CN105436517A - Method for preparing metal powder by utilizing nano crystal seed induction - Google Patents
Method for preparing metal powder by utilizing nano crystal seed induction Download PDFInfo
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- CN105436517A CN105436517A CN201510981595.8A CN201510981595A CN105436517A CN 105436517 A CN105436517 A CN 105436517A CN 201510981595 A CN201510981595 A CN 201510981595A CN 105436517 A CN105436517 A CN 105436517A
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- 239000002184 metal Substances 0.000 title claims abstract description 48
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 48
- 239000000843 powder Substances 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title abstract description 20
- 239000002159 nanocrystal Substances 0.000 title abstract description 4
- 230000006698 induction Effects 0.000 title abstract 2
- 239000002270 dispersing agent Substances 0.000 claims abstract description 46
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 31
- 239000007800 oxidant agent Substances 0.000 claims abstract description 31
- 239000002923 metal particle Substances 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 112
- 238000002360 preparation method Methods 0.000 claims description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 239000000428 dust Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 18
- 229910021645 metal ion Inorganic materials 0.000 claims description 17
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 16
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 15
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 13
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims description 9
- 150000004706 metal oxides Chemical class 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 7
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical group ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 7
- 229930003268 Vitamin C Natural products 0.000 claims description 7
- 238000005189 flocculation Methods 0.000 claims description 7
- 230000016615 flocculation Effects 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 239000011718 vitamin C Substances 0.000 claims description 7
- 235000019154 vitamin C Nutrition 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 229920001219 Polysorbate 40 Polymers 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000013528 metallic particle Substances 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 claims description 6
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 claims description 6
- 229940101027 polysorbate 40 Drugs 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 241000605159 Nitrobacter Species 0.000 claims description 5
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 150000003863 ammonium salts Chemical class 0.000 claims description 4
- 230000000536 complexating effect Effects 0.000 claims description 4
- -1 hydroxylamine compound Chemical class 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000008394 flocculating agent Substances 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229940049964 oleate Drugs 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 2
- 238000007664 blowing Methods 0.000 claims 1
- 239000002082 metal nanoparticle Substances 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 7
- 230000001590 oxidative effect Effects 0.000 abstract 2
- 210000004940 nucleus Anatomy 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
Abstract
The invention discloses a method for preparing metal powder by utilizing nano crystal seed induction. The method concretely comprises the following steps: preparing a dispersant solution, and adding the dispersant solution in a reaction kettle in advance; then, preparing an oxidant solution and a reducing agent solution, and adding the oxidant solution and the reducing agent solution in the reaction kettle at the same; under violent stirring, conducting reduction reaction. Nano metal particles directly added in the dispersant solution in advance are used as crystal seeds or newborn nano metal particles in the initial reaction period are used as the crystal seeds, the nano crystal seeds can effectively control the particle sizes of reduced metal particles in the remaining reaction process. The method can effectively control the particle sizes of metal powder in the production process and meanwhile has good control for the growth rate and the dispersity of crystal nucleuses, and the produced metal powder has good degree of crystallinity and degree of sphericity, high compactness and high dispersity.
Description
Technical field
The present invention relates to field of material technology, particularly a kind of preparation method of micro-sized metal powder.
Background technology
Metal dust is widely used in the electronic devices and components manufacture of electronics industry, plating, the industry such as battery and chemical industry catalysis, jewellery.Along with electronic component is to development that is microminiaturized and high-performance direction, the performance indications such as sintering activity, dispersiveness, sphericity, degree of crystallinity of metal dust are had higher requirement.At present, the preparation method of metal dust comprises physical method and chemical method, and physical method comprises atomization, gas evaporation condensation method, polishing etc., and chemical method mainly comprises liquid phase reduction, electrochemical deposition method, electrolysis etc.Because Physical exists the problem of high cost low-yield, present widely used chemical liquid phase reducing process, namely metal is reduced to by metallic salting liquid or oxide by chemical reaction reaction, as CN1301205, powder used in metallurgy sintering activity metal dust and alloy end method with and its preparation method and application.Chinese patent application CN101597777 discloses a kind of by containing metal oxide or salt, adopts electrolysis mode to be reduced into the method for metal.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method being different from the metal micro level powder of prior art.
In order to solve the problems of the technologies described above, technical scheme of the present invention utilizes nanosized seeds to induce a kind of preparation method producing metal dust, and its feature is, it comprises the steps:
(1) preparation of oxidizing agent solution, metal nitrate or sulfate solid are dissolved in deionized water, or add ammoniacal liquor production complexing metal ammonium salt solution again, keep [metal ion] concentration=0.1 ~ 5 mol/L in oxidizing agent solution, after fully stirring, keep 10 ~ 50 DEG C of temperature constant states;
(2) reductant solution preparation, add one or more hydroxylamine compound solids or vitamin C or formaldehyde or hydrazine hydrate reduction agent in deionized water to dissolve and make, keep [reducing agent] concentration=0.1 ~ 5 mol/L in reductant solution, reductant solution volume is 0.5 ~ 2 times of oxidizing agent solution volume, keeps 10 ~ 50 DEG C of temperature constant states after fully stirring;
(3) dispersant solution preparation, one or more dispersants are joined in deionized water, above-mentioned dispersant gross mass is in deionized water 0.1 ~ 2 times of aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality, abundant stirring directly adds metal nano crystal seed afterwards, or adds one or more metal nitrates or metal sulfate or metal oxide and fully stir rear maintenance 10 ~ 50 DEG C of temperature constant states;
(4) preparation of flocculant, take reaction and generate one or more oleates that the oleic acid of metal dust quality 0.05% ~ 0.5% and reaction generate metal powder quality 0.05% ~ 0.5%, they are added in flocculating agent formulation tank and add after a small amount of alcohol dissolves each other again;
(5) before reaction starts, add the dispersant solution prepared in a kettle. in advance, open and stir, constant flow adds oxidizing agent solution and reductant solution simultaneously subsequently, and flow is: 0.1L ~ 20L/Min; Initial reaction stage, a large amount of dispersant in the dispersant solution added in advance is utilized to suppress the reunion of nano metal particles and the effect of stable newborn nano metal particles, thus in reaction system, utilize existing or newborn quantitative nano metallic particles to control the generation of metallic particles as crystal seed, reach the reduction growth system of size tunable, in the course of reaction of remainder, play the control of good redox rate and nuclei grow speed simultaneously;
(6) after having reacted, solution in reactor is entered in flocculation sediment still, adds flocculant, staticly settle separation after rapid stirring 5 ~ 30min and obtain the metal ball shaped of various different-grain diameter scope and class spherical powder.
In the preferred technical solution of the present invention, in the preparation of described step (2) reductant solution, reducing agent is selected from azanol, HAS, HAN, vitamin C, the formalin of 37% ~ 40%, one or more mixing of hydrazine hydrate, reducing agent with the metal ion mol ratio in abovementioned steps (1) is in the solution: [metal ion]: [azanol]=1:0.1 ~ 5, or [metal ion]: [HAS]=1:0.1 ~ 5, or [metal ion]: [HAN]=1:0.1 ~ 5, or [metal ion]: [vitamin C]=1:0.1 ~ 5, or [metal ion]: [formaldehyde]=1:0.1 ~ 5, or [metal ion]: [hydrazine hydrate]=1:0.1 ~ 5.
The preparation of step (3) dispersant solution, by one or more polyethylene of dispersing agent pyrrolidones (PVP), or PEG400, or polysorbate40, or glycerine joins in the deionized water of aforementioned reductant solution volume 0.5 ~ 2 times, above-mentioned dispersant gross mass is in deionized water 0.1 ~ 2 times of aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality, one or more metal nitrates of 0.01% ~ 1.0% of aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality or sulfate or metal oxide is added again after abundant stirring, or directly add aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality 0.01% ~ 0.5% nano-metal particle, 10 ~ 50 DEG C of temperature constant states are kept after abundant stirring, this step utilizes id reaction initial stage a large amount of dispersant to suppress the reunion of nano metal particles and the effect of stable newborn nano metal particles, thus in reaction system, there is quantitative nano-metal particle as crystal seed to control the generation of metallic particles, reach the reduction growth system of size tunable, in course of reaction, play the control of good redox rate and nuclei grow speed.
In the preferred technical solution of the present invention, in the preparation of described step (3) dispersant solution nanosized seeds step described in claim 1 (5) can be selected in initial reaction stage to utilize one or more metallic salts in the dispersant solution added in advance or metal oxide to be reduced and the nano metal particles of new life as crystal seed, join that slaine in dispersant solution or metal oxide gross mass are metal nitrate or metal sulfate quality in described step (1) oxidizing agent solution in advance 0.01% ~ 1.0%.
In the preferred technical solution of the present invention, in the preparation of described step (3) dispersant solution, nanosized seeds is for directly to add nano-metal particle as crystal seed, add that nano-metal particle quality is metal nitrate or sulfate quality in step (1) oxidizing agent solution 0.01% ~ 0.5%.
In the preferred technical solution of the present invention, the preparation of the flocculant of described step (4), described oleate is selected from unrighted acid and ammonium salt thereof.
In the preferred technical solution of the present invention, in step (5), the mode of the oxidizing agent solution that abovementioned steps two kinds is quantitatively prepared by micropore by the pressure utilizing pump or compressed air to produce and reductant solution constant flow joins in reactor, the flow-control scope of two kinds of solution is 0.1L/min ~ 20L/min, and react under vigorous stirring, mixing speed: 200rpm ~ 500rpm, is separated by flocculation sediment after reacting completely again and obtains all kinds of ball-type and class ball-type metal powder.
In the preferred technical solution of the present invention, in step (6), flocculant rapid loading mode is adopted in flocculation sediment process, adding speed is 1L/min ~ 10L/min, and strong agitation, mixing speed 200rpm ~ 500rpm, after fully stirring 5 ~ 30 minutes, staticly settles separation and obtains the metal ball shaped of various different-grain diameter scope and class spherical powder.
In the preferred technical solution of the present invention, metal comprises silver, copper, nickel.
In the preferred technical solution of the present invention, described metal dust is spherical and the spherical micron particles of class.
The reaction system of preferred system solution of the present invention keeps 10 ~ 50 DEG C of temperature constant states, is conducive to the carrying out reacted, certainly too high or too low the carrying out all being unfavorable for reacting.Dispersant solution in the present invention, regulate in dispersant at the nano-metal particle of initial reaction stage new life or the content of nano-metal particle that directly adds according to the production requirement of different metal powder diameter, produce the micro-sized metal powder-product of different-grain diameter, when nano-metal particle content is 0.01% ~ 0.4% of reaction production metal dust quality, the silver powder particle diameter produced is bigger than normal, and D50 is between 1.0um ~ 2.5um; When nano-metal particle content is 0.4% ~ 1% of reaction production metal dust quality, the metal particle diameter produced is less than normal, and D50 is between 0.2um ~ 1.0um; Therefore adjustment nano-metal particle content can be carried out according to the Particle size requirements of the concrete metal dust produced in production process.
Advantage of the present invention and beneficial effect are:
(1) dispersant solution of the inventive method is interior introduces nanosized seeds, thus make metal ion size tunable in reduction process, can fast and stable from containing ammonia complexing metal salt solution or containing metal nitrate or metallic sulfate-containing by metallic, as silver ion reduction becomes silver powder, and ensure that the morphologies that formed is ball-type or class ball-type and particle diameter can be regulated by introducing nanosized seeds quantity.
(2) while method of the present invention adopts constant flow oxidizing agent solution and reductant solution, feed postition controls the dispersiveness of metal dust in course of reaction effectively, solve existing metal dust, as the agglomeration traits in silver powder production process, and metal dust average grain diameter is 0.1um ~ 10um.
(3) this inventive method effectively can control metal ball shaped and class spherical powder reaction rate in process of production, to nucleus growth speed and dispersiveness, there is good control, spherical and the class globular metallic powder produced has extraordinary degree of crystallinity, sphericity, high jolt ramming and polymolecularity.
(4) preparation method of the present invention can be applied to suitability for industrialized production, and large-scale production is for silver powder: can reach 5-150kg/ batch, and the laboratory preparation method of relatively existing silver powder production technology has significant superiority.
(5) preparation method of the present invention is simple, and raw material is cheap, and process is easy to control, reacts completely, steady quality between institute's production product batches, thus greatly reduces product disqualification rate, brings considerable economic benefit to enterprise.
Accompanying drawing explanation
Fig. 1 is the flow chart of method of the present invention.
Fig. 2 A, 2B, 2C are the droplet measurement schematic diagram of the metal dust that the inventive method prepares.
Fig. 3 is the SEM electron microscopic figure of the ball shape silver powder that the inventive method prepares, wherein, Fig. 3 A is the ball shape silver powder figure that SEM Electronic Speculum amplifies × 10000 times, Fig. 3 B is the ball shape silver powder figure that SEM Electronic Speculum amplifies × 10000 times, Fig. 3 C is the ball shape silver powder figure that SEM Electronic Speculum amplifies × 5000 times, Fig. 3 D is that SEM Electronic Speculum amplifies the ball shape silver powder figure of × 5000 times, and Fig. 3 E is the ball shape silver powder figure that SEM Electronic Speculum amplifies × 5000 times, Fig. 3 F is the ball shape silver powder figure that SEM Electronic Speculum amplifies × 2000 times.
Detailed description of the invention:
For understanding the present invention further, below in conjunction with specific embodiment, preferred version of the present invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
(1) oxidizing agent solution containing liquor argenti nitratis ophthalmicus is prepared, the silver nitrate liquid of nitric acid silver salt solid or equivalent is dissolved in deionized water, keep silver ion molar concentration [silver ion]=0.5mol/l in solution, ammoniacal liquor (20%) is added again after abundant stirring, regulate pH between 2.5 ~ 9.5, keep solution 10 ~ 50 DEG C of temperature constant states;
(2) reductant solution containing hydrazine hydrate is prepared, add hydrazine hydrate solution in deionized water to make, according to the silver content in argentiferous oxidizing agent solution, keep mol ratio [silver ion] in solution: [hydrazine hydrate]=1:0.1 ~ 5, keep solution 10 ~ 50 DEG C of temperature constant states;
(3) dispersant solution preparation: the polysorbate40 or the PEG400 dissolving that add one or more are in deionized water made, its content is 20 ~ 100g/l, abundant stirring, then add nano metal Argent grain (100nm ~ 200nm) 0.01-0.05g, keep solution 10 ~ 50 DEG C of temperature constant states;
(4) utilize measuring pump in advance the dispersant solution containing polysorbate40 or PEG400 compound to be squeezed into reactor, quantitatively the oxidizing agent solution containing ammonia complexing silver is carried out metered injection to (flow is: 0.1L ~ 20L/Min) in reactor with the reductant solution containing hydrazine hydrate by micropore subsequently; (300rpm) reduction reaction under vigorous stirring, obtains the silver powder of various different-grain diameter scope by adding flocculant precipitate and separate after having reacted.
Embodiment 2
Oxidizing agent solution is prepared: the liquor argenti nitratis ophthalmicus 500ml preparing argentiferous 200g/L in 2000ml wide-mouth bottle, toward wherein adding the ammoniacal liquor 200ml that mass percentage concentration is 20%, obtaining silver ammino solution, being heated to 45 DEG C of constant temperature for subsequent use,
Reductant solution is prepared: in another 2000ml wide-mouth bottle, preparation is containing vitamin c solution and HAS: 50g HAS and 50g vitamin C are dissolved in 500ml deionized water, are heated to 45 DEG C of constant temperature for subsequent use,
Dispersant solution prepare: the dispersant solution prepared in 500ml wide-mouth bottle: be dissolved in 300ml deionized water by 85gPVP and 50ml polysorbate40, adds 1g silver oxide, be heated to 45 DEG C for subsequent use,
Measuring pump is utilized to be squeezed into by dispersant solution in advance in 5000ml wide-mouth bottle, quantitatively above-mentioned two kinds of oxidizing agent solutions prepared and reductant solution are carried out in 5000ml wide-mouth bottle dropping mixing by micropore subsequently simultaneously, the flow-control of two kinds of solution is 250ml/min, and start to stir, stir speed (S.S.) 400rpm, after reaction terminates, add flocculant, stirs and after 10 minutes, to staticly settle that to be separated the spherical or spherical average grain diameter of class of acquisition be the silver powder of 0.1um ~ 10um.
Embodiment 3
In 2000ml wide-mouth bottle, prepare the copper-bath 650ml of cupric 300g/L, toward wherein adding the ammoniacal liquor 350ml that mass percentage concentration is 20%, obtaining copper ammon solution, being heated to 35 DEG C,
In another 2000ml wide-mouth bottle, preparation is containing the reductant solution of azanol: be dissolved in 1000ml deionized water by 150g azanol, be heated to 35 DEG C,
The dispersant solution prepared in 500ml wide-mouth bottle: be dissolved in by 25gPVP in 250ml deionized water, adds 1g copper nanoparticle, is heated to 35 DEG C,
Measuring pump is utilized to be squeezed into by dispersant solution in advance in 5000ml wide-mouth bottle, by measuring pump, above-mentioned two kinds of copper ammon solutions prepared and hydroxylamine solution are carried out injection mixing in 5000ml wide-mouth bottle subsequently, the injection flow of two kinds of solution controls as 500ml/min, and start to stir, stir speed (S.S.): 400rpm, obtains spherical or class spherical copper powder by adding flocculant precipitate and separate after reacting completely.
Embodiment 4: batch production
In the preparing tank of 1000L, add 135 kilograms of silver nitrate solids, add deionization 800L, toward wherein adding the ammoniacal liquor 250L that mass percentage concentration is 15% after abundant stirring and dissolving, obtaining silver ammino solution, being heated to 35 DEG C (oxidizing agent solution) for subsequent use,
In the preparing tank of another 1000L, add 500L deionized water, add 50 kilograms of vitamin Cs and 5 kilograms of HANs subsequently, be heated to 35 DEG C (reductant solution) for subsequent use after fully dissolving,
In 500L preparing tank, 50kgPVP is dissolved in 400L deionized water, adds 5kg polyethylene glycol, add nano-Ag particles 500g after fully stirring, be heated to 35 DEG C (dispersant solution) for subsequent use,
Measuring pump is utilized to be squeezed in advance by dispersant solution in 3000L reactor, quantitatively the above-mentioned two kinds oxidizing agent solutions and reductant solution prepared are carried out in retort injection mixing by micropore subsequently, the injection flow of two kinds of solution controls as 5L/min, and start to stir, stir speed (S.S.) 120rpm, dispersant solution is dripped in course of reaction, after reacting completely, reactant liquor is drained in 5000L flocculation sediment still, add flocculant, open and stir, stir speed (S.S.) 300rpm, fully stir fast after 30 minutes, staticly settle and be separated that to obtain the spherical or spherical average grain diameter of class be the silver powder of 0.1um ~ 10um.
Detection data if Fig. 1 is three groups of silver powder that invention according to the present invention prepares:
And the Electronic Speculum figure of silver powder S001 is 3A and 3D, the Electronic Speculum figure of silver powder S002 is 3B and 3E, and the Electronic Speculum figure of silver powder S003 is 3C and 3F.
Technology contents of the present invention and technical characteristic have disclosed as above; but those of ordinary skill in the art still may do all replacement and the modification that do not deviate from spirit of the present invention based on teaching of the present invention and announcement; therefore; scope should be not limited to the content that embodiment discloses; and various do not deviate from replacement of the present invention and modification should be comprised, and contained by present patent application claim.
Claims (11)
1. utilize nanosized seeds to induce the preparation method producing metal dust, it is characterized in that, it comprises the steps:
(1) preparation of oxidizing agent solution, metal nitrate or sulfate solid are dissolved in deionized water, or add ammoniacal liquor generation complexing metal ammonium salt solution again, keep [metal ion] concentration=0.1 ~ 5 mol/L in oxidizing agent solution, after fully stirring, keep 10 ~ 50 DEG C of temperature constant states;
(2) reductant solution preparation, add one or more hydroxylamine compound solids or vitamin C or formaldehyde or hydrazine hydrate reduction agent in deionized water to dissolve and make, keep [reducing agent] concentration=0.1 ~ 5 mol/L in reductant solution, reductant solution volume is 0.5 ~ 2 times of oxidizing agent solution volume, keeps 10 ~ 50 DEG C of temperature constant states after fully stirring;
(3) dispersant solution preparation, by one or more dispersants, polyvinylpyrrolidone PVP or PEG400 or polysorbate40 or glycerine join in deionized water, above-mentioned dispersant gross mass is in deionized water 0.1 ~ 2 times of aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality, add nano metal crystal seed after abundant stirring again or add one or more metal nitrates of 0.01% ~ 1.0% or the mixture of sulfate or metal oxide of metal nitrate or sulfate quality in oxidizing agent solution, 10 ~ 50 DEG C of temperature constant states are kept after abundant stirring,
(4) preparation of flocculant, take reaction and generate one or more oleates that the oleic acid of metal dust quality 0.05% ~ 0.5% or reaction generate metal dust quality 0.05% ~ 0.5%, they are added in flocculating agent formulation tank and add after a small amount of alcohol dissolves each other again;
(5) before reaction starts, add the dispersant solution prepared in a kettle. in advance, open and stir, constant flow adds oxidizing agent solution and reductant solution simultaneously subsequently, and flow is: 0.1L ~ 20L/Min; Initial reaction stage, a large amount of dispersant in the dispersant solution added in advance is utilized to suppress the reunion of the nano metal particles directly joined in dispersant solution and stablize by the effect of the nano metal particles of initial reaction stage new life, thus in whole reaction system, utilize existing or newborn quantitative nano metallic particles to control the generation of metallic particles as crystal seed, reach the reduction growth system of size tunable, in course of reaction, play the control of good redox rate and nuclei grow speed simultaneously;
(6) after having reacted, solution in reactor is drained in flocculation sediment still, adds flocculant, after rapid stirring 5 ~ 60min, staticly settle the ball-type or the class ball-type metal dust that are separated and obtain various different-grain diameter scope.
2. preparation method according to claim 1, it is characterized in that, in the preparation of described step (2) reductant solution, reducing agent is selected from azanol, HAS, HAN, vitamin C, the formalin of 37% ~ 40%, one or more mixture of hydrazine hydrate, reducing agent with the metal ion mol ratio in abovementioned steps (1) is in the solution: [metal ion]: [azanol]=1:0.1 ~ 5, or [metal ion]: [HAS]=1:0.1 ~ 5, or [metal ion]: [HAN]=1:0.1 ~ 5, or [metal ion]: [vitamin C]=1:0.1 ~ 5, or [metal ion]: [formaldehyde]=1:0.1 ~ 5, or [metal ion]: [hydrazine hydrate]=1:0.1 ~ 5, 10 ~ 50 DEG C of temperature constant states are kept after abundant stirring.
3. preparation method according to claim 1, it is characterized in that, in the preparation of described step (3) dispersant solution, dispersant selects one or more dispersants: polyvinylpyrrolidone PVP, or PEG400, or polysorbate40, or glycerine joins in the deionized water of step described in aforementioned claim 1 (2) reductant solution volume 0.5 ~ 2 times, above-mentioned dispersant gross mass is in deionized water 0.1 ~ 2 times of metal nitrate or sulfate gross mass in step described in aforementioned claim 1 (1) oxidizing agent solution, 10 ~ 50 DEG C of temperature constant states are kept after abundant stirring.
4. preparation method according to claim 1, it is characterized in that, described step (3) dispersant solution preparation in nanosized seeds step described in claim 1 (5) can be selected in initial reaction stage to utilize the mixture of one or both metallic salts in the dispersant solution added in advance or metal oxide to be reduced and the nano metal particles of new life as crystal seed, join that one or more slaines in dispersant solution or metal oxide gross mass are metal nitrate or sulfate quality in described step (1) oxidizing agent solution in advance 0.01% ~ 1.0%.
5. preparation method according to claim 1, it is characterized in that, in the preparation of described step (3) dispersant solution, nanosized seeds can be selected and directly adds nano-metal particle as crystal seed, add that nano-metal particle quality is metal nitrate or sulfate quality in step (1) oxidizing agent solution 0.01% ~ 0.5%.
6. the preparation method according to claim 4 or 5, it is characterized in that, the metal nanoparticle utilizing one or more metal nitrates or metal sulfate or metal oxide of adding in advance in initial reaction stage dispersant solution and the reductant solution added first to react production uses as crystal seed, and the particle diameter of the nano-metal particle of these new lives is 1nm ~ 800nm; Or the metallic particles directly adding nanometer particle size uses as crystal seed, the particle diameter of the nano-metal particle directly added is 1nm ~ 800nm.
7. preparation method according to claim 1, is characterized in that, the oleate in the flocculant of described step (4) is selected from unrighted acid and ammonium salt thereof.
8. preparation method according to claim 1, it is characterized in that, in described step (5), the mode of the oxidizing agent solution that middle step (1) and step (2) are quantitatively prepared by micropore by the pressure utilizing pump or compressed air to produce and reductant solution constant flow joins in reactor, the flow-control scope 0.1L/min ~ 10L/min of two kinds of solution, and react under vigorous stirring, mixing speed: 200rpm ~ 500rpm, is separated by flocculation sediment after reacting completely again and obtains all kinds of ball-type or class ball-type metal dust.
9. preparation method according to claim 1, it is characterized in that, in described step (6), in flocculation sediment still, adopt quick blowing mode to add flocculant, adding speed is 1L/min ~ 10L/min, and strong agitation, mixing speed 200rpm ~ 500rpm, abundant stirring, after 5 ~ 60 minutes, staticly settles separation and obtains the metal ball shaped of various different-grain diameter scope and class spherical powder.
10. preparation method according to claim 1, is characterized in that, described metal comprises silver, copper, nickel.
11. preparation methods according to claim 1, is characterized in that, described metal dust is spherical and the spherical micron particles of class.
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