CN100457340C - Prepn process of monodisperse nanometer Fe-Pt alloy particle - Google Patents
Prepn process of monodisperse nanometer Fe-Pt alloy particle Download PDFInfo
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- CN100457340C CN100457340C CNB2006100291888A CN200610029188A CN100457340C CN 100457340 C CN100457340 C CN 100457340C CN B2006100291888 A CNB2006100291888 A CN B2006100291888A CN 200610029188 A CN200610029188 A CN 200610029188A CN 100457340 C CN100457340 C CN 100457340C
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Abstract
The present invention relates to material technology, and is especially preparation process of monodisperse nanometer Fe-Pt alloy particle. The reaction precursor of Pt containing inorganic salt or complex and Fe containing inorganic salt or complex, organic solvent and phase catalyst diphenyl crown ether are reacted to produce phase transfer and coreduction of the precursor inside a high pressure autoclave with oleic acid as stabilizer at 120-150 deg.c for 8-15 hr, so as to form the monodisperse nanometer Fe-Pt alloy particle of particle size 2-15 nm. The said process has controllable and narrowly distributed particle size, stable reaction system, simple operation, convenient product treatment, low cost and easy industrial application.
Description
Technical field
The invention belongs to the material technology field, be specifically related to a kind of monodisperse iron platinum alloy nanometer particle process method.
Background technology
L1
0The ferroplatinum of structure has very high each diversity of single shaft magnetocrystalline, is very suitable for preparing the super-high density magnetic storage medium material, therefore aspect magnetic recording media and the microdevice good application prospects is being arranged.And compare with pure platinum, ferroplatinum has more superior electrochemical catalysis activity in the methyl alcohol sulfuric acid system.Like this, the development to ferroplatinum material with certain pattern and specific dimensions becomes new magnetic material key in application problem.And the iron platinum particulate with nano-scale can show character, the particularly giant magnetoresistance effect of ferroplatinum film such as more outstanding electrochemistry, magnetics, optics behind the ordered arrangement that carries out two dimension on the microcosmic.
Nano material has the not available unusual or unusual physics of traditional material, chemical characteristic, can produce four big effects: small-size effect, quantum effect (containing macro quanta tunnel effect), skin effect and interfacial effect.The method that wet chemical prepares the monodispersity ferroplatinum in the bibliographical information is mainly sol-gal process.This method is based on mainly that acetyl acetone platinum reduces, simultaneously iron pentacarbonyl decomposes two fundamental reactions in pyrosol in long chain diol.The liquid phase coreduction alloy preparation method of acetyl acetone platinum and frerrous chloride or acetyl acetone platinum and acetyl acetone iron has been proposed again in recent years.These methods all in various degree all have equipment, a specification requirement harshness, prices of raw and semifnished materials costliness, cost height, and iron pentacarbonyl has severe toxicity, has very big problems such as danger.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of easy to operate, manageable monodisperse nanometer Fe-Pt alloy.
The preparation method of the monodisperse nanometer Fe-Pt alloy that the present invention proposes, with platiniferous inorganic salts/contain platinum complex, iron content inorganic salts/contain iron complex as pre-reaction material, pre-reaction material, organic solvent, phase catalyst hexichol crown ether are placed in the autoclave, under 120-150 ℃ of temperature, utilize the phase transfer between the reactant and the coreduction of pre-reaction material, with oleic acid as stabilizing agent, reacted 8-15 hour, and made required product, its particle diameter is 2-15nm.
The preparation method of the monodisperse nanometer Fe-Pt alloy that the present invention proposes, its concrete steps are as follows:
(1) with the platiniferous inorganic salts or contain platinum complex and iron content inorganic salts or contain iron complex as pre-reaction material, be dissolved in respectively in the organic solvent, add an amount of enuatrol solid and phase catalyst hexichol crown ether, ultrasonic processing 8-15 minute; Platiniferous inorganic salts or contain platinum complex and iron content inorganic salts or the mol ratio that contains iron complex are 1: 1～1: 4, enuatrol and iron content inorganic salts or contain iron complex and platiniferous inorganic salts or the mol ratio that contains the total amount of substance of platinum complex are 5: 1～10: 1, the mol ratio of hexichol crown ether and molysite and the total amount of substance of platinum salt is 1: 30～1: 100; The mol ratio of organic solvent and molysite and the total amount of substance of platinum salt is 34: 1～85: 1;
(2) measure propylene glycol solution and mix, stir, make it abundant mixing, mixed solution is joined in the step (1) with oleic acid, join autoclave then together, reaction is 8-15 hour under 120-150 ℃ of temperature, washing, centrifugation promptly gets required product, and its particle diameter is 2-15nm; Wherein the volume ratio of propane diols and oleic acid is 2: 1～3: 1, the mol ratio of propane diols and molysite and the total amount of substance of platinum salt be 30: 1～--80: 1.
Among the present invention, described platiniferous inorganic salts be in chloroplatinic acid or the platinous chloride etc. any, contain platinum complex and be dichloride dicyan diphenyl and close in platinum (II) or the acetyl acetone platinum (II) etc. any, the iron content inorganic salts are frerrous chloride etc., contain iron complex and be in ferric oxalate, acetyl acetone iron (II) or the acetyl acetone iron (III) etc. any.
Among the present invention, described organic solvent is absolute ethyl alcohol or ethylene glycol etc.
Among the present invention, the stirring described in the step (2) is ultrasonic concussion or magnetic agitation etc.
Among the present invention, the centrifugation rotating speed is 3000-5000 rev/min described in the step (2), and the time is 10-20 minute.
The monodisperse nanometer Fe-Pt alloy particle that utilizes the present invention to prepare is applied to hard disk HAMR technology.Utilize the inventive method to prepare that monodispersity is good, the nanometer Fe-Pt particle of uniform particle diameter, thereby have excellent physicochemical property.For example aspect the lifting hard-disk capacity, Seagate Technology develops the HAMR technology.By return to zero with data record to the high stability medium, thereby improved memory space per square inch greatly, make the magnetic recording limit further surmount people's the imagination.
The inventive method is easy to operate, easy to control, and the product of preparing can be prepared alloy firm as LB, impregnating method by further operation.
The present invention has the following advantages:
1, this method can be controlled the particle diameter that forms nanometer Fe-Pt alloy particle, and the particle diameter narrow distribution, has very high practicality.
2, the reaction system that the present invention relates to is more stable relatively, and the technology operation more simply, particularly the product processing is convenient simple and direct, is easy to industrialization.
3, the present invention adopt iron platinum respectively simple inorganic salts as predecessor, make reducing agent with propane diols, reduce greatly than preparation method's cost of other reducing agents.
Description of drawings
The product TEM photo of Fig. 1 under the multiple of 100nm, obtaining among the embodiment 1.
The product TEM photo of Fig. 2 under the multiple of 50nm, obtaining among the embodiment 1.
The product TEM photo of Fig. 3 under the multiple of 100nm, obtaining among the embodiment 2.
The product TEM photo of Fig. 4 under the multiple of 50nm, obtaining among the embodiment 3.
The product TEM photo of Fig. 5 under the multiple of 100nm, obtaining among the embodiment 4.
The product TEM photo of Fig. 6 under the multiple of 50nm, obtaining among the embodiment 5.
The specific embodiment
The invention is further illustrated by the following examples.
Embodiment 1:
1,0.000031mol chloroplatinic acid and 0.0000625mol (1: 2) Iron dichloride tetrahydrate fully are dissolved in the absolute ethyl alcohol of 2ml together, add 0.1g enuatrol and 2mg hexichol crown ether, ultrasonic concussion 10 minutes.
2, accurately measure 3ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of step (1), and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 15 hours down at 120 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 5000 rev/mins centrifugal 10 minutes, promptly getting required product, its particle diameter is 10-15nm, final particle can be dispersed in absolute ethyl alcohol or the chloroform again.From Fig. 1, TEM electromicroscopic photograph shown in Figure 2, just can clearly see the existence of product.
Embodiment 2:
1,0.000031mol chloroplatinic acid and 0.000125mol (1: 4) ferric oxalate fully are dissolved in the absolute ethyl alcohol of 4ml together, add 0.1g enuatrol and 2mg hexichol crown ether, ultrasonic concussion 15 minutes.
2, accurately measure 2ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of the first step, and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 10 hours down at 140 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 3500 rev/mins centrifugal 15 minutes.Promptly get required product, its particle diameter is 2-6nm, and final particle can be dispersed in absolute ethyl alcohol or the chloroform again.From TEM electromicroscopic photograph shown in Figure 3, just can clearly see the existence of product.
Embodiment 3
1,0.000031mol chloroplatinic acid and 0.0000625mol (1: 2) Iron dichloride tetrahydrate fully are dissolved in together the ethylene glycol of 3ml, add 0.1g enuatrol and 2mg hexichol crown ether, ultrasonic concussion 12 minutes.
2, accurately measure 3ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of step (1), and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 13 hours down at 120 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 3000 rev/mins centrifugal 20 minutes, promptly getting required product, its particle diameter is 2-7nm, final particle can be dispersed in absolute ethyl alcohol or the chloroform again.From TEM electromicroscopic photograph shown in Figure 4, just can clearly see the existence of product.
Embodiment 4
1,0.0000625mol l dichloride dicyan diphenyl is closed the absolute ethyl alcohol that platinum (II) and 0.0000625mol (1: 1) Iron dichloride tetrahydrate fully are dissolved in 6ml together, add 0.1g enuatrol and 2mg hexichol crown ether, ultrasonic concussion 10 minutes.
2, accurately measure 5ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of step (1), and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 12 hours down at 130 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 4000 rev/mins centrifugal 12 minutes, promptly getting required product, its particle diameter is 8-12nm, final particle can be dispersed in absolute ethyl alcohol or the chloroform again.From TEM electromicroscopic photograph shown in Figure 4, just can clearly see the existence of product.
Embodiment 5
1,0.000031mol dichloride dicyan diphenyl is closed the absolute ethyl alcohol that platinum (II) and 0.0000625mol (1: 2) ferric oxalate fully are dissolved in 6ml together, add 0.2g enuatrol and 4mg hexichol crown ether, ultrasonic concussion 10 minutes.
2, accurately measure 3ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of step (1).Ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 10 hours down at 120 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 5000 rev/mins centrifugal 10 minutes.Promptly get required product, its particle diameter is 2-6nm, and final particle can be dispersed in absolute ethyl alcohol or the chloroform again.From TEM electromicroscopic photograph shown in Figure 6, just can clearly see the existence of product.
Embodiment 6
1,0.000031mol platinous chloride and 0.0000625mol (1: 2) ferric oxalate fully are dissolved in together the ethylene glycol of 4ml, add 0.15g enuatrol and 3mg hexichol crown ether, ultrasonic concussion 8 minutes.
2, accurately measure 2ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of step (1), and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 15 hours down at 120 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 5000 rev/mins centrifugal 10 minutes.Promptly get required product, its particle diameter is 2-6nm, and final particle can be dispersed in absolute ethyl alcohol or the chloroform again.Can from the TEM electromicroscopic photograph, clearly see the existence of product equally.
Embodiment 7
1,0.000031mol platinous chloride and 0.0000935mol (1: 3) ferric oxalate fully are dissolved in together the absolute ethyl alcohol of 8ml, add 0.3g enuatrol and 5mg hexichol crown ether, ultrasonic concussion 15 minutes.
2, accurately measure 4ml 1, the 2-propane diols fully mixes with 2ml oleic acid, joins in the system of step (1), and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 14 hours down at 130 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 4000 rev/mins centrifugal 15 minutes.Promptly get required product, its particle diameter is 2-15nm, and final particle can be dispersed in absolute ethyl alcohol or the chloroform again.Can from the TEM electromicroscopic photograph, clearly see the existence of product equally.
Embodiment 8
1,0.000031mol chloroplatinic acid and 0.0000625mol (1: 2) acetyl acetone iron (III) fully are dissolved in together the ethylene glycol of 2ml, add 0.1g enuatrol and 2mg hexichol crown ether, ultrasonic concussion 15 minutes.
2, accurately measure 4ml 1, the 2-propane diols fully mixes with 1.5ml oleic acid, joins in the system of step (1), and magnetic agitation 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 13 hours down at 140 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 5000 rev/mins centrifugal 10 minutes.Promptly get required product, its particle diameter is 2-15nm, and final particle can be dispersed in absolute ethyl alcohol or the chloroform again.Can from the TEM electromicroscopic photograph, clearly see the existence of product equally.
Embodiment 9
1,0.000031mol acetyl acetone platinum (II) and 0.0000625mol (1: 2) Iron dichloride tetrahydrate fully are dissolved in together the ethylene glycol of 3ml, add 0.1g enuatrol and 2mg hexichol crown ether, ultrasonic concussion 12 minutes.
2, accurately measure 3ml 1, the 2-propane diols fully mixes with 1ml oleic acid, joins in the system of step (1), and ultrasonic processing 10 minutes makes it abundant mixing, then whole mixed system is joined in the reaction autoclave together, heats 13 hours down at 120 ℃.Reaction finishes the back with ethanol washing particle 3-5 time, and under 3000 rev/mins centrifugal 20 minutes, promptly getting required product, its particle diameter is 2-7nm, final particle can be dispersed in absolute ethyl alcohol or the chloroform again.From TEM electromicroscopic photograph shown in Figure 4, just can clearly see the existence of product.
Claims (5)
1, a kind of preparation method of monodisperse nanometer Fe-Pt alloy is characterized in that concrete steps are as follows:
(1) with the platiniferous inorganic salts or contain platinum complex and iron content inorganic salts or contain iron complex as pre-reaction material, be dissolved in respectively in the organic solvent, add an amount of enuatrol solid and phase catalyst hexichol crown ether, ultrasonic processing 8-15 minute; Platiniferous inorganic salts or contain platinum complex and iron content inorganic salts or the mol ratio that contains iron complex are 1: 1～1: 4, enuatrol and iron content inorganic salts or contain iron complex and platiniferous inorganic salts or the mol ratio that contains the total amount of substance of platinum complex are 5: 1～10: 1, hexichol crown ether and iron content inorganic salts or contain iron complex and platiniferous inorganic salts or the mol ratio that contains the total amount of substance of platinum complex are 1: 30～1: 100; Organic solvent and iron content inorganic salts or contain iron complex and platiniferous inorganic salts or the mol ratio that contains the total amount of substance of platinum complex are 34: 1～85: 1;
(2) measure propylene glycol solution and mix, stir, make it abundant mixing, mixed solution is joined in the step (1) with oleic acid, join autoclave then together, reaction is 8-15 hour under 100-150 ℃ of temperature, washing, centrifugation promptly gets required product, and its particle diameter is 2-15nm; Wherein the volume ratio of propane diols and oleic acid is 2: 1～3: 1, propane diols and iron content inorganic salts or contain iron complex and platiniferous inorganic salts or the mol ratio that contains the total amount of substance of platinum complex are 30: 1～80: 1.
2, the preparation method of monodisperse nanometer Fe-Pt alloy according to claim 1, it is characterized in that described platiniferous inorganic salts be in chloroplatinic acid or the platinous chloride any, contain platinum complex and be dichloride dicyan diphenyl and close in platinum (II) or the acetyl acetone platinum (II) any, the iron content inorganic salts are frerrous chloride, contain iron complex and be in ferric oxalate, acetyl acetone iron (II) or the acetyl acetone iron (III) any.
3, the preparation method of monodisperse nanometer Fe-Pt alloy according to claim 1 is characterized in that described organic solvent is absolute ethyl alcohol or ethylene glycol.
4, the preparation method of monodisperse nanometer Fe-Pt alloy according to claim 1 is characterized in that the stirring described in the step (2) is ultrasonic concussion or magnetic agitation.
5, the preparation method of monodisperse nanometer Fe-Pt alloy according to claim 1 is characterized in that the centrifugation rotating speed is 3000-5000 rev/min described in the step (2), and the time is 10-20 minute.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101524762B (en) * | 2009-04-14 | 2011-05-25 | 上海师范大学 | Method for preparing ferroplatinum nano-particle |
| CN102029402B (en) * | 2011-01-14 | 2012-05-30 | 武汉理工大学 | Method for synthesizing ferroplatinum alloy nano material |
| CN102218543B (en) * | 2011-05-20 | 2013-01-23 | 湖北大学 | Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof |
| CN102489717B (en) * | 2011-12-22 | 2013-09-04 | 云南云天化股份有限公司 | Preparation method of nanometer silver particles |
| CN105414558A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院山西煤炭化学研究所 | Preparation method of mono-dispersed spherical nano copper and ferrum |
| CN106583744B (en) * | 2017-01-21 | 2018-06-19 | 杨林 | It is a kind of to prepare noble metal nano particles method |
| CN106693962B (en) * | 2017-01-21 | 2019-10-01 | 明光市天骄科技发展有限公司 | A kind of preparation method of double noble metal nano catalyst |
| CN111554946B (en) * | 2020-04-23 | 2022-05-17 | 广东泰极动力科技有限公司 | Pt alloy with high HOR catalytic activity and preparation method and application thereof |
| CN114628706B (en) * | 2022-04-11 | 2024-02-13 | 西安凯立新材料股份有限公司 | Catalyst for proton exchange membrane fuel cell and preparation method thereof |
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| CN1100016A (en) * | 1993-09-11 | 1995-03-15 | 中国科学院金属研究所 | Submicron iron-platinum single-phase alloy particles preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100016A (en) * | 1993-09-11 | 1995-03-15 | 中国科学院金属研究所 | Submicron iron-platinum single-phase alloy particles preparation |
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| CN1557587A (en) * | 2004-01-16 | 2004-12-29 | 清华大学 | Reverse micelle method for preparing FePt alloy nanoparticles |
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