is added drop-wise in the reverse micro emulsion of silver-colored source often to drip 0.1mL, guarantee that silver-colored source is completely reduced, constantly stir in dropping process, after dropping reducing agent reverse micro emulsion completes, continue to stir half an hour, be obtained by reacting the reverse micro emulsion containing nano-Ag particles,
3) centrifugation: carry out 2-4 centrifugation to the reverse micro emulsion containing nano-Ag particles, isolate oil phase organic matter and aqueous phase solution, obtain the nano-Ag particles adsorbed by compound surfactant;
4) nano-Ag particles that the compound surfactant obtained in step 3) adsorbs is mixed with organic carrier, adjusting viscosity, obtained low temperature-sintered nano silver paste.
Described compound surfactant constituent is non-ionic surface active agent.
Described cosurfactant adopts carbon atom number to be the alcohol of 3-6.
Described oil phase organic matter adopts carbon atom number to be the alkane of 5-8.
Described organic carrier is high molecular polymer.
The advantage of this low temperature-sintered nano silver paste is: the surfactant in low temperature-sintered nano silver paste is non-ionic surface active agent (organic matter), volatilization can be decomposed during sintering, because this reducing the impact of impurity on low temperature-sintered nano silver paste sintering character, improve the sintering character of low temperature-sintered nano silver paste, nano-Ag particles can reach 10-50nm simultaneously, the surface that nano-Ag particles has or performance greatly, contribute to reducing sintering temperature.
The advantage of this technique is: nano-Ag particles grows into the final slurry of formation from forming core has surfactant to wrap up, greatly reduce the phenomenon of nano-Ag particles generation hard aggregation, and the granular size of Nano Silver prepared by this technique is controlled, simplifies preparation technology simultaneously.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the reverse micro emulsion in argentiferous source in embodiment;
Fig. 2 is the schematic diagram containing the reverse micro emulsion of reducing agent in embodiment;
Fig. 3 is the schematic diagram that in embodiment, silver-colored source and reducing agent two kinds of materials react under compound surfactant/cosurfactant wraps up;
Fig. 4 is the schematic diagram that in embodiment, silver-colored source and reducing agent generate nano particle after reacting;
Fig. 5 be in embodiment containing nano-Ag particles microemulsion centrifugal after schematic diagram;
Fig. 6 is the schematic diagram of embodiment low temperature sintering nanometer silver paste.
In figure, 1 is sorbester p17 and triton x-100, and 2 is n-hexyl alcohol, and 3 is normal heptane, and 4 is PVP(polyvinylpyrrolidone), A is silver nitrate, and B is hydrazine hydrate, and C is nano-Ag particles.
Detailed description of the invention
Below in conjunction with drawings and Examples, content of the present invention is further elaborated, but is not limitation of the invention.
A kind of low temperature-sintered nano silver paste preparation technology, comprises the steps:
1) blank reverse micro emulsion is prepared, do pseudoternary phase diagram: in compound surfactant, different ratios got by two kinds of surfactants, compound surfactant: the mass ratio of cosurfactant is 2:1, the gross mass of compound surfactant and cosurfactant: the organic mass ratio of oil phase is 1:1, by each for compound surfactant composition, cosurfactant and oil phase organic matter add in different colorimetric cylinders successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to two kinds of surfactant optimum quality ratio K1 in maximum water solubilization determination compound surfactant,
The compound surfactant of K1 ratio composition gets different mass ratioes from cosurfactant, the gross mass of compound surfactant and cosurfactant: the organic mass ratio of oil phase is 1:1, each for compound surfactant composition, cosurfactant are added in different colorimetric cylinders from oil phase organic matter successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to the optimum quality ratio K2 of maximum water solubilization determination compound surfactant and cosurfactant;
Compound surfactant and cosurfactant ratio are K2, wherein in compound surfactant, the mass ratio of two kinds of surfactants is K1, gross mass and the oil phase organic matter of composite surfactant and cosurfactant get different ratios, by each for compound surfactant composition, cosurfactant and oil phase organic matter add in different colorimetric cylinders successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to the surfactant in reverse micro emulsion blank during solubilising maximum amount of water, cosurfactant, oil phase organic matter, the mass ratio of distilled water, make pseudoternary phase diagram,
2) preparation is containing the reverse micro emulsion of nano-Ag particles: by silver-colored source, reducing agent replaces distilled water, according to the compound surfactant in the pseudoternary phase diagram that step 1) obtains, cosurfactant, the organic optimum proportioning of oil phase, prepare silver-colored source reverse micro emulsion respectively, reducing agent reverse micro emulsion, reducing agent reverse micro emulsion is added drop-wise in the reverse micro emulsion of silver-colored source often to drip 0.1mL, guarantee that silver-colored source is completely reduced, constantly stir in dropping process, after dropping reducing agent reverse micro emulsion completes, continue to stir half an hour, be obtained by reacting the reverse micro emulsion containing nano-Ag particles,
3) centrifugation: carry out 2-4 centrifugation to the reverse micro emulsion containing nano-Ag particles, isolate oil phase organic matter and aqueous phase solution, obtain the nano-Ag particles adsorbed by compound surfactant;
4) nano-Ag particles that the compound surfactant obtained in step 3) adsorbs is mixed with organic carrier, adjusting viscosity, obtained low temperature-sintered nano silver paste.
Described compound surfactant constituent is non-ionic surface active agent, and this routine compound surfactant consists of sorbester p17, triton x-100.
Described cosurfactant adopts carbon atom number to be the alcohol of 3-6, and this example is n-hexyl alcohol.
Described oil phase organic matter adopts carbon atom number to be the alkane of 5-8, and this example is normal heptane.
Described organic carrier is high molecular polymer, and this example is PVP.
Silver source is silver nitrate, and reducing agent is hydrazine hydrate.
Embodiment:
A preparation technology for low temperature-sintered nano silver paste, comprises the steps:
1) prepare blank reverse micro emulsion, do pseudoternary phase diagram:
Sorbester p17: triton x-100 gets different mass ratio 3:7,1:4,1:5,1:6,1:7,1:8, sorbester p17 and triton x-100 1: the mass ratio of n-hexyl alcohol 2 is 2:1, the gross mass of sorbester p17, triton x-100 and n-hexyl alcohol 2: the mass ratio of normal heptane 3 is 1:1, sorbester p17, triton x-100, n-hexyl alcohol 2 are added in each colorimetric cylinder with normal heptane 3 by corresponding proportion successively, under 30 DEG C of conditions, dripping distilled water while stirring prepare blank reverse micro emulsion, is 1:5 according to maximum water solubilization determination sorbester p17 and triton x-100 1 optimum quality ratio K1;
Sorbester p17: the mass ratio of triton x-100 is that the compound surfactant of 1:5 composition is got different quality with n-hexyl alcohol 2 and compared 3:1,2:1,1:1,1:2, the gross mass of sorbester p17, triton x-100 and n-hexyl alcohol 2: the mass ratio of normal heptane 3 is 1:1, sorbester p17, triton x-100, n-hexyl alcohol 2 are added in each colorimetric cylinder with normal heptane 3 by corresponding proportion successively, under 30 DEG C of conditions, dripping distilled water while stirring prepare blank reverse micro emulsion, is 2:1 according to maximum water solubilization determination sorbester p17 and triton x-100 1 with n-hexyl alcohol 2 optimum quality ratio K2, sorbester p17 and triton x-100 1: n-hexyl alcohol 2 mass ratio K2 is 2:1, wherein sorbester p17: triton x-100 is optimum quality ratio K1 is 1:5, sorbester p17, the gross mass of triton x-100 and n-hexyl alcohol 2: the mass ratio of oil phase organic matter normal heptane 3 is 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1, by sorbester p17, triton x-100, n-hexyl alcohol 2 and normal heptane 3 add in each colorimetric cylinder by corresponding proportion successively, under 30 DEG C of conditions, drip distilled water while stirring prepare blank reverse micro emulsion, according to the surfactant in reverse micro emulsion blank during solubilising maximum amount of water, cosurfactant, oil phase organic matter, the mass ratio of distilled water, make pseudoternary phase diagram,
2) preparation is containing the reverse micro emulsion of nano-Ag particles: by silver-colored source silver nitrate solution A, reducing agent hydrazine hydrate B solution replaces distilled water, be 32wt% according to the compound surfactant sorbester p17 of optimum proportioning in the pseudoternary phase diagram that step 1) obtains and triton x-100 1, cosurfactant n-hexyl alcohol 2 is 16wt%, oil phase organic matter normal heptane 3 is 32wt%, prepare silver nitrate A reverse micro emulsion respectively, hydrazine hydrate B reverse micro emulsion, obtain the silver nitrate A reverse micro emulsion that content is 15wt%, obtain the hydrazine hydrate B reverse micro emulsion that content is 15wt%, as Fig. 1, shown in Fig. 2, compound surfactant sorbester p17 is connected with oil phase organic matter with the lipophilic group outwardly of the micelle that triton x-100 1 forms with cosurfactant n-hexyl alcohol 2, hydrophilic group and silver nitrate A inwardly, hydrazine hydrate B is connected, thus silver nitrate A, hydrazine hydrate B is wrapped in micelle, hydrazine hydrate B reverse micro emulsion is added drop-wise in silver nitrate A reverse micro emulsion often to drip 0.1mL, as shown in Figure 3, in the process dripping hydrazine hydrate B, under the effect of stirring, compound surfactant sorbester p17 and triton x-100 1 are constantly opened with closed with the micelle that cosurfactant n-hexyl alcohol 2 forms, in opening procedure, there is phase hybrid reaction and generate nano-Ag particles C in silver nitrate A and hydrazine hydrate B, guarantee that silver nitrate A is completely reduced, constantly stir in dropping process, after dropping hydrazine hydrate B reverse micro emulsion completes, continue to stir half an hour, be obtained by reacting the reverse micro emulsion containing nano-Ag particles C, as shown in Figure 4, nano-Ag particles C or hydrazine hydrate B is wrapped in the micelle that compound surfactant sorbester p17 and triton x-100 1 and cosurfactant n-hexyl alcohol 2 form,
3) centrifugation: carry out 2-4 centrifugation to the reverse micro emulsion containing nano-Ag particles C, isolate oil phase organic matter and aqueous phase solution, obtain the nano-Ag particles C adsorbed by compound surfactant, as shown in Figure 5, separating most normal heptane 3, part n-hexyl alcohol 2, part sorbester p17 and triton x-100 1, hydrazine hydrate B and react the water generated, obtain the nano-Ag particles adsorbed by compound surfactant;
4) the nano-Ag particles C that the compound surfactant obtained in step 3) adsorbs is mixed with organic carrier PVP4, adjusting viscosity, obtained low temperature-sintered nano silver paste, as shown in Figure 6, organic carrier PVP4 backbone connects each compound surfactant, wherein compound surfactant absorption nano-Ag particles C.
Claims (6)
1. a low temperature-sintered nano silver paste preparation technology, comprises the steps:
1) blank reverse micro emulsion is prepared, do pseudoternary phase diagram: in compound surfactant, different ratios got by two kinds of surfactants, compound surfactant: the mass ratio of cosurfactant is 2:1, the gross mass of compound surfactant and cosurfactant: the organic mass ratio of oil phase is 1:1, by each for compound surfactant composition, cosurfactant and oil phase organic matter add in different colorimetric cylinders successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to two kinds of surfactant optimum quality ratio K1 in maximum water solubilization determination compound surfactant,
The compound surfactant of K1 ratio composition gets different mass ratioes from cosurfactant, composite surface-active agent and the gross mass of cosurfactant: the organic mass ratio of oil phase is 1:1, each for compound surfactant composition, cosurfactant are added in different colorimetric cylinders from oil phase organic matter successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to the optimum quality ratio K2 of maximum water solubilization determination compound surfactant and cosurfactant;
Compound surfactant and cosurfactant ratio are K2, wherein in compound surfactant, the mass ratio of two kinds of surfactants is K1, gross mass and the oil phase organic matter of compound surfactant and cosurfactant get different ratios, by each for compound surfactant composition, cosurfactant and oil phase organic matter add in different colorimetric cylinders successively, drip distilled water at a constant temperature while stirring and prepare blank reverse micro emulsion, according to the surfactant in reverse micro emulsion blank during solubilising maximum amount of water, cosurfactant, oil phase organic matter, the mass ratio of distilled water, make pseudoternary phase diagram,
2) preparation is containing the reverse micro emulsion of nano-Ag particles: by silver-colored source, reducing agent replaces distilled water, according to the compound surfactant in the pseudoternary phase diagram that step 1) obtains, cosurfactant, the organic optimum proportioning of oil phase, prepare silver-colored source reverse micro emulsion respectively, the reverse micro emulsion of reducing agent, reducing agent reverse micro emulsion is added drop-wise in the reverse micro emulsion of silver-colored source often to drip 0.1mL, guarantee that silver-colored source is completely reduced, constantly stir in dropping process, after dropping reducing agent reverse micro emulsion completes, continue to stir half an hour, be obtained by reacting the reverse micro emulsion containing nano-Ag particles,
3) centrifugation: carry out 2-4 centrifugation to the reverse micro emulsion containing nano-Ag particles, isolate oil phase organic matter and aqueous phase solution, obtain the nano-Ag particles adsorbed by compound surfactant;
4) nano-Ag particles that the compound surfactant obtained in step 3) adsorbs is mixed with organic carrier, adjusting viscosity, obtained low temperature-sintered nano silver paste.
2. low temperature-sintered nano silver paste preparation technology according to claim 1, is characterized in that, described compound surfactant constituent is non-ionic surface active agent; Described cosurfactant adopts carbon atom number to be the alcohol of 3-6; Described oil phase organic matter adopts carbon atom number to be the alkane of 5-8; Described organic carrier is high molecular polymer.
3. low temperature-sintered nano silver paste preparation technology according to claim 2, is characterized in that, described non-ionic surface active agent is sorbester p17 and triton x-100; Described cosurfactant is n-hexyl alcohol; Described oil phase organic matter is normal heptane; Described organic carrier is PVP.
4. low temperature-sintered nano silver paste preparation technology according to claim 1, is characterized in that, described silver-colored source is silver nitrate, and reducing agent is hydrazine hydrate.
5. low temperature-sintered nano silver paste preparation technology according to claim 1, is characterized in that, comprise the steps:
1) prepare blank reverse micro emulsion, do pseudoternary phase diagram:
Sorbester p17: triton x-100 gets different mass ratio 3:7,1:4,1:5,1:6,1:7,1:8, sorbester p17 and triton x-100: the mass ratio of n-hexyl alcohol is 2:1, the gross mass of sorbester p17, triton x-100 and n-hexyl alcohol: the mass ratio of normal heptane 3 is 1:1, sorbester p17, triton x-100, n-hexyl alcohol and normal heptane are added in each colorimetric cylinder by corresponding proportion successively, under 30 DEG C of conditions, dripping distilled water while stirring prepare blank reverse micro emulsion, is 1:5 according to maximum water solubilization determination sorbester p17 and triton x-100 optimum quality ratio K1;
Sorbester p17: the mass ratio of triton x-100 is that the compound surfactant of 1:5 composition is got different quality with n-hexyl alcohol and compared 3:1,2:1,1:1,1:2, the gross mass of sorbester p17, triton x-100 and n-hexyl alcohol: the mass ratio of normal heptane is 1:1, sorbester p17, triton x-100, n-hexyl alcohol and normal heptane are added in each colorimetric cylinder by corresponding proportion successively, under 30 DEG C of conditions, dripping distilled water while stirring prepare blank reverse micro emulsion, is 2:1 according to maximum water solubilization determination sorbester p17 and triton x-100 1 with n-hexyl alcohol 2 optimum quality ratio K2;
Sorbester p17 and triton x-100: n-hexyl alcohol mass ratio K2 is 2:1, wherein sorbester p17: triton x-100 is optimum quality ratio K1 is 1:5, sorbester p17, the gross mass of triton x-100 and n-hexyl alcohol 2: the mass ratio of oil phase organic matter normal heptane is 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1, by sorbester p17, triton x-100, n-hexyl alcohol and normal heptane add in each colorimetric cylinder by corresponding proportion successively, under 30 DEG C of conditions, drip distilled water while stirring prepare blank reverse micro emulsion, according to the surfactant in reverse micro emulsion blank during solubilising maximum amount of water, cosurfactant, oil phase organic matter, the mass ratio of distilled water, make pseudoternary phase diagram,
2) preparation is containing the reverse micro emulsion of nano-Ag particles: silver-colored source liquor argenti nitratis ophthalmicus, reducing agent hydrazine hydrate solution are replaced distilled water, according to the compound surfactant sorbester p17 of optimum proportioning in the pseudoternary phase diagram that step 1) obtains and triton x-100 be 32wt%, cosurfactant n-hexyl alcohol is 16wt%, oil phase organic matter normal heptane is 32wt%, prepare silver nitrate reverse micro emulsion, hydrazine hydrate reverse micro emulsion respectively, obtain silver nitrate reverse micro emulsion that content is 15wt%, obtain the hydrazine hydrate reverse micro emulsion that content is 15wt%; Hydrazine hydrate reverse micro emulsion is added drop-wise in silver nitrate reverse micro emulsion often to drip 0.1mL, guarantee that silver nitrate is completely reduced, constantly stir in dropping process, after dropping reducing agent reverse micro emulsion completes, continue to stir half an hour, be obtained by reacting the reverse micro emulsion containing nano-Ag particles;
3) centrifugation: the reverse micro emulsion containing nano-Ag particles carries out 2-4 centrifugation, isolates oil phase organic matter and aqueous phase solution, obtains the nano-Ag particles adsorbed by compound surfactant;
4) nano-Ag particles that the compound surfactant obtained in step 3) adsorbs is mixed with organic carrier PVP, adjusting viscosity, obtained low temperature-sintered nano silver paste.
6. the low temperature-sintered nano silver paste that the low temperature-sintered nano silver paste preparation technology according to any one of claim 1-5 obtains.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510614853.9A CN105127435B (en) | 2015-09-24 | 2015-09-24 | A kind of low temperature-sintered nano silver paste and preparation technology |
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| CN107570912A (en) * | 2017-08-30 | 2018-01-12 | 桂林电子科技大学 | A kind of preparation method of the nano mattisolda with high wettability energy |
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Application publication date: 20151209 Assignee: Guilin Xinyi Semiconductor Technology Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980046246 Denomination of invention: A low-temperature sintered nano silver slurry and its preparation process Granted publication date: 20170623 License type: Common License Record date: 20231108 |
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