CN104551004B - The chemical preparation process of a kind of ferro-cobalt Nanoalloy powder body - Google Patents
The chemical preparation process of a kind of ferro-cobalt Nanoalloy powder body Download PDFInfo
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Abstract
The chemical preparation process of a kind of ferro-cobalt Nanoalloy powder body, it relates to prepare nano-powder material to chemical process. The present invention using hydrazine hydrate, POTASSIUM BOROHYDRIDE jointly as reductive agent, cobalt metal in specific solvent, iron ion are first reduced into the thick ferro-cobalt precursor of lightpink with hydrazine hydrate by the first step, ferro-cobalt precursor thick for lightpink is reduced to cobalt metal, iron atom by the solution of potassium borohydride that the 2nd step specific solvent dissolves, and atoms metal is assembled again, final acquisition ferro-cobalt Nanoalloy particle of growing up. Can this technique prepare the cobalt Nanoalloy powder that taps a blast furnace, and can realize the control of granule-morphology, the ferro-cobalt Nanoalloy particle of preparation, and in spherical, particle diameter is 50 ~ 800? nm, is evenly distributed, for the practical application of ferro-cobalt Nanoalloy powder body provides condition.
Description
Technical field
The present invention relates to chemical process and prepare nano-powder material, particularly relate to the preparation of a nanometer ferro-cobalt (CoFe) alloy powder.
Background technology
Nano material, because of the physics and chemistry character of the uniqueness such as small-size effect, surface effects, has a wide range of applications in fields such as energy and material, ecological environment material nd, functional coating material, high-performance electronic materials. CoFe alloy is a kind of metal soft magnetic material, is widely used in the functional element manufactures such as magnetic recording, sensor, ferrofluid. Meanwhile, the magnetic property of ferro-cobalt Nanoalloy powder body, catalytic performance and microwave absorbing characteristic etc. change with particle chemistry composition and the difference of grain size. Select certain preparation method, diameter of particle and the controlled alloy powder of chemical composition can be obtained, and then adjustment and the design magnetic of alloy powder, catalytic performance and microwave absorbing characteristic, there is extremely important meaning for the application and development of ferro-cobalt Nanoalloy powder body in fields such as thermotherapy, catalytic material and microwave absorbing materials.
Liquid phase reduction prepares nano material, is select suitable dissolution with solvents metal-salt, and adds a certain amount of reductive agent, metal-salt is reduced in liquid phase solvent, and through nucleation and growth two processes, finally forms nano material. Appropriate tensio-active agent is added during Liquid preparation methods nanoparticle, the tensio-active agent being adsorbed on particle surface can the organic coating layer of formative dynamics, slow down collision and the reunion of particle, strengthen the stability of particle, make nanoparticle keep stable monodisperse status and control its growth.
According to " PowderTechnology " 28 (2011) 623-627 report, preparing Fe-Co nano particle by the method for the reaction of self-propagating high-temperature in the process of ball milling, first the first stage loads cobalt chloride, iron(ic) chloride and a certain amount of sodium salt ion with 8000M steel ball and is connected with in the high energy ball mill of shielding gas argon gas and carries out ball milling; Subordinate phase, by adding different bright sodium-chlor in presoma good for first stage ball milling, carries out ball milling and probes into sodium-chlor to the impact of iron cobalt nano-particle shape looks and magnetic property. This method can prepare the iron cobalt Nanoalloy powder of different ratios, and it is also high to produce rate, but it is even not to prepare the nano particle shape, it is very difficult to prepares spherical nanoparticle.
According to " JournalofAppliedPhysics " 111,07B533 (2012) report, with Fe (CO)5And Co2(CO)8For presoma, preparing CoFe alloy nano particle by the method for thermolysis, concrete steps are solvent taking oleylamide, and is heated to 160 DEG C, by Co2(CO)8��Fe(CO)5Back flow reaction prepares Fe Co nano particle for one hour with being dissolved in oleylamide after the mixing of a certain amount of kerosene. In order to improve the saturation magnetization energy of Fe Co nano particle, the Fe Co nano powder prepared is carried out low-temperature annealing in a vacuum furnace. This method can prepare the Fe Co nano powder of higher saturation magnetization energy, but the size distribution of Fe Co nano powder is uneven, and equipment fraud valency height.
Report according to " MaterialsResearchBulletin " 48 (2013) 3,157 3163, preparing CoFe alloy nano particle taking 1-18 (carbon) alkene and oleic acid as the method for thermolysis in solvent, first utilize Iron trichloride hexahydrate (FeCl36H2O) and sodium oleate preparation tap a blast furnace and the complex compound of oleic acid, complex compound through separation, clean, after vacuum drying treatment, by oleic acid iron (Fe (C18H33O2)3) and CoCL2 6H2O (CoCl26H2O) regular hour is heated 120 DEG C and 317 DEG C when logical nitrogen taking a certain amount of 1-18 (carbon) alkene and oleic acid respectively as solvent, thus obtained CoFe alloy nano particle. This method can the CoFe alloy nano particle of different mol ratio of a step, but experimentation is complicated, long reaction time, limits its suitability for industrialized production.
According to " Vacuum " 101 (2014) 371-376 report; plasma sputtering method prepares Fe Co nano powder; first taking oxidized silicon as matrix; lead to into shielding gas argon gas in a vacuum furnace; and pressurize, in matrix sputtering precipitation, a certain proportion of iron and cobalt powder body are formed thickness is the film of 4nm to 10nm. Now carry out pre-treatment under the environment of exist at ask the visitor in plasma body 700 DEG C of Fe Co film, it is that film shape core grows up into nanometer Fe Co alloy particle. But the techniques such as the region supersaturation ratio that tiny nucleus is formed, air pressure, gaseous species and cooling conditions are the principal elements of impact nanometer performance, and equipment requirements is higher.
Report according to Yu Hongying, identical apply for a patent " chemical preparation process of a kind of cobalt nickel Nanoalloy powder body " of Lu ten thousand, using the one in hydrazine hydrate or sodium borohydride as reductive agent, the salts solution of reduction cobalt nickel, prepare in spherical, particle diameter is 50��700nm, the cobalt nickel hybrid alloys powder body being evenly distributed. This invented technology is easy, low raw-material cost, and can realize economic preparation in macroscopic quantity, but is only difficult to reduction by the one in hydrazine hydrate or sodium borohydride as reductive agent and prepares ferro-cobalt (CoFe) alloy powder. Prepare ferro-cobalt (CoFe) alloy powder to need to find suitable reductive agent, and adjust reductive agent add-on and sequentially could successfully prepare ferro-cobalt (CoFe) alloy powder, and control ferrocobalt powder shape looks and particle diameter.
Summary of the invention
It is an object of the invention to provide a kind of method adopting liquid-phase reduction to prepare ferro-cobalt Nanoalloy, using hydrazine hydrate, POTASSIUM BOROHYDRIDE jointly as reductive agent, cobalt metal in specific solvent, iron ion are first reduced into the thick ferro-cobalt precursor of lightpink with hydrazine hydrate by the first step, ferro-cobalt precursor thick for lightpink is reduced to cobalt metal, iron atom by the solution of potassium borohydride that the 2nd step specific solvent dissolves, and atoms metal is assembled again, final acquisition ferro-cobalt Nanoalloy particle of growing up. This technique can not only prepare the cobalt Nanoalloy powder that taps a blast furnace, and can realize the control of granule-morphology, for the practical application of ferro-cobalt Nanoalloy powder body provides condition.
The implementation process of the present invention is as follows:
The preparation of step 1. reaction soln:
1.1) preparing metal salts solution: taking ethylene glycol, deionized water as solvent, in metal salt solution 0.01��3.00mol/L, the preparation of tensio-active agent 0.10��25.00g/L ratio; Temperature is between 20��30 DEG C, stirs 20��30 minutes, and wherein in metal salt solution, the stoichiometric ratio of Co/Fe is between 0.10��16.00;
1.2) reductant solution is prepared 1.: taking ethylene glycol, deionized water as solvent, potassium hydroxide 0.20��6.00mol/L dissolves, and adds hydrazine hydrate 2.00��32.00mL, and temperature is between 20��30 DEG C, stirs 20��30 minutes;
1.3) preparing reductant solution 2.: taking ethylene glycol, deionized water as solvent, potassium hydroxide dissolves, and adds POTASSIUM BOROHYDRIDE or sodium borohydride; Temperature is between 20��30 DEG C, stirs 20��30 minutes; Potassium hydroxide add-on is 0.20��6.00mol/L; POTASSIUM BOROHYDRIDE or sodium borohydride add-on are 0.67g��5.40g/L.
The preparation of step 2. nanometer ferro-cobalt powder:
1., 2. metal salt solution step 1 prepared and reductant solution distinguish heating in water bath to 60��100 DEG C, then first 1. join in the metal salt solution of cobalt metal, iron ion with reductant solution, react 20��30 minutes, until cobalt metal, iron ion are reduced into the thick ferro-cobalt precursor of lightpink; 2. join in the thick ferro-cobalt precursor of lightpink with reductant solution again, react 20��30 minutes, until reacting complete, then centrifugation solution and ferro-cobalt Nanoalloy powder body, again successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 2��3 times, collect after dry.
Metal-salt used is CoCl2/FeCl2��CoSO4/FeSO4Or Co (NO3)2/Fe(NO3)3Among any one.
Reductive agent used is hydrazine hydrate (N2H4��H2And POTASSIUM BOROHYDRIDE (KBH O)4) or hydrazine hydrate (N2H4��H2And sodium borohydride (NaBH O)4) two groups in arbitrary group.
Described tensio-active agent is any one among polyvinylpyrrolidone (PVPK30), polyvinylpyrrolidone (PVPK15), sodium laurylsulfonate (SDS), CETRIMIDE POWDER (CTAB).
It is characteristic of the invention that the size that can be adjusted product by the change technological factor such as adding of the kind of metal salt concentrations, reductive agent add-on, reductive agent addition sequence, solvent, temperature of reaction, reaction times, tensio-active agent; Controlled the Co/Fe stoichiometric ratio of product by the Co/Fe stoichiometric ratio in initial salt, namely control the composition of CoFe Nanoalloy powder body.
Compared with prior art, technological process of the present invention is simple, and reaction conditions is gentle, preparation cost is cheap, therefore, it is possible to realize preparation in macroscopic quantity. Particularly by the change of processing condition, such as the interpolation etc. of metal salt concentrations, reductive agent add-on, tensio-active agent, it is possible to realize the controlling and adjustment to ferro-cobalt Nanoalloy diameter of particle size; Meanwhile, also by adjustment reactant in ferro-cobalt metal ingredient than realizing the controlling and adjustment to product component. Adopting ferro-cobalt Nanoalloy particle prepared by the present invention, in spherical, particle diameter is 50��800nm, is evenly distributed, and its shape looks are shown in Fig. 1��Fig. 8. The powder body prepared is ferro-cobalt hybrid alloys powder body, and its material phase analysis is such as Fig. 9.
Accompanying drawing explanation
Fig. 1 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 1;
Fig. 2 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 2;
Fig. 3 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 3;
Fig. 4 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 4;
Fig. 5 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 5;
Fig. 6 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 6;
Fig. 7 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 7;
Fig. 8 is ferro-cobalt Nanoalloy powder body FESEM photo prepared by embodiment 8;
Fig. 9 is ferro-cobalt Nanoalloy powder body XRD figure spectrum prepared by embodiment 8.
Embodiment
Embodiment 1:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) the solution heating in water bath to 60 DEG C respectively that will prepare as stated above;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 74nm. Its shape looks are as shown in Figure 1.
Embodiment 2:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) the solution heating in water bath to 90 DEG C respectively that will prepare as stated above;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 187nm. Its shape looks are as shown in Figure 2.
Embodiment 3:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking water.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking water.
2) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking water.
2, the preparation of ferro-cobalt nano particle:
(1) solution prepared as stated above is heated to 70 DEG C respectively;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 173nm. Its shape looks are as shown in Figure 3.
Embodiment 4:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) solution prepared as stated above is heated to 80 DEG C respectively;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 62nm. Its shape looks are as shown in Figure 4.
Embodiment 5:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) solution prepared as stated above is heated to 80 DEG C respectively;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 371nm. Its shape looks are as shown in Figure 5.
Embodiment 6:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) solution prepared as stated above is heated to 100 DEG C respectively;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 645nm. Its shape looks are as shown in Figure 6.
Embodiment 7:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) solution prepared as stated above is heated to 95 DEG C respectively;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 736nm. Its shape looks are as shown in Figure 7.
Embodiment 8:
1, the preparation of reaction soln:
1) preparation of metal salt solution:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2) reductant solution preparation 1.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
3) reductant solution preparation 2.:
It is that solvent is in following ratio obtain solution taking ethylene glycol.
2, the preparation of ferro-cobalt nano particle:
(1) solution prepared as stated above is heated to 90 DEG C respectively;
(2) 1. reductant solution is added dropwise in metal salt solution;
(3) react 20��30 minutes, until lightpink sticky mass occurs;
(4) 2. reductant solution is added dropwise in the thick precursor of lightpink;
(5) react 20��30 minutes, until reacting completely;
(6) centrifugation solution and ferro-cobalt Nanoalloy powder body;
(7) successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 3 times;
(8) dry collection.
Obtaining powder body spherical in shape, be evenly distributed, median size is 897nm. Its shape looks are as shown in Figure 8. Its XRD figure is composed as shown in Figure 9.
Claims (3)
1. the chemical preparation process of a ferro-cobalt Nanoalloy powder body, it is characterised in that, concrete steps are as follows:
1) preparation of reaction soln
A) preparing metal salts solution: taking ethylene glycol or deionized water as solvent, in metal salt solution 0.01��3.00mol/L, the preparation of tensio-active agent 0.10��25.00g/L ratio; Temperature is between 20��30 DEG C, stirs 20��30 minutes, and wherein in metal salt solution, the stoichiometric ratio of Co/Fe is between 0.10��16;
B) reductant solution is prepared 1.: taking ethylene glycol or deionized water as solvent, potassium hydroxide 0.20��6.00mol/L dissolves, and adds hydrazine hydrate 2.00��32.00mL, and temperature is between 20��30 DEG C, stirs 20��30 minutes;
C) reductant solution is prepared 2.: taking ethylene glycol or deionized water as solvent, potassium hydroxide 0.20��6.00mol/L dissolves, and adds POTASSIUM BOROHYDRIDE or sodium borohydride 0.67��5.40g/L; Temperature is between 20��30 DEG C, stirs 20��30 minutes;
2) preparation of nanometer ferro-cobalt powder
1., 2. metal salt solution step 1 prepared and reductant solution distinguish heating in water bath to 60��100 DEG C, then first 1. join in the metal salt solution of cobalt metal, iron ion with reductant solution, react 20��30 minutes, until cobalt metal, iron ion are reduced into the thick ferro-cobalt precursor of lightpink; 2. join in the thick ferro-cobalt precursor of lightpink with reductant solution again, react 20��30 minutes, until reacting complete, then centrifugation solution and ferro-cobalt Nanoalloy powder body, again successively with deionized water, acetone, absolute ethanol washing ferro-cobalt Nanoalloy powder body 2��3 times, collect after dry.
2. the chemical preparation process of ferro-cobalt Nanoalloy powder body as claimed in claim 1, it is characterised in that, described metal-salt is CoCl2/FeCl2��CoSO4/FeSO4With Co (NO3)2/Fe(NO3)3Among any one.
3. the chemical preparation process of ferro-cobalt Nanoalloy powder body as claimed in claim 1, it is characterized in that, described tensio-active agent is any one among polyvinylpyrrolidone PVPK30, polyvinylpyrrolidone PVPK15, sodium laurylsulfonate SDS, CETRIMIDE POWDER CTAB.
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