Silver particles manufacturing method

10478898 ยท 2019-11-19

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Inventors

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International classification

Abstract

A silver particles manufacturing method comprises following steps: providing a silver containing compound; providing an organic solution; adding the silver containing compound into the organic solution, to perform ultrasonic vibrations or a heating process until the silver containing compound is dissolved completely into the organic solution, to form a silver ion solution; performing the ultrasonic vibrations or the heating process, and then let the solution settle down for a period, to form a silver particles synthesized solution; and placing the silver particles synthesized solution into a centrifuge to perform centrifugation and separation, to obtain m-scale silver particles and nm-scale silver particles. The silver particles manufacturing method has the advantages of low pollution, low cost, high yield, and mass production.

Claims

1. A silver particles manufacturing method, comprising following steps: providing a silver nitrate (AgNO.sub.3); providing a N-Methyl Pyrrolidone (NMP) solution; adding the silver nitrate (AgNO.sub.3) into the N-Methyl Pyrrolidone (NMP) solution, to perform ultrasonic vibrations until the silver containing compound is dissolved completely into the organic solution, to form a silver ion solution, wherein silver ion concentration of the silver ion solution is 0.001M to 10M; performing the ultrasonic vibrations without additional reducing agent for 2 to 5 hours, and then let the solution settle down for a period, to form a silver particles synthesized solution; and placing the silver particles synthesized solution into a centrifuge to perform centrifugation and separation, to obtain m-scale silver particles and nm-scale silver particles, wherein power of the ultrasonic vibrations is 10 W to 1600 W.

2. The silver particles manufacturing method as claimed in claim 1, wherein rotation speed of the centrifuge is in a range of 100 rpm to 15000 rpm.

3. A silver particles manufacturing method, comprising following steps: providing a silver nitrate (AgNO.sub.3); providing a N-Methyl Pyrrolidone (NMP) solution; adding the silver nitrate (AgNO.sub.3) into the N-Methyl Pyrrolidone (NMP) solution, to perform ultrasonic vibrations until the silver containing compound is dissolved completely into the organic solution, to form a silver ion solution; providing a polymer additive for raising yield of the silver particles; putting the polymer additive into the silver ion solution, to form a silver ion solution containing polymer, wherein silver ion concentration of the silver ion solution is 0.001M to 10M; performing the ultrasonic vibrations for the silver ion solution containing polymer without additional reducing agent for 2 to 5 hours, and then let it settle down for a period, to form a silver particles synthesized solution; and placing the silver particles synthesized solution into a centrifuge to perform centrifugation and separation, to obtain m-scale particles and nm-scale particles, wherein power of the ultrasonic vibrations is 10 W to 1600 W.

4. The silver particles manufacturing method as claimed in claim 3, wherein the polymer additive is selected from one of following group consisting of: Polyethylene Terephthalate (PET), Poly (Methyl Methacrylate) (PMMA), Polyvinylidene Fluoride (PVDF), Polyvinyl Alcohol (PVA), Carboxymethyl Cellulose (CMC), Polyamide (PA), Polycarbonate (PC), Polyethylene (PE), Polypropylene (PP), Polystyrene (PS), Polyurethanes (PU), and any combinations of the above.

5. The silver particles manufacturing method as claimed in claim 3, wherein concentration of the polymer additive is 1 wt % to 3 wt %.

6. The silver particles manufacturing method as claimed in claim 3, wherein rotation speed of the centrifuge is in a range of 100 rpm to 15000 rpm.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) The related drawings in connection with the detailed descriptions of the present invention to be made later are described briefly as follows, in which:

(2) FIG. 1 is a flowchart of the steps of a silver particles manufacturing method according to a first category embodiment of the present invention;

(3) FIG. 2 is a flowchart of the steps of a silver particles manufacturing method according to a second category embodiment of the present invention;

(4) FIG. 3 is a scanning photograph of nm-scale silver particles obtained through using an electronic microscope according to the present invention;

(5) FIG. 4 is a scanning photograph of m-scale silver particles obtained through using an electronic microscope according to the present invention;

(6) FIG. 5 is a spectrum of the silver particles manufactured according to the present invention; and

(7) FIG. 6 is an X-ray diffraction pattern of the silver particles manufactured according to the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

(8) The purpose, construction, features, functions and advantages of the present invention can be appreciated and understood more thoroughly through the following detailed description with reference to the attached drawings.

(9) Refer to FIGS. 1 to 6 respectively for a flowchart of the steps of a silver particles manufacturing method according to a first category embodiment of the present invention; a flowchart of the steps of a silver particles manufacturing method according to a second category embodiment of the present invention; a scanning photograph of nm-scale silver particles obtained through using an electronic microscope according to the present invention; a scanning photograph of m-scale silver particles obtained through using an electronic microscope according to the present invention; a spectrum of the silver particles manufactured according to the present invention; and an X-ray diffraction pattern of the silver particles manufactured according to the present invention.

(10) As shown in FIG. 1, the silver particles manufacturing method 100 includes the following steps: providing a silver containing compound (step S110); providing an organic solution (step S120); adding the silver containing compound into the organic solution, to perform ultrasonic vibrations or a heating process until the silver containing compound is dissolved completely into the organic solution, to form a silver ion solution (step S130). For the steps mentioned above, the silver containing compound is silver nitride (AgNO.sub.3) powder, the organic solution is N-Methyl Pyrrolidone (NMP) solution, while the silver ion concentration is 0.001M to 10M. But the present invention is not limited to this.

(11) Moreover, the silver particles manufacturing method includes the following steps: performing ultrasonic vibrations or a heating process for the silver ion solution, and then let the solution settle down for a period of time, to obtain a silver particles synthesized solution (step S140). In the step mentioned above, the heating temperature is 30 C. to 110 C., and the heating is performed for a period of 1 second to 10 hours. On the other hand, the power required for the ultrasonic vibrations is 10 W to 1600 W, while the ultrasonic vibrations are performed for a period of 1 second to 10 hours. Further, the settle-down period is 1 to 30 days depending on requirement. But the present invention is not limited to this.

(12) Further, the silver particles manufacturing method includes the following steps: placing the silver particles synthesized solution into a centrifuge to perform centrifugation and separation, to obtain nm-scale silver particles (upper layer solution) and m-scale silver particles (lower layer powder), then the particles are rinsed with acetone several times, to complete manufacturing the nm-scale silver particles and the m-scale silver particles (step S150). In the step mentioned above, the rotation speed of the centrifuge is 100 rpm to 15000 rpm, while the centrifugation is performed for a period of 1 second to 10 hours. But the present invention is not limited to this.

(13) Then, refer to FIG. 2 for a flowchart of the steps of a silver particles manufacturing method according to a second category embodiment of the present invention. As shown in FIG. 2, the silver particles manufacturing method 200 includes the following steps: providing a silver containing compound (step S210); providing an organic solution (step S220); adding the silver containing compound into the organic solution, to perform ultrasonic vibrations or a heating process until the silver containing compound is dissolved completely into the organic solution, to form a silver ion solution (step S230). For the steps mentioned above, the silver containing compound is silver nitride (AgNO.sub.3) powder, the organic solution is N-Methyl Pyrrolidone (NMP) solution, while the silver ion concentration is 0.001M to 10M. But the present invention is not limited to this.

(14) Moreover, the silver particles manufacturing method further includes the following steps: providing a polymer additive (step S240). The polymer additive can be selected from one of the following group consisting of: Polyethylene Terephthalate (PET), Poly (Methyl Methacrylate) (PMMA), Polyvinylidene Fluoride (PVDF), Polyvinyl Alcohol (PVA), Carboxymethyl Cellulose (CMC), Polyamide (PA), Polycarbonate (PC), Polyethylene (PE), Polypropylene (PP), Polystyrene (PS), Polyurethanes (PU), and any combinations of the above.

(15) Further, the silver particles manufacturing method includes the following steps: adding the polymer additive into the silver ion solution, and stir them to dissolve the polymer additive completely, to obtain a silver ion solution containing polymer (step S250).

(16) In addition, the silver particles manufacturing method further includes the following steps: performing ultrasonic vibrations or a heating process for the silver ion solution containing polymer, and then let the solution settle down for a period of time, to obtain a silver particles synthesized solution (step S260). In the step mentioned above, the heating temperature is 30 C. to 110 C., and the heating is performed for a period of 1 second to 10 hours. On the other hand, the power required for the ultrasonic vibrations is 10 W to 1600 W, while the ultrasonic vibration is performed for a period of 1 second to 10 hours. Further, the settle-down period is 1 to 30 days.

(17) Further, the silver particles manufacturing method includes the following steps: placing the silver particles synthesized solution into a centrifuge to perform centrifugation and separation, to obtain nm-scale silver particles (upper layer solution) and m-scale silver particles (lower layer powder). Then the particles are rinsed with acetone several times, to complete manufacturing the nm-scale silver particles and the m-scale silver particles (step S270). In the step mentioned above, the rotation speed of the centrifuge is 100 rpm to 15000 rpm, while the centrifugation is performed for a period of 1 second to 10 hours. But the present invention is not limited to this.

(18) In the following, various embodiments are described in explaining the technical characteristics of the present invention. Wherein, embodiments 1-4 and embodiments 5-8 belong to the first category embodiment; while embodiments 9-12 and embodiments 13-16 belong to the second category embodiment.

Embodiments 1-4

(19) Put silver nitride (AgNO.sub.3) powder of 15%, 20%, 30%, and 60% (w/w) respectively into 2 g N-Methyl Pyrrolidone (NMP) solution, and then perform ultrasonic vibrations to make the silver nitride (AgNO.sub.3) powder dissolve completely, to obtain the silver ion solution. Subsequently, perform heating process in a temperature of 65 C., 75 C., and 85 C. respectively for two hours for the silver ion solution thus obtained, then place the solution for settle-down period as required, to obtain the synthesized silver particles solution. In case the settle-down period is 1-5 days, then the nm-scale silver particles can be obtained. Further, in case the settle-down period is over 6 days, then the m-scale silver particles can be obtained. Finally, place the synthesized silver particles solution into a high speed centrifuge to rotate at 10000 rpm for 20 minutes, to obtain nm-scale silver particles (upper layer solution) and m-scale silver particles (lower layer powder), then rinse the particles with acetone several times, to complete manufacturing the nm-scale silver particles and the m-scale silver particles. The results of the steps mentioned above can be summarized in Table 1 as follows:

(20) TABLE-US-00001 TABLE 1 reaction temperature AgNO.sub.3 content ( C.) embodiment (w/w) 65 75 85 1 15 + + + 2 20 + + + 3 30 + + + 4 60 + + + +: indicates that silver particles can be obtained : indicates that no silver particles can be obtained

Embodiments 5-8

(21) Put silver nitride (AgNO.sub.3) powder of 15%, 20%, 30%, and 60% (w/w) respectively into 2 g N-Methyl Pyrrolidone (NMP) solution, and then perform ultrasonic vibrations to make the silver nitride (AgNO.sub.3) powder dissolve completely, to obtain the silver ion solution. Subsequently, perform ultrasonic vibrations for 2, 3, 4, 5 hours respectively for the silver ion solution thus obtained, then place the solution in a settle-down period as required, to obtain the synthesized silver particles solution. In case the settle-down period is 1-5 days, then the nm-scale silver particles can be obtained. Further, in case the settle-down period is over 6 days, then m-scale silver particles can be obtained. Finally, place the synthesized silver particles solution into a high speed centrifuge to rotate at 10000 rpm for 20 minutes, to obtain nm-scale silver particles (upper layer solution) and m-scale silver particles (lower layer powder), then rinse the particles with acetone several times, to complete manufacturing the nm-scale silver particles and the m-scale silver particles. The results of the steps mentioned above can be summarized in the Table 2. as follows.

(22) TABLE-US-00002 TABLE 2 ultrasonic vibration period AgNO.sub.3 content (hr) embodiment (w/w) 2 3 4 5 5 15 + + + + 6 20 + + + + 7 30 + + + + 8 60 + + + + +: indicates that silver particles can be obtained : indicates that silver particles can not be obtained

Embodiments 9-12

(23) Put silver nitride (AgNO.sub.3) powder of 15%, 20%, 30%, and 60% (w/w) respectively into 2 g N-Methyl Pyrrolidone (NMP) solution, and then perform ultrasonic vibrations to make the silver nitride (AgNO.sub.3) powder dissolve completely, to obtain a silver ion solution. Subsequently, add polymer additive of Poly (Methyl Methacrylate) (PMMA) or Polyethylene Terephthalate (PET) of 1 wt %, 2 wt %, and 3 wt % respectively into the silver ion solution, to obtain a silver ion solution containing polymer. Then, perform ultrasonic vibrations until the polymer is completely dissolved. Then, perform heating process in a temperature of 65 C., 75 C., and 85 C. respectively for two hours, and then place the solution in settle-down period as required, to obtain the synthesized silver particles solution. In case the settle-down period is 1-5 days, then the nm-scale silver particles can be obtained. Further, in case the settle-down period is over 6 days, then m-scale silver particles can be obtained. Finally, place the synthesized silver particles solution into a high speed centrifuge to rotate at 10000 rpm for 20 minutes, to obtain nm-scale silver particles (upper layer solution) and m-scale silver particles (lower layer powder). Then, rinse the particles with acetone several times, to complete manufacturing the nm-scale silver particles and the m-scale silver particles. The results of the steps mentioned above can be summarized in Table 3 as follows:

(24) TABLE-US-00003 TABLE 3 reaction temperature AgNO.sub.3 content polymer content ( C.) embodiment (w/w) (w/w) 65 75 85 9 15 1 + + + 2 + + + 3 + + + 10 20 1 + + + 2 + + + 3 + + + 11 30 1 + + + 2 + + + 3 + + + 12 60 1 2 3 +: indicates that silver particles can be obtained : indicates that no silver particles can be obtained

Embodiments 13-16

(25) Put silver nitride (AgNO.sub.3) powder of 15%, 20%, 30%, and 60% (w/w) respectively into 2 g N-Methyl Pyrrolidone (NMP) solution, and then perform ultrasonic vibrations to make the silver nitride (AgNO.sub.3) powder dissolve completely, to obtain a silver ion solution. Subsequently, add polymer additive of Poly (Methyl Methacrylate) (PMMA) or Polyethylene Terephthalate (PET) of 1 wt %, 2 wt %, and 3 wt % respectively into the silver ion solution, to obtain a silver ion solution containing polymer. Then, perform ultrasonic vibrations until the polymer is completely dissolved. Then, perform ultrasonic vibrations for 2, 3, 4, 5 hours respectively, then place the solution for settle-down period as required, to obtain the synthesized silver particles solution. In case the settle-down period is 1-5 days, then nm-scale silver particles can be obtained. Further, in case the settle-down period is over 6 days, then m-scale silver particles can be obtained. Finally, place the synthesized silver particles solution into a high speed centrifuge to rotate at 10000 rpm for 20 minutes, to obtain nm-scale silver particles (upper layer solution) and m-scale silver particles (lower layer powder). Then, rinse the particles with acetone several times, to complete manufacturing the nm-scale silver particles and the m-scale silver particles. The results of the steps mentioned above can be summarized in Table 4 as follows:

(26) TABLE-US-00004 TABLE 4 AgNO3 polymer ultrasonic vibration period content content (hr) embodiment (w/w) (w/w) 2 3 4 5 13 15 1 + + + + 2 + + + + 3 + + + + 14 20 1 + + + + 2 + + + + 3 + + + + 15 30 1 + + + + 2 + + + + 3 + + + + 16 60 1 2 3 +: indicates that silver particles can be obtained : indicates that silver particles can not be obtained

(27) The above detailed description of the preferred embodiment is intended to describe more clearly the characteristics and spirit of the present invention. However, the preferred embodiments disclosed above are not intended to be any restrictions to the scope of the present invention. Conversely, its purpose is to include the various changes and equivalent arrangements that are within the scope of the appended claims.