CN103506619A - Silver wire wrapped by Fe3O4 nanometer magnetic particles and preparation and application thereof - Google Patents
Silver wire wrapped by Fe3O4 nanometer magnetic particles and preparation and application thereof Download PDFInfo
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- CN103506619A CN103506619A CN201210215958.3A CN201210215958A CN103506619A CN 103506619 A CN103506619 A CN 103506619A CN 201210215958 A CN201210215958 A CN 201210215958A CN 103506619 A CN103506619 A CN 103506619A
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Abstract
The invention belongs to the technical fields of nanocomposites and preparation and application thereof, and particularly relates to a silver wire wrapped by Fe3O4 nanometer magnetic particles and preparation and application thereof. The silver wire wrapped by the Fe3O4 nanometer magnetic particles is prepared in an atmospheric environment, and the mass ratio of silver and Fe3O4 is 1:0.5-0.01. The preparation of the silver wire wrapped by the Fe3O4 nanometer magnetic particles comprises the steps that a silver wire solution is firstly prepared, hydrogen peroxide is used for surface treatment, the treated silver wire solution is added in a mixed solution of ferric iron and ferrous, the molar ratio of the ferric iron and the ferrous of the mixed solution is 2:1, a solution of the silver wire wrapped by the Fe3O4 nanometer magnetic particles is obtained through a co-precipitation method, and lastly deionized water is added in the solution of the silver wire wrapped by the Fe3O4 nanometer magnetic particles to carry out scrubbing repeatedly. The silver wire wrapped by the Fe3O4 nanometer magnetic particles and the preparation and application thereof are simple in technology, low in cost and beneficial to achieving industrialized production. According to the prepared composite, the orientation and the distribution of silver wires can be controlled through the action of magnets, and anisotropy electric conduction can be achieved, or circuits arranged in stripe-shaped parallel same as the magnets in rows can be formed and applied to the field of electronic products and the like.
Description
Technical field
The invention belongs to nano composite material and preparation and applied technical field, particularly a kind of Fe
3o
4silver-colored line and preparation and purposes that magnetic nanoparticle is coated.
Background technology
In recent years, due to its unique physicochemical properties and at chemical-biological analysis and nano-device, the applications well prospect aspect constructing attracts wide attention the metal material of nanostructured.The nanometer of metal material makes it have unique character, as skin effect, bulk effect, quantum size effect and macroscopic quantum effect etc., thereby there is the unusual performance of the aspect such as optical, electrical, magnetic, thermodynamics and chemical reaction that is different from ordinary metallic material.As far back as 1992, Ducamp-Sanguesa etc. prepared nano silver wire, and were furtherd investigate in recent years.
Yet nano metal material has very large specific area, and surface-active is high, very easily reunites, dispersed very poor, have a strong impact on its application.Utilizing physics, chemistry and other method to carry out surface to nano metal powder is coated and modifies, by changing composition, structure and the state on nano metal powder surface, not only can improve the dispersiveness of nano metal powder, improve the compatibility between nano metal powder and other materials, can also produce new physics, chemistry, mechanical performance and new function, and reduce production costs etc.Therefore, Coating Nano-metal Materials, as a kind of important functional material, is with a wide range of applications.
Coated just the utilized this point of magnetic particle to nano-silver thread, produces the new functional material simultaneously with magnetic electricity performance, and this is to attempt first, is also characteristic of the present invention place.Further application to it, will produce new industrial prospect.
Summary of the invention
The object of this invention is to provide and a kind ofly there is magnetic property and outstanding electric property simultaneously and can realize anisotropic Fe
3o
4the silver-colored line that magnetic nanoparticle is coated.
Another object of the present invention is to provide a kind ofly to be had magnetic and outstanding electric property simultaneously and can realize anisotropic Fe
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated.
A further object of the present invention is to provide above-mentioned Fe
3o
4the purposes of the silver-colored line that magnetic nanoparticle is coated.
Technical scheme of the present invention is as follows:
Fe provided by the invention
3o
4the silver-colored line that magnetic nanoparticle is coated, its Fe for preparing under atmospheric environment
3o
4the silver-colored line that magnetic nanoparticle is coated, wherein, silver and Fe
3o
4the proportion by weight of magnetic nanoparticle is 1:0.5 ~ 0.01.
Described Fe
3o
4the coated silver-colored linear diameter of magnetic nanoparticle is 200-600nm, Fe
3o
4magnetic nanoparticle particle diameter is 10-50nm.
Fe provided by the invention
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, its step is as follows:
(1) prepare silver-colored line solution
Get ethylene glycol and add iron chloride and PVP, be stirred to iron chloride and PVP dissolves completely, obtain A solution;
Get with the ethylene glycol of A solution moderate and add silver nitrate, be stirred to silver nitrate and dissolve completely, obtain B solution;
A solution is mixed with the volume ratio of 1:1 with B solution; The mixed solution mixing is transferred in autoclave, in 140 ℃ ~ 180 ℃, heats 2 ~ 4 hours, obtain silver-colored line mixed liquor;
Gained silver line mixed liquor is first washed with acetone, use afterwards ethanol cyclic washing, finally, with deionized water washing, make silver-colored line solution;
(2) silver-colored line solution is carried out to surface treatment
Silver-colored line solution is carried out to surface treatment with strong oxidizer, use afterwards deionized water cyclic washing, obtain the silver-colored line solution after surface treatment;
(3) prepare Fe
3o
4the mixed liquor of the silver-colored line that magnetic nanoparticle is coated
Get ferric iron and ferrous mixture that mol ratio is 2:1, add in the resulting silver-colored line solution of step (2);
Oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Be warming up to subsequently 60 ~ 70 ℃, and add the aqueous slkali of 6mol/L, continue to stir 50 ~ 80min; Continue to be warming up to 80 ~ 90 ℃, add surfactant, remove oil bath heating, stirring is also cooling, obtains Fe
3o
4the mixed liquor of the silver-colored line that magnetic nanoparticle is coated;
(4) preparation is containing Fe
3o
4the aqueous solution of the silver-colored line that magnetic nanoparticle is coated
With gained Fe in ndfeb magnet adsorption step (3)
3o
4fe in the mixed liquor of the silver-colored line that magnetic nanoparticle is coated
3o
4the silver-colored line that magnetic nanoparticle is coated; With deionized water wash to pH be 6 ~ 8, must contain Fe
3o
4the aqueous solution of the silver-colored line that magnetic nanoparticle is coated; Described Fe
3o
4the coated silver-colored linear diameter of magnetic nanoparticle is 200-600nm, described Fe
3o
4the particle diameter of magnetic nanoparticle is 10-50nm; Described Fe
3o
4silver-colored line and Fe in the silver-colored line that magnetic nanoparticle is coated
3o
4magnetic nanoparticle mass ratio is 1:0.5 ~ 0.01.
Described strong oxidizer is hydrogen peroxide or nitric acid.Described ferric iron is iron chloride, ferric nitrate or ferric sulfate.Described ferrous iron is frerrous chloride, ferrous nitrate or ferrous sulfate.Described aqueous slkali is sodium hydroxide solution or ammoniacal liquor.Described surfactant is SDS, polyethylene glycol or OP-10.
Fe of the present invention
3o
4a purposes of the silver-colored line that magnetic nanoparticle is coated is: as filler, join in epoxy resin, by external magnetic field, control its orientation and distribution, prepare anisotropy conductiving glue, for electronic package material.
Fe of the present invention
3o
4another purposes of the silver-colored line that magnetic nanoparticle is coated is: as filler, join in Polymer Solution, make Fe
3o
4the silver-colored line film that magnetic nanoparticle is coated, controls its orientation by external magnetic field and forms the circuit that strip is arranged in parallel, for the preparation of electronic product circuit.
The present invention be take silver-colored line as basis, adopts coprecipitation to be coated silver-colored line, prepares uniformly by Fe
3o
4the silver-colored line that magnetic nanoparticle is coated; Its compared with prior art, tool of the present invention has the following advantages:
1, Fe of the present invention
3o
4the coated silver-colored line of magnetic nanoparticle is prepared and is still belonged to the first time under atmospheric environment.
2, preparation method of the present invention, technique is simple, with low cost, is easy to realize suitability for industrialized production.
3, Fe provided by the invention
3o
4the silver-colored line that magnetic nanoparticle is evenly coated, can be used as a kind of filler adds in polyvinyl alcohol film or epoxy resin-base, by external magnetic field, do to control its orientation and distribution, form and there is anisotropic conductive path or conducting resinl, can be used for electronic product or chip package.
Accompanying drawing explanation
Fig. 1 is Fe
3o
4the surface sweeping electron microscope picture of the silver-colored line that magnetic nanoparticle is coated;
Fig. 2 is external magnetic field orientation schematic diagram, and M represents ndfeb magnet, and 1 representative is coated with Fe
3o
4the glass plate of the silver-colored line solution that magnetic nanoparticle is coated, the silver-colored line after white fine rule section representative is wherein wrapped by; 2 representatives, when magnet is placed orientation below glass plate, form the conductive path of strip; When 3 representatives are placed orientation when magnet in glass plate both sides, the orientation of the microscopic anisotropy of formation;
Fig. 3 a is Fe of the present invention
3o
4after the polyvinyl alcohol that the coated silver-colored line solution of magnetic nanoparticle is 7% with mass fraction mixes with the mass fraction of 1:1, external magnetic field is orientated the film of the similar winding displacement circuit of formation afterwards below glass plate; Fig. 3 b is the front and back contrast light microscope picture of external magnetic field after the orientation of glass plate both sides, and wherein (a) is for before being orientated, (b) for after orientation.
The specific embodiment
Below in conjunction with drawings and Examples (but being not limited to illustrated embodiment) and comparative example, further describe the present invention:
1) 200mL ethylene glycol is placed in to the 500mL conical flask of dried and clean, adds 27mg ferric chloride hexahydrate and 16.65g PVP, magnetic agitation to ferric chloride hexahydrate and PVP dissolves completely, obtains A solution;
The 500mL conical flask that 200mL ethylene glycol is placed in to another dried and clean, adds 17g silver nitrate, and magnetic agitation to silver nitrate dissolves completely, obtains B solution;
A solution is mixed with 1:1 volume ratio with B solution; The mixed solution mixing is transferred in autoclave, in 140 ℃ ~ 180 ℃, heats 2 ~ 4 hours, obtain silver-colored line mixed liquor; The silver-colored line mixed liquor obtaining is first washed with acetone, then use ethanol cyclic washing, finally with deionized water washing, obtain the silver-colored line solution of 0.025g/g;
2) get the beaker that above-mentioned silver-colored line solution 3.2g is placed in the 200mL of dried and clean, add 8g hydrogen peroxide, glass bar is stirred to and reacts completely, and with deionized water washing for several times, obtains the silver-colored line solution after surface treatment afterwards;
3) above-mentioned silver-colored line solution is carried out to cell ultrasonic, be placed in the 100mL conical flask of dried and clean, add 92.96mg ferric chloride hexahydrate and 47.8mg green vitriol, add appropriate amount of deionized water to 1/3 ~ 1/2 volume of conical flask, oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Oil bath temperature is risen to 60 ~ 70 ℃, add 6mol/L sodium hydroxide solution 0.2292 ~ 0.2500mL, continue mechanical agitation 50 ~ 80min; Oil bath temperature is risen to 80 ~ 90 ℃, add 0.01 ~ 0.03g SDS, remove oil bath heating, mechanical agitation is also cooled to room temperature, obtains Fe
3o
4the mixed liquor of the silver-colored line that magnetic nanoparticle is coated;
4) the use ndfeb magnet adsorption step 3) Fe in gained mixed liquor
3o
4the silver-colored line that magnetic nanoparticle is coated; Repeatedly with deionized water wash to pH value of solution be 6 ~ 8, then with ethanol washing, remove SDS wherein, then with deionized water washing, make Fe
3o
4magnetic nanoparticle is the aqueous solution of coated silver-colored line evenly, wherein, and described Fe
3o
4the coated silver-colored linear diameter of magnetic nanoparticle is 200-600nm, Fe
3o
4the particle diameter of magnetic nanoparticle is 10-50nm; Fe
3o
4silver-colored line and Fe in the silver-colored line that magnetic nanoparticle is coated
3o
4magnetic nanoparticle mass ratio is 1:0.5.
Silver line solution manufacturing process is with embodiment 1 step 1).
Get the beaker that above-mentioned silver-colored line solution 4g is placed in the 200mL of dried and clean, add 10g hydrogen peroxide, with glass bar, be stirred to and react completely, with deionized water washing for several times, obtain the silver-colored line solution after surface treatment;
Silver-colored line solution after above-mentioned surface treatment is carried out to cell ultrasonic, be placed in the 100mL conical flask of dried and clean, add 69.6mg ferric chloride hexahydrate and 35.95mg green vitriol, add appropriate amount of deionized water to 1/3 ~ 1/2 volume of conical flask, oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Oil bath temperature is risen to 60 ~ 70 ℃, add sodium hydroxide solution 0.1724 ~ 0.2000mL of 6mol/L, continue with mechanical agitation 50 ~ 80min; Oil bath temperature is risen to 80 ~ 90 ℃, adds 0.02 ~ 0.04gSDS, remove oil bath heating, by mechanical agitation to room temperature.
With ndfeb magnet, adsorb the Fe in above-mentioned gained mixed liquor
3o
4the silver-colored line that magnetic nanoparticle is coated; Repeatedly with deionized water wash to pH value of solution be 6 ~ 8, then with ethanol washing, remove SDS wherein, then make Fe with deionized water washing
3o
4the silver-colored line solution that magnetic nanoparticle is evenly coated.
This Fe
3o
4silver-colored line and Fe in magnetic nanoparticle coated with silver line
3o
4magnetic nanoparticle mass ratio is 1:0.3.
Silver line solution manufacturing process is with embodiment 1 step 1).
Get the beaker that above-mentioned silver-colored line solution 12g is placed in the 200mL of dried and clean, add 30g hydrogen peroxide, with glass bar, be stirred to and react completely, with deionized water washing for several times.
Above-mentioned silver-colored line solution is carried out to cell ultrasonic, be placed in the 100mL conical flask of dried and clean, add 69.6mg ferric chloride hexahydrate, 35.95mg green vitriol, add appropriate amount of deionized water to 1/3 ~ 1/2 volume of conical flask, oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Oil bath temperature is risen to 60 ~ 70 ℃, add sodium hydroxide solution 0.1724 ~ 0.2000mL of 6mol/L, continue with mechanical agitation 50 ~ 80min; Oil bath temperature is risen to 80 ~ 90 ℃, adds 0.03 ~ 0.05gSDS, remove oil bath heating, by mechanical agitation to room temperature.
With ndfeb magnet, adsorb the Fe in above-mentioned gained mixed liquor
3o
4the silver-colored line that magnetic nanoparticle is coated; Repeatedly with deionized water wash to pH value of solution be 6 ~ 8, then with ethanol washing, remove SDS wherein, then make Fe with deionized water washing
3o
4the silver-colored line solution that magnetic nanoparticle is evenly coated.
This Fe
3o
4silver-colored line and Fe in magnetic nanoparticle coated with silver line
3o
4magnetic nanoparticle mass ratio is 1:0.1.
Silver line solution manufacturing process is with embodiment 1 step 1).
Get the beaker that above-mentioned silver-colored line solution 16g is placed in the 200mL of dried and clean, add 40g hydrogen peroxide, with glass bar, be stirred to and react completely, with deionized water washing for several times.
Above-mentioned silver-colored line solution is carried out to cell ultrasonic, be placed in the 100mL conical flask of dried and clean, add 46.48mg ferric chloride hexahydrate, 23.9mg green vitriol, add appropriate amount of deionized water to 1/3 ~ 1/2 volume of conical flask, oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Oil bath temperature is risen to 60 ~ 70 ℃, add sodium hydroxide solution 0.1146 ~ 0.1500mL of 6mol/L, continue with mechanical agitation 50 ~ 80min; Oil bath temperature is risen to 80 ~ 90 ℃, adds 0.04 ~ 0.06gSDS, remove oil bath heating, by mechanical agitation to room temperature.
With ndfeb magnet, adsorb the Fe in above-mentioned gained mixed liquor
3o
4the silver-colored line that magnetic nanoparticle is coated; Repeatedly with deionized water wash to pH value of solution be 6 ~ 8, then with ethanol washing, remove SDS wherein, then make Fe with deionized water washing
3o
4the silver-colored line solution that magnetic nanoparticle is evenly coated.
This Fe
3o
4silver-colored line and Fe in magnetic nanoparticle coated with silver line
3o
4magnetic nanoparticle mass ratio is 1:0.05.The visible Fig. 1 of its scanning electron microscope diagram sheet.
Silver line solution manufacturing process is with embodiment 1 step 1).
Get the beaker that above-mentioned silver-colored line solution 80g is placed in the 500mL of dried and clean, add 70g hydrogen peroxide, with glass bar, be stirred to and react completely, with deionized water washing for several times.
Above-mentioned silver-colored line solution is carried out to cell ultrasonic, be placed in the 100mL conical flask of dried and clean, add 46.48mg ferric chloride hexahydrate, 23.9mg green vitriol, add appropriate amount of deionized water to 1/3 ~ 1/2 volume of conical flask, oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Oil bath temperature is risen to 60 ~ 70 ℃, add sodium hydroxide solution 0.1146 ~ 0.1500mL of 6mol/L, continue with mechanical agitation 50 ~ 80min; Oil bath temperature is risen to 80 ~ 90 ℃, adds 0.15 ~ 0.25gSDS, remove oil bath heating, by mechanical agitation to room temperature.
With ndfeb magnet, adsorb the Fe in above-mentioned gained mixed liquor
3o
4the silver-colored line that magnetic nanoparticle is coated; Repeatedly with deionized water wash to pH value of solution be 6 ~ 8, then with ethanol washing, remove SDS wherein, then make Fe with deionized water washing
3o
4the silver-colored line solution that magnetic nanoparticle is evenly coated.
This Fe
3o
4silver-colored line and Fe in magnetic nanoparticle coated with silver line
3o
4magnetic nanoparticle mass ratio is 1:0.01.
Comparative example 1
The polyvinyl alcohol that is 7% with mass fraction by the silver-colored line solution being wrapped by mixes with the mass fraction of 1:1, and is stirred to and mixes with glass bar, and be evenly coated with and be laid on glass plate, the film that obtains being evenly distributed, all directions are all conducted electricity.
Comparative example 2
The polyvinyl alcohol that is 7% with mass fraction by the silver-colored line solution being wrapped by mixes with the mass fraction of 1:1, and be stirred to and mix with glass bar, evenly be coated with and be laid on glass plate, ndfeb magnet is put under glass plate, obtain the film that strip distributes, strip region conduction is good, but not strip region, the direction vertical with strip are all non-conductive.The visible Fig. 3 a of film preparing.
Claims (10)
1. a Fe
3o
4the silver-colored line that magnetic nanoparticle is coated, its Fe for preparing under atmospheric environment
3o
4the silver-colored line that magnetic nanoparticle is coated, wherein, silver and Fe
3o
4the proportion by weight of magnetic nanoparticle is 1:0.5 ~ 0.01.
2. press the Fe described in claims 1
3o
4the silver-colored line that magnetic nanoparticle is coated, is characterized in that described Fe
3o
4the coated silver-colored linear diameter of magnetic nanoparticle is 200-600nm, Fe
3o
4magnetic nanoparticle particle diameter is 10-50nm.
3. the Fe described in a claim 1
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, its step is as follows:
(1) prepare silver-colored line solution
Get ethylene glycol and add iron chloride and PVP, be stirred to iron chloride and PVP dissolves completely, obtain A solution;
Get with the ethylene glycol of A solution moderate and add silver nitrate, be stirred to silver nitrate and dissolve completely, obtain B solution;
A solution is mixed with the volume ratio of 1:1 with B solution; The mixed solution mixing is transferred in autoclave, in 140 ℃ ~ 180 ℃, heats 2 ~ 4 hours, obtain silver-colored line mixed liquor;
Gained silver line mixed liquor is first washed with acetone, use afterwards ethanol cyclic washing, finally, with deionized water washing, make silver-colored line solution;
(2) silver-colored line solution is carried out to surface treatment
Silver-colored line solution is carried out to surface treatment with strong oxidizer, use afterwards deionized water cyclic washing, obtain the silver-colored line solution after surface treatment;
(3) prepare Fe
3o
4the mixed liquor of the silver-colored line that magnetic nanoparticle is coated
Get ferric iron and ferrous mixture that mol ratio is 2:1, add in the resulting silver-colored line solution of step (2);
Oil bath is heated to 30 ~ 50 ℃, mechanical agitation 20 ~ 40min; Be warming up to subsequently 60 ~ 70 ℃, and add the aqueous slkali of 6mol/L, continue to stir 50 ~ 80min; Continue to be warming up to 80 ~ 90 ℃, add surfactant, remove oil bath heating, stirring is also cooling, obtains Fe
3o
4the mixed liquor of the silver-colored line that magnetic nanoparticle is coated;
(4) preparation is containing Fe
3o
4the aqueous solution of the silver-colored line that magnetic nanoparticle is coated
With gained Fe in ndfeb magnet adsorption step (3)
3o
4fe in the mixed liquor of the silver-colored line that magnetic nanoparticle is coated
3o
4the silver-colored line that magnetic nanoparticle is coated; With deionized water wash to pH be 6 ~ 8, must contain Fe
3o
4the aqueous solution of the silver-colored line that magnetic nanoparticle is coated; Described Fe
3o
4the coated silver-colored linear diameter of magnetic nanoparticle is 200-600nm, described Fe
3o
4the particle diameter of magnetic nanoparticle is 10-50nm; Described Fe
3o
4silver-colored line and Fe in the silver-colored line that magnetic nanoparticle is coated
3o
4magnetic nanoparticle mass ratio is 1:0.5 ~ 0.01.
4. by Fe claimed in claim 3
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, is characterized in that, described strong oxidizer is hydrogen peroxide or nitric acid.
5. by Fe claimed in claim 3
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, is characterized in that, described ferric iron is iron chloride, ferric nitrate or ferric sulfate.
6. by Fe claimed in claim 3
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, is characterized in that, described ferrous iron is frerrous chloride, ferrous nitrate or ferrous sulfate.
7. by Fe claimed in claim 3
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, is characterized in that, described aqueous slkali is sodium hydroxide solution or ammoniacal liquor.
8. by Fe claimed in claim 3
3o
4the preparation method of the silver-colored line that magnetic nanoparticle is coated, is characterized in that, described surfactant is SDS, polyethylene glycol or OP-10.
9. a Fe claimed in claim 1
3o
4the purposes of the silver-colored line that magnetic nanoparticle is coated, it joins in epoxy resin as filler, by external magnetic field, controls its orientation and distribution, prepares anisotropy conductiving glue, for electronic package material.
10. a Fe claimed in claim 1
3o
4the purposes of the silver-colored line that magnetic nanoparticle is coated, it joins in Polymer Solution as filler, makes Fe
3o
4the silver-colored line film that magnetic nanoparticle is coated, controls its orientation by external magnetic field and forms the circuit that strip is arranged in parallel, for the preparation of electronic product circuit.
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CN110283450B (en) * | 2019-07-03 | 2021-09-14 | 昆明理工大学 | Method for preparing flexible conductive composite material by regulating graphene arrangement through magnetic field |
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CN114799160A (en) * | 2021-01-27 | 2022-07-29 | 中国科学院理化技术研究所 | Method for modifying surface of magnetic particle |
CN114799160B (en) * | 2021-01-27 | 2024-03-26 | 中国科学院理化技术研究所 | Method for modifying surface of magnetic particle |
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