CN105436517B - 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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- 239000002184 metal Substances 0.000 title claims abstract description 50
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 50
- 239000000843 powder Substances 0.000 title claims abstract description 19
- 230000006698 induction Effects 0.000 title claims abstract description 5
- 238000000034 method Methods 0.000 title abstract description 19
- 239000002159 nanocrystal Substances 0.000 title abstract description 4
- 239000002270 dispersing agent Substances 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- 239000007800 oxidant agent Substances 0.000 claims abstract description 30
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 28
- 239000002923 metal particle Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract 3
- 239000000243 solution Substances 0.000 claims description 114
- 238000002360 preparation method Methods 0.000 claims description 26
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 25
- 239000000428 dust Substances 0.000 claims description 19
- 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 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-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 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 12
- 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
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims description 8
- 150000004706 metal oxides Chemical class 0.000 claims description 8
- 238000005189 flocculation Methods 0.000 claims description 7
- 230000016615 flocculation Effects 0.000 claims description 7
- -1 hydroxylamine compound Chemical class 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 241000605159 Nitrobacter Species 0.000 claims description 6
- 229930003268 Vitamin C Natural products 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000011718 vitamin C Substances 0.000 claims description 6
- 235000019154 vitamin C Nutrition 0.000 claims description 6
- 238000007792 addition Methods 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 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
- 239000013528 metallic particle Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 4
- 229920001219 Polysorbate 40 Polymers 0.000 claims description 4
- 150000003863 ammonium salts Chemical class 0.000 claims description 4
- 230000000536 complexating effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229940049964 oleate Drugs 0.000 claims description 4
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 claims description 4
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 claims description 4
- 229940101027 polysorbate 40 Drugs 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 3
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 150000003839 salts Chemical class 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
- 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
- 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
- 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
- AIMMVWOEOZMVMS-UHFFFAOYSA-N cyclopropanecarboxamide Chemical compound NC(=O)C1CC1 AIMMVWOEOZMVMS-UHFFFAOYSA-N 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 239000012263 liquid product Substances 0.000 claims 1
- 239000002082 metal nanoparticle Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229920000136 polysorbate Polymers 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000006722 reduction reaction Methods 0.000 abstract description 9
- 210000004940 nucleus Anatomy 0.000 abstract 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 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
- OTCVAHKKMMUFAY-UHFFFAOYSA-N oxosilver Chemical compound [Ag]=O OTCVAHKKMMUFAY-UHFFFAOYSA-N 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- ONFQTORHROMJSV-UHFFFAOYSA-N 5-(2-amino-5,6-dimethyl-1H-benzimidazol-1-yl)pentanoic acid Chemical compound C1=C(C)C(C)=CC2=C1N(CCCCC(O)=O)C(N)=N2 ONFQTORHROMJSV-UHFFFAOYSA-N 0.000 description 1
- 241001269238 Data Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 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
- 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
- 238000010586 diagram Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement 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
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 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, more particularly to a kind of preparation method of micro-sized metal powder.
Background technology
The industries such as metal dust is manufactured in the electronic component of electronics industry, plating, battery and chemical industry catalysis, jewellery have extensively
General application.As electronic component is to miniaturization and the development in high-performance direction, sintering activity, dispersiveness to metal dust,
The performance indications such as sphericity, crystallinity propose requirement higher.At present, the preparation method of metal dust include physical method and
Chemical method, physical method including atomization, gas evaporation condensation method, polishing etc., chemical method mainly include liquid phase reduction,
Electrochemical deposition method, electrolysis etc..Because there is high cost low-yield, very widely used today chemical liquid phase in Physical
Reducing process, i.e., be reduced to metal, such as CN1301205, powder by salting liquid or oxide containing metal by the reaction that chemically reacts
It is last metallurgical with sintering activity metal dust and alloy end method with and its preparation method and application.Chinese patent application
CN101597777 discloses one kind by containing metal oxide or salt, and the method for metal is reduced into using electrolysis mode.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of system of the metal micro level powder different from prior art
Preparation Method.
In order to solve the above-mentioned technical problem, the technical scheme is that using nanosized seeds induction production metal dust
A kind of preparation method, its feature is that it comprises the following steps：
(1) preparation of oxidizing agent solution, metal nitrate or sulfate solid is dissolved in deionized water, or added
Ammoniacal liquor produces complexing metal ammonium salt solution, keeps [metal ion] concentration=0.1~5 mol/L in oxidizing agent solution, is sufficiently stirred for
10~50 DEG C of temperature constant states are kept afterwards；
(2) reductant solution is prepared, and one or more hydroxylamine compound solid or vitamin C are added in deionized water
Or formaldehyde or hydrazine hydrate reduction agent dissolving are made, and keep [reducing agent] concentration=0.1~5 mol/L in reductant solution, reduction
Agent solution volume is 0.5~2 times of oxidizing agent solution volume, and 10~50 DEG C of temperature constant states are kept after being sufficiently stirred for；
(3) dispersant solution prepare, one or more dispersant is added in deionized water, above-mentioned dispersant go from
Gross mass in sub- water is 0.1~2 times of aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality, straight after being sufficiently stirred for
Addition metal nano crystal seed is connect, or adds one or more metal nitrate or metal sulfate or metal oxide fully to stir
10~50 DEG C of temperature constant states are kept after mixing；
(4) preparation of flocculant, the oleic acid and reaction for weighing reaction generation metal dust quality 0.05%~0.5% is generated
One or more oleate of metal powder quality 0.05%~0.5%, adds them into and is added in flocculating agent formulation tank on a small quantity
After alcohol dissolves each other；
(5) before reaction starts, the dispersant solution for preparing is previously added in a kettle., open stirring, then simultaneously
Constant flow adds oxidizing agent solution and reductant solution, and flow is：0.1L~20L/Min；Initial reaction stage, using what is be previously added
A large amount of dispersants suppress the reunion of nano metal particles and the effect of the newborn nano metal particles of stabilization in dispersant solution, from
And the generation of metallic particles is controlled by the use of the quantitative nano metallic particles of existing or new life as crystal seed in reaction system, reach
To size tunable reduction grow system, while played in remaining course of reaction good redox rate and nucleus into
The control of speed long；
(6) react after the completion of, solution in reactor is entered in flocculation sediment kettle, add flocculant, quickly stir 5~
The metal ball shaped and spherical powder of isolated various different-grain diameter scopes is staticly settled after 30min.
In the preferred technical solution of the present invention, reducing agent is selected from azanol, sulfuric acid during step (2) reductant solution is prepared
Azanol, HAN, vitamin C, 37%~40% formalin, one or more mixing of hydrazine hydrate, reduction
Agent is in the solution with the metal ion mol ratio in abovementioned steps (1)：[metal ion]:[azanol]=1:0.1~5, or [gold
Category 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 poly- second
Glycol 400, or polysorbate40, or glycerine are added in the deionized water of 0.5~2 times of foregoing reductant solution volume, above-mentioned point
Powder gross mass in deionized water is 0.1~2 times of aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality, is filled
Divide aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate quality are added after stirring 0.01%~1.0% one kind or many
Metal nitrate or sulfate or metal oxide are planted, or is directly added into aforementioned oxidizer GOLD FROM PLATING SOLUTION genus nitrobacter or sulfate
The nano-metal particle of the 0.01%~0.5% of quality, keeps 10~50 DEG C of temperature constant states after being sufficiently stirred for；The step is using certainly
The a large amount of dispersants of body initial reaction stage suppress the reunion of nano metal particles and the effect of the newborn nano metal particles of stabilization, so that
There is quantitative nano-metal particle in reaction system and controlled as crystal seed the generation of metallic particles, reach size tunable
Reduction growth system, plays the control of good redox rate and nucleus growth rate during the course of the reaction.
In the preferred technical solution of the present invention, nanosized seeds can be from power during step (3) dispersant solution is prepared
Profit requires step described in 1 (5) in initial reaction stage using one or more metallic salt in the dispersant solution being previously added
Or metal oxide is reduced and the nano metal particles of new life are pre-added to the slaine in dispersant solution as crystal seed
Or metal oxide gross mass is 0.01% of metal nitrate or metal sulfate quality in the step (1) oxidizing agent solution
~1.0%.
In the preferred technical solution of the present invention, nanosized seeds are to be directly added into during step (3) dispersant solution is prepared
Nano-metal particle as crystal seed, add nano-metal particle quality be in step (1) oxidizing agent solution metal nitrate or
The 0.01%~0.5% of sulfate quality.
In the preferred technical solution of the present invention, the preparation of the flocculant of the step (4), the oleate is selected from unsaturation
Aliphatic acid and its ammonium salt.
In the preferred technical solution of the present invention, in step (5), the pressure produced using pump or compressed air is fixed by micropore
Be added to the mode of two kinds of oxidizing agent solutions for preparing of abovementioned steps and reductant solution constant flow in reactor by amount, two kinds
The flow-control scope of solution is 0.1L/min~20L/min, and is reacted under vigorous stirring, mixing speed：200rpm~
500rpm, is separated by flocculation sediment and obtains all kinds of ball-types and class ball-type metal powder again after reaction completely.
In the preferred technical solution of the present invention, in step (6), flocculant rapid loading side is used during flocculation sediment
Formula, addition speed is 1L/min~10L/min, and strong agitation, mixing speed 200rpm~500rpm, is sufficiently stirred for 5~30
After minute, the metal ball shaped and spherical powder of isolated various different-grain diameter scopes is staticly settled.
In the preferred technical solution of the present invention, metal includes silver, copper, nickel.
In the preferred technical solution of the present invention, the metal dust is spherical and spherical micron particles.
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 of reaction, when
Right too high or too low the carrying out for being all unfavorable for reaction.Dispersant solution in the present invention, according to the production of different metal powder diameter
It is required that in the newborn nano-metal particle of initial reaction stage or the content of the nano-metal particle being directly added into, life in regulation dispersant
The micro-sized metal powder product of different-grain diameter is produced, nano-metal particle content is the 0.01% of reaction production metal dust quality
When~0.4%, the silver powder particle diameter for being produced is bigger than normal, and D50 is between 1.0um~2.5um；Nano-metal particle content is given birth to for reaction
When pan belongs to the 0.4%~1% of powder quality, the metal particle diameter for being produced is less than normal, and D50 is between 0.2um~1.0um；Therefore
Nano-metal particle content can be adjusted in production process according to the Particle size requirements of the metal dust of specific production.
The advantages of the present invention are：
(1) nanosized seeds are introduced in the dispersant solution of the inventive method, so that metal ion is in reduction process
Size tunable, can with fast and stable from metal salt solution containing ammonia complexing or containing in metal nitrate or metallic sulfate-containing by gold
Category particle, such as silver ion reduction ensure that formed morphologies can pass through for ball-type or class ball-type and particle diameter into silver powder
Nanosized seeds quantity is introduced to be adjusted.
(2) feed postition is effectively controlled while the method for the present invention uses constant flow oxidizing agent solution and reductant solution
Metal dust dispersiveness during the course of the reaction is made, existing metal dust has been solved, such as reunion in silver powder production process has been asked
Topic, and metal dust average grain diameter is 0.1um~10um.
(3) inventive method can effectively control metal ball shaped and spherical powder reaction rate in process of production,
There is good control to nucleus growth speed and dispersiveness, the spherical and spherical metal dust for being produced has extraordinary
Crystallinity, sphericity, jolt ramming high and polymolecularity.
(4) preparation method of the invention can apply to industrialized production, and large-scale production is by taking silver powder as an example：Can reach 5-
150kg/ batches, 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, and reaction is complete, produces between product batches
Steady quality, so as to greatly reduce product disqualification rate, considerable economic benefit is brought to enterprise.
Brief description of the drawings
Fig. 1 is the flow chart of the method for the present invention.
The droplet measurement schematic diagram of the metal dust that Fig. 2A, 2B, 2C are prepared for the inventive method.
The SEM electron microscopic figures of the ball shape silver powder that Fig. 3 is prepared for the inventive method, wherein, Fig. 3 A are put for SEM Electronic Speculum
Ball shape silver powder figure greatly × 10000 times, Fig. 3 B are the ball shape silver powder figure that SEM Electronic Speculum amplifies × 10000 times, and Fig. 3 C are SEM Electronic Speculum
Amplify × 5000 times of ball shape silver powder figure, Fig. 3 D are the ball shape silver powder figure that SEM Electronic Speculum amplifies × 5000 times, and Fig. 3 E are SEM Electronic Speculum
Amplify × 5000 times of ball shape silver powder figure, Fig. 3 F are the ball shape silver powder figure that SEM Electronic Speculum amplifies × 2000 times.
Specific embodiment：
To further understand the present invention, preferred scheme of the present invention is described with reference to specific embodiment, but should
Work as understanding, these descriptions are simply to further illustrate the features and advantages of the present invention, rather than the limit to the claims in the present invention
System.
Embodiment 1
(1) oxidizing agent solution containing silver nitrate solution is prepared, and the silver nitrate liquid of nitric acid silver salt solid or equivalent is molten
Solution keeps silver ion molar concentration [silver ion]=0.5mol/l in solution in deionized water, and ammonia is added after being sufficiently stirred for
Water (20%), pH is between 2.5~9.5 for regulation, keeps 10~50 DEG C of temperature constant states of solution；
(2) reductant solution containing hydrazine hydrate is prepared, and adds hydrazine hydrate solution to be made in deionized water, according to argentiferous oxygen
Silver content in agent solution, keeps mol ratio [silver ion] in solution:[hydrazine hydrate]=1:0.1~5, keep solution 10~50
DEG C temperature constant state；
(3) dispersant solution is prepared：One or more polysorbate40 or PEG400 is added in deionized water
Dissolving is made, and its content is 20~100g/l, is sufficiently stirred for, and is subsequently adding nano metal Argent grain (100nm~200nm)
0.01-0.05g, keeps 10~50 DEG C of temperature constant states of solution；
(4) dispersant solution containing polysorbate40 or PEG400 compound is squeezed into reactor in advance using measuring pump,
Then metered injection is carried out with the reductant solution containing hydrazine hydrate by the quantitative oxidizing agent solution that will contain ammonia complexing silver of micropore to arrive
(flow is in reactor：0.1L~20L/Min)；(300rpm) reduction reaction, passes through to add after the completion of reaction under vigorous stirring
Enter the silver powder that flocculant precipitate and separate obtains various different-grain diameter scopes.
Embodiment 2
Oxidizing agent solution is prepared：The silver nitrate solution 500ml of argentiferous 200g/L is prepared in 2000ml wide-mouth bottles, thereto
The ammoniacal liquor 200ml for adding mass percentage concentration to be 20%, obtains silver ammino solution, and it is standby to be heated to 45 DEG C of constant temperature,
Reductant solution is prepared：Prepared in another 2000ml wide-mouth bottles and contain vitamin c solution and HAS：By 50g
HAS and 50g vitamin Cs are dissolved into 500ml deionized waters, and it is standby to be heated to 45 DEG C of constant temperature,
Dispersant solution is prepared：The dispersant solution prepared in 500ml wide-mouth bottles：85gPVP and 50ml polysorbate40s is molten
Solution in 300ml deionized waters, add 1g silver oxides, be heated to 45 DEG C it is standby,
Dispersant solution is squeezed into 5000ml wide-mouth bottles in advance using measuring pump, then quantitatively simultaneously will be upper by micropore
State two kinds of oxidizing agent solutions for preparing and reductant solution carries out dropwise addition mixing, two kinds of streams of solution in 5000ml wide-mouth bottles
Amount is controlled to 250ml/min, and starts stirring, and stir speed (S.S.) 400rpm after reaction terminates, adds flocculant, stirs 10 minutes
The silver powder for separating and obtaining that spherical or spherical average grain diameter is 0.1um~10um is staticly settled afterwards.
Embodiment 3
The copper-bath 650ml of cupric 300g/L is prepared in 2000ml wide-mouth bottles, quality percentage is charged with dense
The ammoniacal liquor 350ml for 20% is spent, copper ammon solution is obtained, 35 DEG C are heated to,
The reductant solution containing azanol is prepared in another 2000ml wide-mouth bottles：By 150g azanols be dissolved into 1000ml go from
In sub- water, 35 DEG C are heated to,
The dispersant solution prepared in 500ml wide-mouth bottles：25gPVP is dissolved in 250ml deionized waters, 1g is added
Copper nanoparticle, is heated to 35 DEG C,
Dispersant solution is squeezed into 5000ml wide-mouth bottles in advance using measuring pump, then passes through measuring pump by above two
The copper ammon solution and hydroxylamine solution for preparing carry out injection mixing, two kinds of injection flow controls of solution in 5000ml wide-mouth bottles
It is 500ml/min, and starts stirring, stir speed (S.S.)：400rpm, ball is obtained after reaction completely by adding flocculant precipitate and separate
Shape or spherical copper powder.
Embodiment 4：Batch production
135 kilograms of silver nitrate solids, plus deionization 800L are added in the preparing tank of 1000L, it is past after being sufficiently stirred for dissolving
The ammoniacal liquor 250L that mass percentage concentration is 15% is wherein added, silver ammino solution is obtained, 35 DEG C standby (oxidizing agent solution) is heated to,
500L deionized waters are added in the preparing tank of another 1000L, 50 kilograms of vitamin Cs and 5 kilograms of nitre are subsequently added
35 DEG C standby (reductant solution) is heated to after sour azanol, fully dissolving,
50kg PVP are dissolved in 400L deionized waters in 500L preparing tanks, add 5kg polyethylene glycol, be sufficiently stirred for
Nano-Ag particles 500g is added afterwards, is heated to 35 DEG C standby (dispersant solution),
Dispersant solution is squeezed into 3000L reactors in advance using measuring pump, then by micropore quantitatively by above-mentioned two
The oxidizing agent solution and reductant solution that kind is prepared carry out injection mixing, two kinds of injection flows controls of solution in retort
It is 5L/min, and starts stirring, stir speed (S.S.) 120rpm is added dropwise dispersant solution during the course of the reaction, after reaction completely, will be anti-
Answer liquid to be drained into 5000L flocculation sediment kettles, add flocculant, open stirring, stir speed (S.S.) 300rpm is quickly sufficiently stirred for 30
After minute, the silver powder for separating and obtaining that spherical or spherical average grain diameter is 0.1um~10um is staticly settled.
If Fig. 1 is three groups of detection datas of silver powder that invention according to the present invention is prepared：
And the electron microscope of silver powder S001 is 3A and 3D, the electron microscope of silver powder S002 is 3B and 3E, the electron microscope of silver powder S003
It is 3C and 3F.
Technology contents of the invention and technical characteristic have revealed that as above, but those of ordinary skill in the art still may base
Make a variety of replacements and modification without departing substantially from spirit of the present invention in teachings of the present invention and announcement, therefore, the scope of the present invention
Should be not limited to the content disclosed in embodiment, and should include various without departing substantially from replacement of the invention and modification, and be this patent Shen
Please claim covered.
Claims (11)
1. a kind of utilization nanosized seeds induction produces the preparation method of metal dust, it is characterised in that it comprises the following steps：
(1) preparation of oxidizing agent solution, metal nitrate or sulfate solid is dissolved in deionized water, or add ammoniacal liquor
Generation complexing metal ammonium salt solution, keeps concentration of metal ions=0.1~5 mol/L in oxidizing agent solution, is protected after being sufficiently stirred for
Hold 10~50 DEG C of temperature constant states；
(2) reductant solution is prepared, and one or more hydroxylamine compound solid or vitamin C or first are added in deionized water
Aldehyde or hydrazine hydrate reduction agent dissolving are made, and keep reductant concentration=0.1~5 mol/L in reductant solution, and reducing agent is molten
Liquid product is 0.5~2 times of oxidizing agent solution volume, and 10~50 DEG C of temperature constant states are kept after being sufficiently stirred for；
(3) dispersant solution is prepared, by one or more dispersant, polyvinylpyrrolidone PVP or PEG400 or tween
40 or glycerine be added in deionized water, above-mentioned dispersant gross mass in deionized water is aforementioned oxidizer GOLD FROM PLATING SOLUTION
0.1~2 times of genus nitrobacter or sulfate quality, added after being sufficiently stirred for nano metal crystal seed or add oxidizing agent solution in
One or more metal nitrate or sulfate or the metal oxidation of the 0.01%~1.0% of metal nitrate or sulfate quality
The mixture of thing, keeps 10~50 DEG C of temperature constant states after being sufficiently stirred for；
(4) preparation of flocculant, weighs the oleic acid or reaction generation metal of reaction generation metal dust quality 0.05%~0.5%
One or more oleate of powder quality 0.05%~0.5%, adds them into and a small amount of wine is added in flocculating agent formulation tank
After essence is dissolved each other；
(5) before reaction starts, the dispersant solution for preparing is previously added in a kettle., open stirring, then constant current simultaneously
Addition oxidizing agent solution and reductant solution are measured, flow is：0.1L~20L/Min；Initial reaction stage, using the dispersion being previously added
A large amount of dispersants suppress the reunion of the nano metal particles being added directly into dispersant solution and stablize by reacting in agent solution
The effect of the nano metal particles of initial stage new life, so as to the quantitative nano metal in whole reaction system using existing or new life
Particle controls the generation of metallic particles as crystal seed, the reduction growth system of size tunable is reached, while during the course of the reaction
Play the control of good redox rate and nucleus growth rate；
(6) react after the completion of, solution in reactor is drained into flocculation sediment kettle, add flocculant, quickly stir 5~
The ball-type or class ball-type metal dust of isolated various different-grain diameter scopes are staticly settled after 60min.
2. preparation method according to claim 1, it is characterised in that step (2) reductant solution is reduced in preparing
Agent be selected from azanol, HAS, HAN, vitamin C, 37%~40% formalin, hydrazine hydrate one or two
More than mixture, reducing agent is in the solution with the metal ion mol ratio in abovementioned steps (1)：[metal ion]:[hydroxyl
Amine]=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 being sufficiently stirred for.
3. preparation method according to claim 1, it is characterised in that step (3) dispersant solution disperses in preparing
One or more dispersant is selected in agent：Polyvinylpyrrolidone PVP, or PEG400, or polysorbate40, or glycerine are added
To in the deionized water of 0.5~2 times of the reductant solution of step (2) described in preceding claims 1 volume, above-mentioned dispersant is going
Gross mass in ionized water is that metal nitrate or sulfate are total in the oxidizing agent solution of step (1) described in preceding claims 1
0.1~2 times of quality, keeps 10~50 DEG C of temperature constant states after being sufficiently stirred for.
4. preparation method according to claim 1, it is characterised in that step (3) dispersant solution prepare in nanometer
Crystal seed can select step (5) described in claim 1 in initial reaction stage using the one kind in the dispersant solution being previously added
Or the mixture of two kinds of metallic salts or metal oxide is reduced and the nano metal particles of new life are previously added as crystal seed
One or more slaine or metal oxide gross mass in dispersant solution are gold in the step (1) oxidizing agent solution
The 0.01%~1.0% of genus nitrobacter or sulfate quality.
5. preparation method according to claim 1, it is characterised in that step (3) dispersant solution prepare in nanometer
From nano-metal particle is directly added into as crystal seed, it is that step (1) oxidant is molten to add nano-metal particle quality to crystal seed
The 0.01%~0.5% of metal nitrate or sulfate quality in liquid.
6. the preparation method according to claim 4 or 5, it is characterised in that using in initial reaction stage dispersant solution in advance
One or more metal nitrate or metal sulfate or metal oxide for adding first react raw with the reductant solution for adding
The metal nanoparticle of product is used as crystal seed, and the particle diameter of these newborn nano-metal particles is 1nm~800nm；Or it is straight
Connect and add the metallic particles of nanometer particle size to be used as crystal seed, the particle diameter of the nano-metal particle being directly added into for 1nm~
800nm。
7. preparation method according to claim 1, it is characterised in that the oleate choosing in the flocculant of the step (4)
From unrighted acid and its ammonium salt.
8. preparation method according to claim 1, it is characterised in that in the step (5), is produced using pump or compressed air
Raw pressure is by the quantitative oxidizing agent solution and reductant solution constant flow for preparing middle step (1) and step (2) of micropore
Mode be added in reactor, two kinds of flow-control scope 0.1L/min~10L/min of solution, and anti-under vigorous stirring
Should, mixing speed：200rpm~500rpm, is separated by flocculation sediment and obtains all kinds of ball-types or class ball-type gold again after reaction completely
Category powder.
9. preparation method according to claim 1, it is characterised in that in the step (6), used in flocculation sediment kettle
Quick blowing mode adds flocculant, and additions speed is 1L/min~10L/min, and strong agitation, and mixing speed 200rpm~
500rpm, after being sufficiently stirred for 5~60 minutes, staticly settles the metal ball shaped and spherical of isolated various different-grain diameter scopes
Powder.
10. preparation method according to claim 1, it is characterised in that the metal includes silver, copper, nickel.
11. preparation methods according to claim 1, it is characterised in that the metal dust is spherical and spherical micron
Grade particles.
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| CN105880586B (en) * | 2016-04-19 | 2017-12-19 | 南京农业大学 | A kind of Au/Ag/Au core-shell nanos antibacterial material and preparation method thereof |
| CN105834449B (en) * | 2016-05-04 | 2017-09-22 | 苏州思美特表面材料科技有限公司 | It is a kind of that the preparation method for producing silver powder is induced by the use of micro-nano bubble as crystal seed |
| CN105903980A (en) * | 2016-05-16 | 2016-08-31 | 深圳市微纳集成电路与***应用研究院 | Copper nanometer powder and preparation method thereof as well as silver-coated copper powder and preparation method thereof |
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| US20060090597A1 (en) * | 2004-10-29 | 2006-05-04 | Goia Dan V | Polyol-based method for producing ultra-fine metal powders |
| CN101337276A (en) * | 2008-08-07 | 2009-01-07 | 吴建国 | Preparation method of silver particulate solution of high dispersion and antioxidation |
| CN102248177B (en) * | 2011-07-29 | 2012-12-12 | 上海龙翔新材料科技有限公司 | Laser-induced method for preparing spherical silver powder |
| CN102343441A (en) * | 2011-09-22 | 2012-02-08 | 上海交通大学 | Method for preparing monodispersed silver powder with high tap density and low agglomeration |
| CN102941351B (en) * | 2012-11-27 | 2015-08-26 | 中国船舶重工集团公司第七一二研究所 | A kind of preparation method of superfine cupper powder |
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Application publication date: 20160330 Assignee: Suzhou Heyu Finance Leasing Co.,Ltd. Assignor: Yttrium Crystal Technology (Suzhou) Co.,Ltd. Contract record no.: X2024980000488 Denomination of invention: A preparation method for inducing the production of metal powder using nanocrystalline seeds Granted publication date: 20170517 License type: Exclusive License Record date: 20240115 |
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Denomination of invention: A preparation method for inducing the production of metal powder using nanocrystalline seeds Granted publication date: 20170517 Pledgee: Suzhou Heyu Finance Leasing Co.,Ltd. Pledgor: Yttrium Crystal Technology (Suzhou) Co.,Ltd. Registration number: Y2024980004380 |