CN104018197A - Method for preparing ferroferric oxide magnetic layer on stainless steel fiber surface - Google Patents
Method for preparing ferroferric oxide magnetic layer on stainless steel fiber surface Download PDFInfo
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- CN104018197A CN104018197A CN201410252578.6A CN201410252578A CN104018197A CN 104018197 A CN104018197 A CN 104018197A CN 201410252578 A CN201410252578 A CN 201410252578A CN 104018197 A CN104018197 A CN 104018197A
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- stainless steel
- steel fibre
- magnetic layer
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Abstract
The invention discloses a process for preparing a ferroferric oxide magnetic layer on a stainless steel fiber surface. The process comprises the following steps: pretreatment of a stainless steel fiber, electroplating of the stainless steel fiber, treatment of the stainless steel fiber after electroplating, X-ray diffraction (XRD) analysis after electroplating the ferroferric oxide magnetic layer, observation of a surface topography by a scanning electron microscope (SEM), and magnetic vector space model (VSM) analysis, wherein the treatment of the stainless steel fiber after electroplating comprises preparation of electroplate liquid. The ferroferric oxide with good soft magnetic properties is deposited on the stainless steel fiber by adopting an electroplating technique, adjustment on the ingredients and the soft magnetic properties of the ferroferric oxide magnetic layer is achieved, so that the electrical conductivity and the magnetic property of the fiber can be remarkably improved, and the comprehensive electromagnetic properties of the fiber are good. Thus, the ferroferric oxide magnetic layer has good performances on reflection of electromagnetic waves and absorption of the electromagnetic waves, and the process is simple, convenient to operate and low in cost, and is expected to be well applied to the field of broadband electromagnetic shielding.
Description
Technical field
The invention belongs to magnetic alloy material preparation field, be specifically related to the preparation method of Fe 3 O 4 magnetic layer on Stainless Steel Fibre.
Background technology
Along with the development of science and technology and electronic industry, the application of various electronicss is increasing, electromagnetic radiation has become a kind of new social effects of pollution, and the electromagnetic interference that electromagenetic wave radiation causes not only can affect the normal operation of various electronicss, and HUMAN HEALTH is also had to harm.Electromagnetic pollution is named again in electromagnetic radiation, has been acknowledged as the fifth-largest public hazards after topsoil, water pollution, noise pollution and after sound pollution.And cannot see, can not touch, directly act on machine or human body, be harm serious " stealthy killer ".Therefore, the preparation research of electromagnetic shielding material can not allowed to delay.
Fiber filled matrix material is to study at present a more popular and very promising class electromagnetic shielding material.Fiber filled shielding composite fiber used is mainly carbon fiber, steel fiber and metalized fibers etc. at present.Stainless Steel Fibre in steel fiber is the shielding composite fiber of developing the earliest, has good electroconductibility and certain magnetic property, can well reflect and electromagnetic wave absorption, has a high potential in electromagnetic shielding material application aspect.Due to its high conductivity, make it there is good shielding properties at high band, but because its magnetic permeability is lower, almost there is no shielding properties in lower frequency section, a large amount of research discoveries, the harm in lower frequency magnetic field is particularly serious: on the one hand, the interference that lower frequency magnetic field produces is the important factor that affects the normal work of electronic electric equipment, for example, near the lower frequency magnetic field energy that, engine produces makes, the image of computer, reading and signal equipment produce distortion; On the other hand, lower frequency magnetic field can make central nervous system disorder, the cardiovascular systems imbalance of human body, and HUMAN HEALTH is produced to directly impact.Therefore, the shielding of the radiation that lower frequency magnetic field is produced seems particularly important, so be only difficult to effectively shield with the shielding composite that Stainless Steel Fibre is filled the electromagnetic interference that lower frequency magnetic field produces.
Z 250, because preparation technology is simple, cheap, soft magnetic performance is good, is having very large application prospect mainly with it aspect namely magnetic shielding of low-frequency range.But its specific conductivity is lower, have a strong impact on its effect in high-frequency band shielding properties.
Summary of the invention
The present invention is the shielding properties of comprehensive utilization Stainless Steel Fibre and Z 250, the preparation method of a kind of Stainless Steel Fibre surface Fe 3 O 4 magnetic layer is provided, thereby deposition has the Fe 3 O 4 magnetic layer of good soft magnetic performance on Stainless Steel Fibre, the method has technique simple, easy to operate and coating morphology and the controlled feature of magnetic property.After Stainless Steel Fibre surface deposition Fe 3 O 4 magnetic layer, fiber is all improved significantly aspect magnetic property, comprehensive electromagnetic is functional.The product that the present invention prepares has made up the deficiency of single Stainless Steel Fibre magnetic property, obtain having concurrently the fiber of good electrical properties and magnetic property, thereby can lay in wider frequency range shielding effect basicly for Stainless Steel Fibre filled composite materials, have a good application prospect in electromagnetic shielding field.
The preparation method of a kind of Stainless Steel Fibre of the present invention surface magnetite layer, comprises the following steps:
Step 1, Stainless Steel Fibre pre-treatment: use successively dehydrated alcohol, dilute sulphuric acid ultrasonic cleaning;
The plating of step 2, Stainless Steel Fibre: electroplate as negative electrode as anode, Stainless Steel Fibre with iron plate, obtained the surperficial Stainless Steel Fibre with Fe 3 O 4 magnetic layer;
Step 3, Stainless Steel Fibre are electroplated aftertreatment: the fiber of having electroplated is cleaned to 1min in deionized water for ultrasonic, take out and be placed in after air 11～13h, dry 2h in 60 DEG C of loft drier.
Wherein, the laminated metallographic of Stainless Steel Fibre surface magnetism is Z 250 octahedral crystal structure.
In above-mentioned steps two: electroplate liquid used can be selected one of following two kinds of formulas: the iron trichloride of electroplate liquid 1:0.09mol/L, the trolamine of 0.1mol/L, 2mol/L sodium hydroxide; The iron trichloride of electroplate liquid 20.09mol/L, the trolamine of 0.1mol/L, 2mol/L sodium hydroxide, 0.05mol/L～0.12mol/L Trisodium Citrate.Remain on 60 DEG C and with magnetic agitation at electroplate liquid configuration whole process solution temperature.Electroplating technical conditions is: the distance between described negative electrode and anode is 7～9cm, and current density is 10mA/dm
2～500mA/dm
2, electroplating time is 5～25min, and electroplating temperature is 40 DEG C～100 DEG C, and pH value is 9～13.
In the preparation technology of Stainless Steel Fibre surface deposition Fe 3 O 4 magnetic layer of the present invention, can regulate Z 250 grain-size by adjusting electroplate liquid and current density, thus the magnetic of regulation and control magnetite layer.
The present invention has realized the adjusting to Z 250 grain-size and soft magnetic performance, processing condition are simple, easy to operate, with low cost, by regulating electroplate liquid, temperature and current density (as shown in Figure 7) to control the microscopic appearance (being the size of grain-size) of electroplating Fe 3 O 4 magnetic layer, thus the soft magnetic performance of regulation and control Fe 3 O 4 magnetic layer.
In the present invention, preparation-obtained Stainless Steel Fibre surface Fe 3 O 4 magnetic layer is carried out to following performance test: 1) Stainless Steel Fibre is electroplated the XRD analysis after Fe 3 O 4 magnetic layer; 2) Stainless Steel Fibre is electroplated the surface topography after Fe 3 O 4 magnetic layer; 3) the magnetic VSM that Stainless Steel Fibre is electroplated after Z 250 analyzes.
Gained magnetite layer of the present invention and Stainless Steel Fibre bonding force is strong, soft magnetic performance is good, conductivity depends on Stainless Steel Fibre, electromagnetism over-all properties is better, this makes it have good performance at reflection electromagnetic wave and electromagnetic wave absorption, is expected to obtain good application in wide-band electromagnetic shielding field.
Brief description of the drawings
Fig. 1 is the schematic diagram of electroplanting device used in preparation method of the present invention;
Fig. 2 is the SEM figure that embodiment 1 Stainless Steel Fibre is electroplated magnetite layer rear surface pattern;
Fig. 3 is that embodiment 1 Stainless Steel Fibre is electroplated the XRD figure after magnetite layer;
Fig. 4 is the magnetic hysteresis loop figure of VSM test after embodiment 1 Stainless Steel Fibre plating Z 250;
Fig. 5 is the SEM figure that embodiment 2 Stainless Steel Fibres are electroplated Z 250 rear surface pattern;
Fig. 6 is the magnetic hysteresis loop figure of VSM test after embodiment 2 Stainless Steel Fibres plating Z 250s;
Fig. 7 is under different current densities, the SEM comparison diagram of deposition Fe 3 O 4 magnetic layer pattern (and grain-size), wherein: current density (a) is 50mA/dm
3, current density (b) is 200mA/dm
3, current density (c) is 300mA/dm
3;
Fig. 8 is under the different current densities shown in Fig. 7, the magnetic hysteresis loop figure of deposition Fe 3 O 4 magnetic layer VSM test;
Fig. 9 is under differing temps, the comparison diagram of deposition Fe 3 O 4 magnetic layer pattern (and grain-size), wherein: temperature (a) is 60 DEG C, temperature (b) is 70 DEG C, (c) temperature is 80 DEG C, and temperature (d) is 90 DEG C.
Embodiment:
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail, and it is the convenience in order to understand that embodiment is provided, and is never restriction the present invention.
The preparation method of Stainless Steel Fibre electroplating surface Fe 3 O 4 magnetic layer of the present invention mainly comprises: the pre-treatment of Stainless Steel Fibre, the preparation of Z 250 electroplate liquid and plating and plating aftertreatment.
Embodiment 1: the preparation method of Stainless Steel Fibre electroplating surface Fe 3 O 4 magnetic layer, comprising:
1, the pre-treatment of Stainless Steel Fibre
4K (mass of fibers the is 4000 Stainless Steel Fibre monofilament) stainless fiber beam that is 11 μ m by filament diameter is cut into the length of 5cm, be placed in (the ultrasonic apparatus that Kunshan He Chuan ultrasonic instrument company limited produces ultrasonic in the dehydrated alcohol of room temperature, model is Kh5200E) cleaning 30min, complete rear deionized water rinsing 4 times of using of ultrasonic cleaning; Then the fiber of rinsing well is placed in to the H of room temperature
2sO
4(80mL/L) ultrasonic 5min in solution, finally spends dried up flushing 4 times, naturally dries rear placement to be plated.
2, the preparation of electroplate liquid (Z 250 solution)
First configure the liquor ferri trichloridi A of 0.09mol, heating for dissolving, adds the trolamine of 0.1mol in the solution A preparing and obtains solution B, then the Trisodium Citrate of 0.07mol is joined and in solution B, obtains solution C, finally 2mol sodium hydroxide is slowly added in solution C, constant volume is to 1L.(electroplate liquid configuration whole process solution temperature remain on 60 DEG C and with magnetic agitation)
3, electroplate
Using iron plate (electrical pure iron, 40mm × 60mm) as anode, electroplate as negative electrode through the Stainless Steel Fibre of pre-treatment.Electroplanting device used as shown in Figure 1, wherein, the 1st, D.C. regulated power supply, the 2nd, iron anode plate, the 3rd, Stainless Steel Fibre, the 4th, electroplate liquid, the 5th, plating tank, the 6th, water-bath, the 7th, water, the 8th, mechanical stirring device.Distance L=8cm when plating between negative electrode and positive electrode, electroplating current density is 150mA/dm
2, electroplating time is 10min, and electroplating temperature is 70 DEG C, and pH value is 9.
4, electroplate aftertreatment
After plating finishes, by the fibrous bundle of having electroplated deionized water rinsing 4 times, in air, hang and dry in the air after 12 hours, then at 60 DEG C, be dried 2h in loft drier.
5, Stainless Steel Fibre is electroplated the surface topography after Fe 3 O 4 magnetic layer, Fig. 2 shows Stainless Steel Fibre in embodiment 1 and electroplates the SEM figure of Z 250 rear surface pattern, as can be seen from Figure 2 on Stainless Steel Fibre plated surface the magnetite layer of one deck even compact;
6, Stainless Steel Fibre is electroplated the XRD test after Z 250, and Fig. 3 shows Stainless Steel Fibre in embodiment 1 and electroplates the XRD figure after magnetite layer, has really generated Fe 3 O 4 magnetic layer from Fig. 3 to find out fiber surface.
7, Stainless Steel Fibre is electroplated the magnetic property VSM test after Z 250 closes, Fig. 4 shows Stainless Steel Fibre in embodiment 1 and electroplates the magnetic hysteresis loop figure of VSM test after Z 250, electroplates the soft magnetic performance that has obtained high magnetic permeability, low-coercivity Z 250 from Fig. 4 to find out Stainless Steel Fibre.
Embodiment 2: the preparation method of Stainless Steel Fibre electroplating surface Fe 3 O 4 magnetic layer, comprising:
1, the pre-treatment of Stainless Steel Fibre
4K (mass of fibers the is 4000 Stainless Steel Fibre monofilament) stainless fiber beam that is 11 μ m by filament diameter is cut into the length of 5cm, be placed in (the ultrasonic apparatus that Kunshan He Chuan ultrasonic instrument company limited produces ultrasonic in the dehydrated alcohol of room temperature, model is Kh5200E) cleaning 30min, complete rear deionized water rinsing 4 times of using of ultrasonic cleaning; Then the fiber of rinsing well is placed in to ultrasonic 5min in H2SO4 (80mL/L) solution of room temperature, finally spends dried up flushing 4 times, naturally dry rear placement to be plated.
2, the preparation of electroplate liquid (Z 250 solution)
First configure the liquor ferri trichloridi A of 0.09mol, heating for dissolving, adds the trolamine of 0.1mol in the solution A preparing and obtains solution B, finally 2mol sodium hydroxide is slowly added in solution B, and constant volume is to 1L.
3, electroplate
Using iron plate (electrical pure iron, 40mm × 60mm) as anode, electroplate as negative electrode through the Stainless Steel Fibre of pre-treatment.Electroplanting device is shown in accompanying drawing 1, wherein, and 1-D.C. regulated power supply, 2-iron anode plate, 3-Stainless Steel Fibre, 4-electroplate liquid, 5-plating tank, 6-water-bath, 7-water, 8-mechanical stirring device.Distance L=8cm when plating between negative electrode and positive electrode, electroplating current density is 150mA/dm
2, electroplating time is 10min, and electroplating temperature is 70 DEG C, and pH value is 9.
4, aftertreatment
After plating finishes, by the fibrous bundle of having electroplated deionized water rinsing 4 times, in air, hang and dry in the air after 12 hours, then at 60 DEG C, be dried 2h in loft drier.
5, Stainless Steel Fibre is electroplated the surface topography after Fe 3 O 4 magnetic layer, Fig. 5 shows Stainless Steel Fibre in embodiment 2 and electroplates the SEM figure of Z 250 rear surface pattern, as can be seen from Figure 5 on Stainless Steel Fibre plated surface the magnetite layer of one deck even compact.
7, Stainless Steel Fibre is electroplated the magnetic property VSM test after Z 250, Fig. 6 shows the magnetic hysteresis loop figure that electroplates VSM test after Z 250 in embodiment 2, electroplates the soft magnetic performance that has obtained high magnetic permeability, low-coercivity Z 250 from Fig. 6 to find out stainless fiber.
In embodiment 2, (Fig. 5) compares with embodiment 1 (Fig. 2) and can obviously find out the difference of Stainless Steel Fibre surface magnetite layer grain-size, and embodiment 2 (Fig. 6) relatively has obvious magnetic property to change with embodiment 1 (Fig. 4), this shows by regulating electroplating bath components (adding Trisodium Citrate) can adjust Z 250 grain-size, thus the performance of regulation and control Fe 3 O 4 magnetic layer.
In addition, Fig. 7 shows under different current densities, the comparison diagram of deposition Fe 3 O 4 magnetic layer, as can be seen from Figure 7 its surface topography has significant difference, this shows that the present invention can regulate and control by adjusting process parameter the grain-size of Fe 3 O 4 magnetic layer, and Fig. 8 corresponding magnetic hysteresis loop figure that is Fig. 7, thereby can significantly find out in the increase along with current density, grain-size has had reducing in various degree, and the specific magnetising moment is first to increase to subtract afterwards, this shows the excessive or too small magnetic property that all can affect magnetite layer of Fe 3 O 4 magnetic layer crystal particle size.
Fig. 9 is the SEM that electroplates Z 250 under differing temps, wherein, (a) showing temperature is the plating Z 250 SEM figure of 60 DEG C, (b) showing temperature is the plating Z 250 SEM figure of 70 DEG C, (c) showing temperature is the plating Z 250 SEM figure of 80 DEG C, and temperature (d) is the plating Z 250 SEM figure of 90 DEG C.From Fig. 9, can obviously find out the variation of its surface microstructure size, thereby in preparation technology, can regulate and control by adjusting temperature the magnetic property of magnetite layer.
Although in conjunction with figure, invention has been described above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; instead of restrictive; those of ordinary skill in the art is under enlightenment of the present invention; in the situation that not departing from aim of the present invention, can also make a lot of distortion, within these all belong to protection of the present invention.
Claims (6)
1. a preparation technology for Stainless Steel Fibre surface deposition Fe 3 O 4 magnetic layer, is characterized in that, comprises the following steps:
Step 1, Stainless Steel Fibre pre-treatment: use successively dehydrated alcohol, dilute sulphuric acid ultrasonic cleaning;
The plating of step 2, Stainless Steel Fibre: electroplate as negative electrode as anode, Stainless Steel Fibre with iron plate, obtained the surperficial Stainless Steel Fibre with Fe 3 O 4 magnetic layer;
Step 3, Stainless Steel Fibre are electroplated aftertreatment: the fiber of having electroplated is cleaned to 1min in deionized water for ultrasonic, take out and be placed in after air 11～13h, dry 2h in 60 DEG C of loft drier.
2. the preparation technology of Stainless Steel Fibre surface deposition Fe 3 O 4 magnetic layer according to claim 1, is characterized in that, the laminated metallographic of Stainless Steel Fibre surface magnetism is Z 250 octahedral crystal structure.
3. the preparation technology of Stainless Steel Fibre electroplating surface Fe 3 O 4 magnetic layer according to claim 1, in step 2:
Electroplating bath components used is: the iron trichloride of 0.09mol/L, the trolamine of 0.1mol/L, 2mol/L sodium hydroxide;
Electroplate liquid configuration whole process solution temperature remains on 60 DEG C and with magnetic agitation.
4. the preparation technology of Stainless Steel Fibre electroplating surface Fe 3 O 4 magnetic layer according to claim 1, in step 2:
Electroplating bath components used is: the iron trichloride of 0.09mol/L, the trolamine of 0.1mol/L, 2mol/L sodium hydroxide, 0.05mol/L～0.12mol/L Trisodium Citrate;
Electroplate liquid configuration whole process solution temperature remains on 60 DEG C and with magnetic agitation.
5. according to the preparation technology of Stainless Steel Fibre electroplating surface Fe 3 O 4 magnetic layer described in claim 3 or 4, the electroplating technical conditions in step 2 is:
Distance between described negative electrode and anode is 7～9cm, and current density is 10mA/dm
2～500mA/dm
2, electroplating time is 5～25min, and electroplating temperature is 40 DEG C～100 DEG C, and pH value is 9～13.
6. the preparation technology of Stainless Steel Fibre surface deposition Fe 3 O 4 magnetic layer according to claim 1, is characterized in that, regulates Z 250 grain-size by adjusting electroplate liquid, temperature and current density, thus the magnetic of regulation and control magnetite layer.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105591069A (en) * | 2015-12-18 | 2016-05-18 | 浙江天能能源科技有限公司 | Lithium ion battery |
| CN107419288A (en) * | 2017-07-04 | 2017-12-01 | 徐州工程学院 | A kind of method that anodic oxidation co-precipitation prepares magnetic ferroferric oxide |
| CN110277250A (en) * | 2019-07-17 | 2019-09-24 | 中南大学 | A kind of Fe3O4- GO combination electrode and its preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105591069A (en) * | 2015-12-18 | 2016-05-18 | 浙江天能能源科技有限公司 | Lithium ion battery |
| CN107419288A (en) * | 2017-07-04 | 2017-12-01 | 徐州工程学院 | A kind of method that anodic oxidation co-precipitation prepares magnetic ferroferric oxide |
| CN107419288B (en) * | 2017-07-04 | 2019-02-05 | 徐州工程学院 | A kind of method that anodic oxidation-co-precipitation prepares magnetic ferroferric oxide |
| CN110277250A (en) * | 2019-07-17 | 2019-09-24 | 中南大学 | A kind of Fe3O4- GO combination electrode and its preparation method and application |
| CN110277250B (en) * | 2019-07-17 | 2021-02-19 | 中南大学 | Fe3O4-GO composite electrode and preparation method and application thereof |
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