CN104174858A - Preparation method of silver powder or doped silver powder - Google Patents
Preparation method of silver powder or doped silver powder Download PDFInfo
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- CN104174858A CN104174858A CN201310201833.XA CN201310201833A CN104174858A CN 104174858 A CN104174858 A CN 104174858A CN 201310201833 A CN201310201833 A CN 201310201833A CN 104174858 A CN104174858 A CN 104174858A
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Abstract
The invention discloses a preparation method of silver powder or doped silver powder. The preparation method comprises the steps of firstly, preparing silver salt solution, and then carrying out ultrasonic atomization on the silver salt solution to obtain atomized matter, wherein the ultrasonic atomization power is 0.2-10kw, the ultrasonic atomization frequency is 1.7-2.4MHz, and the atomization speed is 0.5-500kg/ h; mixing the atomized matter with carrier airflow, carrying out thermal decomposition, and collecting to obtain the silver powder or doped silver powder, wherein the silver salt solution has the silver ion molar concentration of 0.0001-4mol/ L or contains doped metal ions, and microwave heating is preferentially adopted by the thermal decomposition. After the preparation method is adopted, the silver powder or doped silver powder with the particle sizes of 0.01-5 mu m can be prepared, and power bonding agglomeration can be prevented; the microwave thermal decomposition is short in heating time and high in efficiency, and dopant in the doped silver powder can be evenly distributed; continuous production is realized, the cost is low, and the product quality is stable.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to the preparation method of a kind of silver powder or doping silver powder.
Background technology
Silver powder has high conduction, heat conduction, the performance such as anti-oxidant, is widely used in electronics industry and field of Environment Protection, and its technology of preparing is the emphasis difficult point of domestic research always, and high-end silver powder is abroad monopolized always.The preparation method of silver powder is a lot, mainly contain electron beam irradiation method, direct-current arc heat plasma method, microwave plasma method, mechanochemical synthesis, electrolysis etc., but special equipment and the shortcoming to environmental requirement harshness are consumed energy greatly, need in these methods existence.
Liquid phase reduction is the method for a kind of large-scale industrial production silver powder of generally adopting, by changing kind and the consumption of silver content, reducing agent and dispersant of presoma, regulate the conditions such as reaction density, temperature, stir speed (S.S.) and intensity, control pattern and the granularity of silver powder, but silver powder prepared by the direct pyrolysis of silver nitrate easily lumps, and pattern and granularity are wayward, be difficult to meet the requirement more and more higher to quality of cathode silver.
Wherein, in prior art, there is open pyrolysismethod to prepare silver powder, silver nitrate pressed powder is put into crucible to be placed in tube furnace and to heat, be heated to 550 DEG C with the firing rate of 5-50 DEG C/min, and pass into the air that relative humidity is 80-100%, air mass flow 200-800mL/min, after calcining 2-8h, stop heating and pass into chilled air cools to room temperature, collect solids in crucible, obtain the super fine silver powder that average grain diameter is 0.5-2 μ m, this technique is simple, gained morphologies is regular ball-type, but product granularity is thicker, unstable properties, energy consumption is large, industrialization cost performance is not high.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art, the preparation method of a kind of product degree of crystallinity and granularity height silver powder controlled, energy-conservation, simple to operate or doping silver powder is provided.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A preparation method for silver powder or doping silver powder, comprises following operating procedure:
Preparation silver salt solution, is aerosol by described silver salt solution ultrasonic atomizatio, and the power of described ultrasonic atomizatio is 0.2～10kw, frequency is 1.7～2.4MHz, atomization rates is 0.5～500kg/h, after described aerosol is mixed with carrier gas stream, carries out thermal decomposition, collects and obtains silver powder or doping silver powder;
Wherein, described silver salt solution is that silver ion molar concentration is the silver salt solution of 0.0001～4mol/L or the silver salt solution containing doped metal ion; Described, containing in the silver salt solution of doped metal ion, described doped metal ion is (1～5 × 10 with the ratio of the molar concentration of silver ion
-6): 1.
Above-mentioned employing ultrasonic atomizatio and thermal decomposition are prepared in the method for silver powder or doping silver powder, can be by regulating concentration, ultrasonic power and the frequency of silver salt solution to regulate the generation speed of aerosol and the size of atomized drop in ultrasonic atomizatio process, regulate the particle diameter of silver powder or doping silver powder, prevent powder adhesion reunion, reduce thermal decomposition energy consumption, simple to operate, cost is low, can realize continuous production, constant product quality.
Brief description of the drawings
Fig. 1 is the preparation flow figure of silver powder of the present invention or doping silver powder;
Fig. 2 is the scanning electron microscope (SEM) photograph of the doping silver powder prepared of embodiment 1;
Fig. 3 is the scanning electron microscope (SEM) photograph of the doping silver powder prepared of embodiment 5;
Fig. 4 is the scanning electron microscope (SEM) photograph of the doping silver powder prepared of embodiment 6.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Silver is the best metal material of electric conductivity, and it is widely used, mainly as the metallic conduction phase in electric slurry.And according to the difference of required function, can select to produce the different silver powder needing: as undoped common silver powder, or by adding different metal or semi metallic compound, the uniform doping preparing, the controlled doping silver powder of function.Different doping silver powder can meet various application requirements, as improve electric slurry welding performance, Ohmic contact, carry out the doping of P type or N-type, improve in high temperature sintering performance etc., the consumption that can reduce associated additives simultaneously, can be widely used in the fields such as electronic devices and components, integrated circuit, electronic building brick, circuit board assembling, liquid crystal module, touch-screen, display device, illumination, communication, automotive electronics, smart card, RF identification, electronic tag, solar cell.
The embodiment of the present invention provides the preparation method of a kind of above-mentioned silver powder or doping silver powder, and its operating process as shown in Figure 1.The preparation method of this silver powder or doping silver powder comprises following operating procedure:
S01: the aerosol of preparing silver salt: preparation silver salt solution is aerosol by described silver salt solution ultrasonic atomizatio;
S02: the aerosol of silver salt is mixed with carrier gas stream and carried out thermal decomposition: carry out thermal decomposition after the silver salt aerosol of preparing in step S01 is mixed with carrier gas stream, collect and obtain silver powder or doping silver powder.
Particularly, in above-mentioned steps S01, silver salt solution is that silver ion molar concentration is the silver salt solution of 0.0001～4mol/L or the silver salt solution containing doped metal ion; At this, containing in the silver salt solution of doped metal ion, doped metal ion is (1～5 × 10 with the ratio of the molar concentration of silver ion
-6): 1.In the time not containing other metallic element in above-mentioned silver salt solution, after the thermal decomposition in following ultrasonic atomizatio and step S02, prepare silver powder; In the time containing doped metal ion in above-mentioned silver salt solution, after the thermal decomposition in following ultrasonic atomizatio and step S02, prepare doping silver powder.
Silver compound in silver salt solution all can generate simple substance by thermal decomposition, and functional metal or semimetallic compound can generate metal oxide or simple substance etc. by thermal decomposition.Whether therefore, the producer can the different requirements to required silver powder according to product, select adulterate or choose different functional metal or semimetal and adulterate.In a preferred embodiment, above-mentioned silver ion obtains after being dissolved by argent, silver salt or silver oxide.Described silver salt does not limit, and comprises any soluble Ag-containing compound, specifically comprises at least one in hydracid silver, silver chlorate, silver nitrate, silver carbonate, and as further specific embodiment, described silver salt is preferably silver nitrate.In a preferred embodiment, above-mentioned doped metal ion refers to functional metal or semimetal ion, to be obtained by simple substance, salt or the oxide dissolution of respective metal element, as concrete preferred embodiment, the salt of above-mentioned containing metal element is at least one or the double salt in nitrate, hydracid eye, sulfate, carbonate.Preferably, described doped metal ion is more than one in lead, iron, zinc, copper, magnesium, cerium or aluminium, but be not limited to this, also can be the metal ion that other meet foregoing description, as zirconium, yttrium, cobalt, nickel, tin, antimony, bismuth, chromium, manganese, vanadium, molybdenum, titanium etc.Described lead, zirconium, yttrium, cobalt, nickel, tin, antimony, bismuth, chromium, manganese, vanadium, molybdenum, titanium, iron, zinc, copper, magnesium, cerium or the aluminium element existence form in doping silver powder is simple substance, oxide or salt.
In this step S01, power, frequency and the atomization rates thereof of described ultrasonic atomizatio is larger to the grain diameter influence of the silver powder preparing or doping silver powder, thereby can prepare by the size that regulates power, frequency and the atomization rates thereof of ultrasonic atomizatio to control atomized drop silver powder or the doping silver powder of different-grain diameter size.Repeatedly study discovery through inventor, when the silver ion molar concentration of silver salt solution is that 0.0001～4mol/L, ultrasonic atomizatio power are that 0.2～10kw, frequency are 1.7～2.4MHz, atomization rates while being 0.5～500kg/h, can obtain particle size range at the silver powder of 0.01-5 μ m or doping silver powder.
In above-mentioned steps S02, aerosol, after ultrasonic atomizing device produces, is carried and is left ultrasonic atomizing device by carrier gas stream, and aerosol is mixed with carrier gas stream and flowed together with carrier gas stream.Described carrier gas stream is inert gas, or the mist of inert gas and reducibility gas, and wherein, in the mist of described inert gas and reducibility gas, inert gas is 1:9～9:1 with the mixed volume ratio of reducibility gas.Adopt the mist of inert gas or inert gas and reducibility gas as carrier gas stream, can prevent that metal simple-substance is oxidized, reduce silver powder oxygen content.In further preferred embodiment, described inert gas is nitrogen, helium, and described reducibility gas is hydrogen.Of course it is to be understood that other inert gases or the reducibility gas that in this area, can be used for above-mentioned functions, all in protection scope of the present invention.In further preferred embodiment, the flow velocity of described carrier gas stream is 0.5～1000L/min, and air pressure is 0.1～10MPa, more preferably normal pressure.
In this step S02, the temperature of described thermal decomposition is 500～1200 DEG C, and the time is 1～20min.Mode of heating is unrestricted, can adopt the conventional mode of heating in this area to realize, for example infrared heating or Resistant heating.In concrete preferred embodiment, described thermal decomposition adopts microwave thermal to decompose, and microwave power is 5～50kw.The method that the present invention adopts microwave thermal to decompose is prepared silver powder or is mixed silver powder, its efficiency is high, the heat time is short, energy efficiency is obvious, and the mode of heating of its non-thermal effect can improve the dispersed of doped chemical after thermal decomposition and with silver-colored compatibility, be beneficial to the application performance that improves doping silver powder.
In step S02, the slaine in silver salt solution, after thermal decomposition process, generates silver powder or doping silver powder.In the present invention, the gathering system of powder does not limit, and uses conventional powder gathering system in this area all to collect.As concrete preferred embodiment, in order to realize continuous production, make constant product quality, the present invention adopts tornado collection device to collect.
The present invention adopts the technique of ultrasonic atomizatio and thermal decomposition to prepare silver powder or doping silver powder, and in order to obtain the adjustable product of the parameters such as particle diameter, the technological parameter of its ultrasonic atomizatio and thermal decomposition operation is not strictly limited to described parameter area.Wherein, in ultrasonic atomizatio process, can regulate the size of atomized drop with the generation speed of adjusting aerosol by the concentration, ultrasonic power and the frequency that regulate silver salt solution, thereby regulate the particle diameter of silver powder or doping silver powder.Particularly, concentration is less, and ultrasonic power is larger, and frequency is higher, and atomization rates is faster, and atomized drop diameter is less, and the particle diameter of silver powder or doping silver powder is less.The device of described ultrasonic atomizatio and thermal decomposition is all not particularly limited, and can realize described operation.
Compared with prior art, the present invention has following beneficial effect:
1, the embodiment of the present invention provides the preparation method of doping silver powder, by silver and other alloys are dissolved in solution, can realize the Uniform Doped of metal or semimetal atomic level.
2, the preparation method that the embodiment of the present invention provides, can control silver powder and the granularity of the silver powder that adulterates effectively, controls spherical silver powder or the granularity of the silver powder that adulterates as the concentration of the power by ultrasonic atomization, atomization rates and silver salt solution, and granularity control accuracy is high
3, the specific area that the present invention prepares silver powder or doping silver powder by physical-chemical process is large, but in preparation process, does not need to carry out Separation of Solid and Liquid, avoids reuniting between powder.Also without operations such as washing and filterings, make silver powder or silver-doped powder particles surface cleanness high, application performance is good.
4, the present invention obtains the spherical silver powder of required degree of crystallinity by control heat time, air temperature and current speed, make the degree of crystallinity of silver powder controlled, and employing microwave thermal decomposition efficiency is high, the heat time is short, energy efficiency is obvious, the mode of heating of its non-thermal effect can improve the dispersed of doped chemical after thermal decomposition and with silver-colored compatibility.
The preparation method of the silver powder that 5, the embodiment of the present invention provides or doping silver powder, cost is low, constant product quality, can produce continuously.Illustrate below the preparation method of above-mentioned silver powder or doping silver powder by multiple embodiment.
Embodiment 1
The adulterate preparation method of silver powder, operational flowchart, with reference to figure 1, comprises following operating procedure:
Compound concentration is the silver nitrate aqueous solution 10L of 2mol/L, plumbi nitras, aluminum nitrate, ferric nitrate, copper nitrate, zinc nitrate are dissolved in to described silver nitrate aqueous solution, obtain silver salt solution, wherein, lead ion, aluminium ion, iron ion, copper ion, zinc ion concentration are respectively 0.05mol/L, 0.003mol/L, 0.02mol/L, 0.0005mol/L, 0.0005mol/L, obtain silver salt solution;
In ultrasonic atomizatio equipment, gained silver salt solution is carried out to ultrasonic atomization, ultrasonic power is 500w, frequency is 2.4MHz, ultrasonic atomizatio speed is 20kg/h, atomized thing, aerosol and normal pressure and nitrogen: hydrogen volume than the carrier gas stream that is 3L/min for 6:4, flow mixes laggard enter the sintering cavity of microwave applicator, the microwave that employing power is 10KW heats 3min, the doping silver powder generating is gathered in sintering cavity bottom, collects and obtains the silver powder that adulterates.
Doping silver powder prepared by the present embodiment is the silver powder of doping lead, aluminium, iron, copper, zinc element, and gained doping silver powder is carried out to Xray fluorescence spectrometer (XRF) analysis, and the constituent content of the silver powder that obtains adulterating is in table 1.
Table 1
| Element | Content/wt% |
| Ag | 93.8 |
| Pb | 4.45 |
| Al | 0.69 |
| Fe | 0.15 |
| Cu | 0.068 |
| Zn | 0.097 |
Described doped chemical exists with oxide, salt or simple substance mode, can be used as doping and sintering aid or welding additive etc., it is carried out to scanning electron microscope analysis, the scanning electron microscope (SEM) photograph of the silver powder that obtains adulterating is shown in Fig. 2, visible silver-doped powder particles is spherical in shape, and distribution homogeneous.Further adopt conventional method test obtain adulterating particle diameter distribution, tap density, apparent density, the specific area of silver powder, data are in table 2.
Table 2
Wherein, D10 10% the particle average grain diameter that represents to adulterate in silver powder, D50 50% the particle average grain diameter that represents to adulterate in silver powder, D90 represents in doping silver powder the average grain diameter of 90% particle.
Embodiment 2
A preparation method for silver powder, Fig. 1 of operational flowchart reference example 1, comprises the following steps:
Compound concentration is the silver nitrate aqueous solution 10L of 3mol/L, obtains silver salt solution;
In ultrasonic atomizatio equipment, gained silver salt solution is carried out to ultrasonic atomization, ultrasonic power is 3000w, frequency is 2MHz, ultrasonic atomizatio speed is 150kg/h, atomized thing, aerosol and normal pressure and nitrogen: hydrogen volume is than being 1:3, flow be the carrier gas stream of 800L/min mix laggard enter the sintering cavity of microwave applicator, adopt the microwave that power is 30KW to heat 5min, the doping silver powder of generation is gathered in sintering cavity bottom, collects and obtains silver powder.
Silver powder prepared by the present embodiment is analyzed through Xray fluorescence spectrometer (XRF), learns that its silver content is 99.9.
Gained silver powder is carried out to scanning electron microscope analysis, and the granularity that test obtains silver powder is D
50=3 μ m, 50% diameter of particle is 3 μ m, spherical in shape, distribution homogeneous.
Embodiment 3
A preparation method for silver powder, Fig. 1 of operational flowchart reference example 1, comprises the following steps:
Compound concentration is the silver nitrate aqueous solution 10L of 0.0001mol/L, obtains silver salt solution;
In ultrasonic atomizatio equipment, gained silver salt solution is carried out to ultrasonic atomization, ultrasonic power is 1000w, frequency is 1.8MHz, ultrasonic atomizatio speed is 0.5kg/h, atomized thing, aerosol and normal pressure and nitrogen: hydrogen volume is than being 1:9, flow is that the temperature that enters resistance heater after the carrier gas stream of 1000L/min is mixed is the sintering cavity of 1000 DEG C, heating 20min, the silver powder of generation is gathered in sintering cavity bottom, collects and obtains the silver powder that adulterates.
Silver powder prepared by the present embodiment is to analyze through Xray fluorescence spectrometer (XRF), learns that its silver content is 99.9.Gained silver powder is carried out to laser particle size and electronic microscope photos, and the granularity that test obtains gained silver powder is D
50=0.01 μ m, 50% diameter of particle is 0.01 μ m, spherical in shape, distribution homogeneous.
Embodiment 4
The adulterate preparation method of silver powder, operational flowchart, with reference to figure 1, comprises following operating procedure:
Compound concentration is the silver nitrate aqueous solution 10L of 0.05mol/L, plumbi nitras, cerous nitrate, zinc nitrate, magron are dissolved in to described silver nitrate aqueous solution, obtain silver salt solution, wherein, the concentration of lead ion, cerium ion, zinc ion, magnesium ion is respectively 0.0005mol/L, 0.05mol/L, 2 × 10
-6mol/L, 0.00005mol/L, obtain silver salt solution;
In ultrasonic atomizatio equipment, gained silver salt solution is carried out to ultrasonic atomization, ultrasonic power is 10kw, frequency is 2MHz, ultrasonic atomizatio speed is 500kg/h, atomized thing, aerosol and normal pressure and nitrogen: hydrogen volume is brought the sintering cavity of microwave applicator into after mixing than the carrier gas stream that is 0.5L/min for 9:1, flow, adopt the microwave that power is 50KW to heat 15min, the doping silver powder generating is gathered in sintering cavity bottom, collects and obtains the silver powder that adulterates.
Doping silver powder prepared by the present embodiment is the silver powder of doping lead, cerium, zinc, magnesium elements, and gained doping silver powder is carried out to Xray fluorescence spectrometer (XRF) analysis, and the constituent content of the silver powder that obtains adulterating is in table 3.
Table 3
| Element | Mass content/wt% |
| Ag | 99.00 |
| Pb | 0.47 |
| Ce | 0.51 |
| Zn | 0.0003 |
| Mg | 0.001 |
Described doped chemical exists with oxide, salt or simple substance mode, can be used as doping and sintering aid or welding additive etc., and it is carried out to scanning electron microscope analysis, and the granularity of the silver powder that obtains adulterating is D
50=1.25 μ m, 50% diameter of particle is 1.25 μ m, spherical in shape, distribution homogeneous.
Embodiment 5
The adulterate preparation method of silver powder, operational flowchart, with reference to figure 1, comprises following operating procedure:
Compound concentration is the silver nitrate aqueous solution 10L of 0.5mol/L, yttrium nitrate, zirconium nitrate, Titanium Nitrate, chromic nitrate, bismuth nitrate, copper nitrate are dissolved in to described silver nitrate aqueous solution, obtain silver salt solution, wherein, the concentration of ruthenium ion, zirconium ion, titanium ion, chromium ion, bismuth ion, copper ion is respectively 0.01mol/L, 0.0004mol/L, 5 × 10
-5mol/L, 0.0004mol/L, 0.0004mol/L, 0.00025mol/L, obtain silver salt solution;
In ultrasonic atomizatio equipment, gained silver salt solution is carried out to ultrasonic atomization, ultrasonic power is 200w, frequency is 2.4MHz, ultrasonic atomizatio speed is 300kg/h, atomized thing, the nitrogen carrier gas stream that aerosol is 500L/min with normal pressure, flow enters resistance heater temperature after mixing is the sintering cavity of 1200 DEG C, heating 1min, the doping silver powder generating is gathered in sintering cavity bottom, collects and obtains the silver powder that adulterates.
Doping silver powder prepared by the present embodiment is the silver powder of doped with yttrium, zirconium, titanium, chromium, bismuth, copper, and gained doping silver powder is carried out to Xray fluorescence spectrometer (XRF) analysis, and the constituent content of the silver powder that obtains adulterating is in table 4.
Table 4
| Element | Content/wt% |
| Ag | 97.6 |
| Y | 2.171 |
| Zr | 0.0059 |
| Ti | 0.061 |
| Cr | 0.069 |
| Bi | 0.057 |
| Cu | 0.042 |
Described doped chemical exists with oxide, salt or simple substance mode, can be used as doping and sintering aid or welding additive etc., and it is carried out to scanning electron microscope analysis, obtains scanning electron microscope (SEM) photograph and sees Fig. 3, and the granularity of test doping silver powder is D
50=0.15 μ m, 50% diameter of particle is 0.15 μ m, spherical in shape, distribution homogeneous.
Embodiment 6
The adulterate preparation method of silver powder, operational flowchart, with reference to figure 1, comprises following operating procedure:
Compound concentration is the silver nitrate aqueous solution 10L of 4mol/L, ferric nitrate, zinc nitrate, copper chlorate, magron are dissolved in to described silver nitrate aqueous solution, obtain silver salt solution, wherein, the concentration of iron ion, zinc ion, copper ion, magnesium ion is respectively 0.05mol/L, 0.001mol/L, 0.0005mol/L, 2 × 10
-5mol/L, obtains silver salt solution;
In ultrasonic atomizatio equipment, gained silver salt solution is carried out to ultrasonic atomization, ultrasonic power is 7500w, frequency is 1.7MHz, ultrasonic atomizatio speed is 100kg/h, atomized thing, the helium carrier gas stream that aerosol is 20L/min with normal pressure, flow enters resistance heater temperature after mixing is the sintering cavity of 500 DEG C, heating 15min, the doping silver powder generating is gathered in sintering cavity bottom, collects and obtains the silver powder that adulterates.
Doping silver powder prepared by the present embodiment is the silver powder of doping iron, zinc, copper, magnesium elements, and gained doping silver powder is carried out to Xray fluorescence spectrometer (XRF) analysis, and the constituent content of the silver powder that obtains adulterating is in table 5.
Table 5
| Element | Content/wt% |
| Ag | 98.62 |
| Fe | 1.33 |
| Zn | 0.042 |
| Cu | 0.0135 |
| Mg | 0.00257 |
Described doped chemical exists with oxide, salt or simple substance mode, can make doping and sintering aid or welding additive etc., and it is carried out to scanning electron microscope analysis, obtains scanning electron microscope (SEM) photograph and sees Fig. 4, and the granularity of test doping silver powder is D
50=3.7 μ m, 50% diameter of particle is 3.7 μ m, spherical in shape, distribution homogeneous.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a preparation method for silver powder or doping silver powder, is characterized in that, comprises following operating procedure:
Preparation silver salt solution, is aerosol by described silver salt solution ultrasonic atomizatio, and the power of described ultrasonic atomizatio is 0.2～10kw, frequency is 1.7～2.4MHz, atomization rates is 0.5～500kg/h, after described aerosol is mixed with carrier gas stream, carries out thermal decomposition, collects and obtains silver powder or doping silver powder;
Wherein, described silver salt solution is that silver ion molar concentration is the silver salt solution of 0.0001～4mol/L or the silver salt solution containing doped metal ion; Described, containing in the silver salt solution of doped metal ion, described doped metal ion is (1～5 × 10 with the ratio of the molar concentration of silver ion
-6): 1.
2. the preparation method of silver powder as claimed in claim 1 or doping silver powder, is characterized in that, the temperature of described thermal decomposition is 500～1200 DEG C, and the time is 1～20min.
3. preparation method as claimed in claim 1 or 2, is characterized in that, described thermal decomposition adopts microwave thermal to decompose, and described microwave power is 5～50kw.
4. the preparation method of silver powder as claimed in claim 1 or doping silver powder, it is characterized in that, described doped metal ion is more than one in lead, zirconium, yttrium, cobalt, nickel, tin, antimony, bismuth, chromium, manganese, vanadium, molybdenum, titanium, iron, zinc, copper, magnesium, cerium or aluminium.
5. the preparation method of the silver powder as described in claim 1 or 4 or doping silver powder, is characterized in that, described doped metal ion is more than one in lead, iron, zinc, copper, magnesium, cerium or aluminium.
6. the preparation method of the silver powder as described in claim 1 or 4 or doping silver powder, is characterized in that, the anion in described silver salt solution is more than one in nitrate anion, halide ion, chlorate anions, sulfate radical and carbonate.
7. the preparation method of silver powder as claimed in claim 1 or doping silver powder, is characterized in that, the flow velocity of described carrier gas stream is 0.5～1000L/min.
8. the preparation method of the silver powder as described in claim 1 or 7 or doping silver powder, it is characterized in that, described carrier gas stream is inert gas, or the mist of inert gas and reducibility gas, in the mist of described inert gas and reducibility gas, the volume ratio of inert gas and reducibility gas is 1:9～9:1.
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| CN110819801A (en) * | 2018-08-07 | 2020-02-21 | 昆明理工大学 | Method for purifying zinc sulfate solution by microwave heating of zinc powder |
| CN110819801B (en) * | 2018-08-07 | 2021-01-22 | 昆明理工大学 | Method for purifying zinc sulfate solution by microwave heating of zinc powder |
| CN110819802A (en) * | 2018-08-08 | 2020-02-21 | 昆明理工大学 | Method for strengthening and purifying zinc sulfate solution by microwave heating of zinc powder |
| CN110819802B (en) * | 2018-08-08 | 2021-01-22 | 昆明理工大学 | Method for strengthening and purifying zinc sulfate solution by microwave heating of zinc powder |
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