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Silicon hydroxyl magnetic bead and preparation method and application thereof

A technology of silanol and magnetic beads, which is applied in the field of silanol magnetic beads and its preparation, can solve the problems of inconsistent magnetic content of magnetic bead particles, easy generation of defects in nanoparticles, cumbersome sample screening process, etc., and achieve good packaging compactness and easy Post-processing, avoiding the effect of post-screening

Inactive Publication Date: 2019-10-08
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 3. This method coats SiO 2 When the surface of nanoparticles is prone to defects, SiO 2 Difficulty in Fe 3 o 4 Deposition and growth of cracks and defects on the surface of nanoparticles
[0007] 1. The magnetic content of the magnetic beads is inconsistent, the quality is uneven, and the response is inconsistent;
[0008] 2. SiO on the surface of magnetic beads 2 The density is low, there are many defects, the structure of the magnetic beads is unstable, and the structure is easily destroyed during ultrasonic dispersion;
[0009] 3. The batch stability is not high, the difference between different batches of products is obvious, and the sample screening process is cumbersome

Method used

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  • Silicon hydroxyl magnetic bead and preparation method and application thereof
  • Silicon hydroxyl magnetic bead and preparation method and application thereof
  • Silicon hydroxyl magnetic bead and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1. Fe 3 o 4 Synthesis of Nanoparticles

[0050] (1) 8.1g (0.03mol) of FeCl 3 ·6H 2 O. 120mL (2.15mol) of ethylene glycol (EG), 4.86g (0.0165mol) of trisodium citrate, and 10.0g (0.12mol) of sodium acetate (NaAc) were mixed and stirred, and ultrasonically treated at 30w for 15min to form a uniform Emulsion, then pass the emulsion through a 400-mesh standard sieve to remove the large particles that have not formed the emulsion;

[0051] (2) Transfer the above-mentioned standard emulsion to a polytetrafluoroethylene liner digestion tank, put it into a reaction kettle, and take it out after being incubated at 220°C for 18h;

[0052] (3) After the high-pressure digestion tank is cooled, use a magnet to separate the black precipitate, wash it 3 times with pure water and absolute ethanol, clean it by magnetic suction, and dry it. 3 o 4 The particle size is about 380nm.

[0053] 2. ALD deposition of SiO 2 membrane

[0054] (1) the above-prepared Fe 3 o 4 Take 1.0g of...

Embodiment 2

[0059] 1. Fe 3 o 4 Synthesis of Nanoparticles

[0060] (1) 4.0g (0.015mol) FeCl 3 ·6H 2 O, 100mL (1.8mol) ethylene glycol 1.86mol (EG), 3.12g (0.0106mol) trisodium citrate, 4.86g (0.059mol) sodium acetate (NaAc) mixed and stirred, 30w ultrasonic treatment for 15min to form a uniform Emulsion, then pass the emulsion through a 400-mesh standard sieve to remove the large particles that have not formed the emulsion;

[0061] (2) Transfer the above-mentioned standard emulsion to a polytetrafluoroethylene liner digestion tank, put it into a reaction kettle, and take it out after being incubated at 160° C. for 8 hours;

[0062] (3) After the high-pressure digestion tank is cooled, use a magnet to separate the black precipitate, wash it 3 times with pure water and absolute ethanol, clean it by magnetic suction, and dry it. 3 o 4 Particle size 150nm.

[0063] 2. ALD deposition of SiO 2 membrane

[0064] (1) the above-prepared Fe 3 o 4 Take 1.0g of the powder and place it in ...

Embodiment 3

[0069] 1. Fe 3 o 4 Synthesis of Nanoparticles

[0070] (1) 6.0g (0.022mol) FeCl 3 ·6H 2 0, 120mL (2.15mol) ethylene glycol (EG), 4.86g (0.0165mol) trisodium citrate, 7.92g (0.096mol) sodium acetate (NaAc) mixed and stirred, 30w ultrasonic treatment 15min, make it form uniform emulsion, Afterwards, pass the emulsion through a 400-mesh standard sieve to remove large particles that have not formed the emulsion;

[0071] (2) Transfer the above-mentioned standard emulsion to a polytetrafluoroethylene liner digestion tank, put it into a reaction kettle, and take it out after being incubated at 200°C for 10h;

[0072] (3) After the high-pressure digestion tank is cooled, use a magnet to separate the black precipitate, wash it 3 times with pure water and absolute ethanol, clean it by magnetic suction, and dry it. 3 o 4 Particle size 540nm.

[0073] 2. ALD deposition of SiO 2 membrane

[0074] (1) the above-prepared Fe 3 o 4 Take 1.0g of the powder and place it in the ALD eq...

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Abstract

The invention discloses a preparation method of a silicon hydroxyl magnetic bead. The preparation method comprises the following steps that ferric trichloride, trisodium citrate, sodium acetate and polyhydric alcohol are mixed evenly to obtain a mixed solution, and Fe3O4 nanoparticles are prepared by a solvothermal method; and the surface of the Fe3O4 nanoparticles is coated with SiO2 films by atomic layer deposition to obtain the silicon hydroxyl magnetic bead. The Fe3O4 nanoparticles prepared by the solvothermal method are coated with the SiO2 films by atomic layer deposition (ALD), the SiO2films are plated on the surface of the Fe3O4 nanoparticles in the form of a monatomic film, the SiO2 films laminated by the method can grow at a constant speed on the surface and at defects of the Fe3O4 nanoparticles, the SiO2 films on the surface are a whole after coating, and the coating compactness of the SiO2 films on Fe3O4 is good and the SiO2 films are not prone to falling off, therefore, coating defects on the surface of the magnetic bead can be prevented from being generated. In addition, by adjusting the deposition conditions and the number of cycles, the thickness of the SiO2 filmscan be precisely controlled, the process is simple, operation can be standardized, no complicated operation is required, errors are small, and later screening of the magnetic bead is avoided, so thatthe purpose of improving the product quality and the stability of magnetic bead batches is achieved.

Description

technical field [0001] The embodiments of the present invention relate to the technical field of magnetic material preparation, in particular to a silanol magnetic bead and its preparation method and application. Background technique [0002] The common preparation method of silanol magnetic beads is only in the above Fe 3 o 4 The surface of nanoparticles is decorated with a layer of nano-SiO by the Stober method 2 , the specific operation is to combine ethyl orthosilicate and Fe 3 o 4 Disperse in ethanol solution, then add ammonia water dropwise to hydrolyze ethyl orthosilicate, and the generated nano-SiO 2 in Fe 3 o 4 Surface growth, but this method has the following defects: [0003] 1. SiO is generated during hydrolysis 2 The nucleation and growth rate are not easy to control, resulting in SiO 2 Uneven particle size, SiO 2 Separately grow into pellets and Fe 3 o 4 Problems such as uneven surface coating; [0004] 2. This method coats Fe with a particle size ...

Claims

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Application Information

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IPC IPC(8): C01G49/08H01F1/01H01F41/00C23C16/455C23C16/40B82Y30/00B82Y40/00C12N15/10
CPCB82Y30/00B82Y40/00C01G49/08C01P2004/03C01P2004/04C01P2004/84C12N15/1013C23C16/402C23C16/45555H01F1/01H01F41/00
Inventor 侯立威王鹏吴志能胡三元张军夏振宇周政
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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