CN102277034B - Method for preparing magnetic ink - Google Patents

Method for preparing magnetic ink Download PDF

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CN102277034B
CN102277034B CN2011101449813A CN201110144981A CN102277034B CN 102277034 B CN102277034 B CN 102277034B CN 2011101449813 A CN2011101449813 A CN 2011101449813A CN 201110144981 A CN201110144981 A CN 201110144981A CN 102277034 B CN102277034 B CN 102277034B
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CN102277034A (en
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韩满贵
蔡黎
邓龙江
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University of Electronic Science and Technology of China
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Abstract

The invention relates to a method for preparing magnetic ink, and relates to the technology of electronic materials. The method comprises the following steps of: 1) preparing soft magnetic nanometer magnetic granules serving as raw materials; 2) weighing a certain quantity of dispersing agent, dissolving into a solvent with deionized water, ethanol and isopropanol in a ratio of x:y:z, wherein a mass ratio of the raw materials to the dispersing agent ranges from 25:1 to 4:3, a mass ratio of the raw materials to the solvent ranges from 1:50 to 1:500, x is more than or equal to 6 and is less than or equal to 12, y is more than or equal to 1 and less than or equal to 4, and z is more than or equal to 1 and less than or equal to 3; 3) adding a coupling agent, a surfactant and a defoaming agent into the solvent; and 4) adding the soft magnetic nanometer magnetic granules into solution, dispersing by using ultrasonic waves for 30 to 60 minutes, standing, and separating precipitates out to obtain the nanometer magnetic ink. By the method, large-area electromagnetic wave absorption membranes can be produced in low cost, outputted graphs are high in accuracy, distinct in boundary and uniform in distribution, and various complex ingredients and image flexible wave-absorbing membranes can be prepared.

Description

The preparation method of magnetic ink
Technical field
The invention belongs to technical field of electronic materials.
Background technology
After stepped into information society, the mankind produce and life in the electrical equipment that uses more and more, and this trend also will continue, so the electromagnetic environmental pollution that is caused by the electromagnetism place in living environment is also more and more stronger.The research pay attention to day by day of countries in the world to electromagnetic wave shielding, absorbing material, domestic many units are devoted to this research, achieve initial success.The major measure of controlling at present Contamination of Electromagnetic Wave has: inhale ripple, filtering, antagonism and shielding.The flexible materials of absorption of electromagnetic wave and shielding there are two kinds of absorption-type and reflection-types.And the flexible composite of this absorption and reflection electromagnetic wave, having light, thin, the gentle characteristics of quality can cut randomly, make, paste according to the needs of use occasion.The compatible layer that can be used for electronic devices and components, the protective layer of the shield cap of precision instrument, the wall paper of secret chamber, curtain and door curtain, signal wire, portable shielding account.Can be attached in each electronic product simultaneously, prevent electromagnetic radiation and interference, as the interference between the electromagnetic interference in communication distance, IC chip and computer substrate radiation and internal reflection and liquid crystal and substrate etc.
The method for preparing at present absorption of electromagnetic wave and shielded flexible film has the methods such as magnetron sputtering, chemical vapor deposition, but their complex process, cost is high, and the time is long, is unfavorable for scale operation.And spray ink Printing is as the office means of generally using.A plurality of ink-jet systems are arranged, and each ink-jet system has the ink of distinct colors.The preparation means that is used for the plane function material, the advantage such as it is simple that it possesses the moulding of the complex figure of control, pointwise control, technique, and low and cycle of cost is short.The fexible film that accurately prepares absorption of electromagnetic wave and shielding by one step of preparation magnetic ink has obvious advantage., along with the development of electronics and information industry, thisly by the preparation magnetic ink, come the advantage of the flexible absorbing material of spray ink Printing will be more and more significant.
Summary of the invention
Problem to be solved by this invention is, provides that a kind of technique is simple, cost is low and the cycle is short, and one-step moulding does not need the preparation method of heat treated spray ink Printing with magnetic ink simultaneously.
The technical scheme that the present invention solve the technical problem employing is that the preparation method of magnetic ink, comprise the steps:
1) preparing the soft magnetism nano magnetic particle is raw material;
2) take a certain amount of dispersion agent, fully being dissolved in deionized water, ethanol and Virahol ratio is deionized water: in the solvent of ethanol: Virahol=x: y: z, and 6≤x≤12,1≤y≤4,1≤z≤3; The mass ratio of raw material and dispersion agent is 25: 1-4: 3, and the quality volume of raw material and solvent (g: ml) than being 1: 50-1: 500; Take a certain amount of dispersion agent, fully being dissolved in deionized water, ethanol and Virahol ratio is in the solvent of x: y: z, and the mass ratio of raw material and dispersion agent is 25: 1-4: 3, the mass volume ratio of raw material and solvent is 1: 50-1: 500,6≤x≤12,1≤y≤4,1≤z≤3; Mass unit is gram, and volume unit is milliliter;
Described dispersion agent is the aniorfic surfactant such as Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, dodecyl sodium naphthalene sulfonate, sodium oleate or Sodium hexametaphosphate 99;
3) add linking agent, tensio-active agent in solvent, adjust viscosity in 2-10mpas, surface tension, at 32-45mN/m, adds the defoamer of solvent quality 0.001-0.05%, cmpletely be dissolved in solvent;
4) the soft magnetism nano magnetic particle is slowly added step 3) solution of gained and with ultrasonic wave, disperse 30-60min, isolated precipitation, and namely obtained the nano-magnetic ink in standing 1 day.
Described soft magnetism nano magnetic particle composition is Fe, Co, Ni, Fe 3O 4, CoFe 2O 4Or NiFe 2O 4, particle diameter is less than 50nm.
Further, described step 1) comprising:
(1.1) in mole, dissolve the FeCl of 0.01mol in every 100mL water 24H 2The FeCl of O and 0.04mol 36H 2O, after magnetic agitation, slowly drip excessive ammonia solution, cleans, and obtains pre-reaction material;
(1.2) after the precursor ultra-sonic dispersion, and the tensio-active agent mixing, 180 ℃ of hydrothermal treatment consists 12h;
(1.3) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 4h, obtains Fe under 60 ℃ 3O 4Powder is as the soft magnetism nano magnetic particle.
Described step 2) dispersion agent that adds 1/25～3/4 raw materials quality after in, deionized water, ethanol and Virahol mix; Dispersion agent is sodium laurylsulfonate, dodecyl sodium naphthalene sulfonate, sodium oleate or Sodium hexametaphosphate 99.
Step 3) in, the defoamer add-on is the hexadecanol of 0.001-0.05% solution quality, and tensio-active agent is the polyoxyethylene glycol of 0.5%-5% solution quality; Linking agent is the water-base resin of 1-5% solution quality;
Step 4) in, take the soft magnetism nano magnetic particle that makes and slowly add in mixing solutions,
Carry out simultaneously ultrasonic wave and disperse 30-60min.
Perhaps, described step 1) comprising:
(2.1) in mole, dissolve the Ni (NO of 0.01mol in every 120mL water 3) 26H 2Fe (the NO of O, 0.02mol 3) 39H 2O, after magnetic agitation, slowly dripping excessive ammonia solution to pH value is 10, after fully reacting one hour, with suction filtration, cleans 3～5 times, obtains pre-reaction material;
(2.2) precursor of ultra-sonic dispersion and tensio-active agent are changed in hydrothermal reaction kettle over to 200 ℃ of hydrothermal treatment consists 15h;
(2.3) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 3h, obtains NiFe under 60 ℃ of vacuum drying ovens 2O 4Black powder as the soft magnetism nano magnetic particle.
Described step 2)～step 4), in the mixed solvent of 120ml deionized water, 20ml ethanol and 10ml Virahol or 95ml deionized water, 31.5ml ethanol and 23.5ml Virahol, add the Sodium dodecylbenzene sulfonate of 0.25g as dispersion agent; Add defoamer hexadecanol 0.048g and surfactant polyethylene 4.8g, add the linking agent adjusting viscosity to 5mpas, linking agent is the mixing solutions of water-borne acrylic resin 3g and ethylene glycol 4.3ml; Take the NiFe that 1g makes 2O 4Slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse 30min.
Magnetic ink technology of preparing of the present invention can be used for printing the fexible film of big area absorption of electromagnetic wave and shielding, the anti-electromagnetic interference that can be used for electronic devices and components, guarantee the stability of electronic product in complex electromagnetic environment, in military stealthy technique field, also possess potential using value.The present invention has realized the low cost production of big area electromagentic wave absorption film, and the output pattern precision is high, graphic limit is clear and be evenly distributed and the preparation of various complicated ingredient and image flexible wave absorbing thin film.
Description of drawings
Fig. 1 does not add dispersion agent Fe 3O 4The sreen analysis graphic representation.
Fig. 2 is the dispersion effect graphic representation of different dispersion agents.
Fig. 3 is the zeta current potential influence curve figure of dispersion agent add-on.
Fig. 4 is spray ink Printing Fe 3O 4The dynamic permeadility graphic representation of magneticthin film.
Fig. 5 is spray ink Printing Fe 3O 4The dynamic specific inductivity collection of illustrative plates of magneticthin film.
Fig. 6 is Fe in magnetic ink 3O 4Magnetic hysteresis loop figure.
Fig. 7 is the magnetic Fe of ink-jet printing process preparation 3O 4The absorbing property graphic representation of film.
Fig. 8 is NiFe in magnetic ink 2O 4Magnetic hysteresis loop figure.
Fig. 9 is the NiFe of ink-jet printing process preparation 2O 4The absorption of electromagnetic wave performance graphic representation of magneticthin film.
Figure 10 is the magnetic hysteresis loop figure of Fe Nano-Powders in magnetic ink.
Figure 11 is the absorption of electromagnetic wave performance graphic representation that ink-jet printing process prepares flexible magnetic iron film.
Embodiment
, as an embodiment, the present invention includes following step:
1) prepare the raw material of magnetic ink for the soft magnetism nano particle conduct that goes out the optimum size distribution with the hydro-thermal legal system;
2) getting the nano magnetic particle of preparing is raw material, takes a certain amount of dispersion agent, fully is dissolved in the solvent of deionized water, ethanol and Virahol.The mass ratio of raw material and dispersion agent is 25: 1-4: 3, and the mass ratio of raw material and solvent is 1: 50-1: 500;
3) add linking agent, tensio-active agent to adjust viscosity in 2-10mpas, surface tension, at 32-45mN/m, adds the defoamer of solvent quality 0.001-0.05%, cmpletely be dissolved in solvent.
4) nano magnetic particle is slowly added solution and with ultrasonic wave, disperse 30-60min, isolated precipitation, and namely prepared the nano-magnetic ink in standing 1 day.
5) magnetic ink that will prepare is poured in ink-jet print cartridge and carries out spray ink Printing on fexible film.
In the present invention, prepared raw material is as Fe, Co, Ni, Fe 3O 4, CoFe 2O 4, NiFe 2O 4Deng the soft magnetism nano magnetic particle of particle diameter less than 50nm.Prepare the spray ink Printing magnetic ink and must add dispersion agent could form even colloid, dispersion agent is Sodium dodecylbenzene sulfonate (SDBS), sodium oleate or Sodium hexametaphosphate 99 (SMHP).Be no more than 500nm with the largest particle particle diameter that dispersant-coated prepares in ink, for realizing printing, require discrete particles maximum particle diameter and injection diameter ratio less than 1: 50.The fexible film of printing in experiment is the films such as PET, PE and PVC.
Preparation process is as follows more specifically:
Embodiment 1: nanometer Fe 3O 4The magnetic ink preparation
Fe 3O 4Preparation:
(a) with FeCl 24H 2O (2.54g, 0.01mol), FeCl 36H 2O (6.5g, 0.04mol) is dissolved in 100mL water, after magnetic agitation, slowly drips excessive ammonia solution, with suction filtration, cleans 3-5 time, obtains pre-reaction material.
(b) precursor of ultra-sonic dispersion and tensio-active agent are changed in hydrothermal reaction kettle over to 180 ℃ of hydrothermal treatment consists 10h.
(c) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 8h, obtains Fe under 60 ℃ of vacuum drying ovens 3O 4Black powder.
The preparation of ink:
(a) in the mixed solvent of 120ml deionized water, 15ml ethanol and 15ml Virahol, add the Sodium hexametaphosphate 99 (SMHP) of 0.25g as dispersion agent; Add defoamer (hexadecanol 0.048g) and tensio-active agent (polyoxyethylene glycol 4.8g), viscosity adjustment (ethylene glycol 4.3ml).
(b) take the Fe that 1g makes 3O 4Slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse half an hour.
(c) reaction finishes, standing one day filtering-depositing, the magnetic ink that must prepare.
Embodiment 2: nano-Ni/Fe 2O 4The magnetic ink preparation
NiFe 2O 4Preparation:
(a) with Ni (NO 3) 26H 2O (2.905g, 0.01mol), Fe (NO 3) 39H 2O (8.08g, 0.02mol) is dissolved in 120mL water, and after magnetic agitation, slowly dripping excessive ammonia solution to pH value is 10, after fully reacting one hour, with suction filtration, cleans 3-5 time, obtains pre-reaction material.
(b) precursor of ultra-sonic dispersion and tensio-active agent are changed in hydrothermal reaction kettle over to 200 ℃ of hydrothermal treatment consists 15h.
(c) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 3h, obtains NiFe under 60 ℃ of vacuum drying ovens 2O 4Black powder.
The preparation of ink:
1) (a) in the mixed solvent of 120ml deionized water, 20ml ethanol and 10ml Virahol, add the Sodium dodecylbenzene sulfonate of 0.25g as dispersion agent; Add defoamer (hexadecanol 0.048g) and tensio-active agent 35mN/m (polyoxyethylene glycol 4.8g), add linking agent adjusting viscosity 5mpas (water-borne acrylic resin 3g, ethylene glycol 4.3ml).
(b) take the NiFe that 1g makes 2O 4Slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse 30min.
(c) reaction finishes, standing one day filtering-depositing, the magnetic ink that must prepare.
Perhaps, ink prepares according to following step:
(a) in the mixed solvent of 95ml deionized water, 31.5ml ethanol and 23.5ml Virahol, add the Sodium dodecylbenzene sulfonate of 0.25g as dispersion agent; Add defoamer (hexadecanol 0.048g) and tensio-active agent 35mN/m (polyoxyethylene glycol 4.8g), add linking agent adjusting viscosity 5mpas (water-borne acrylic resin 3g, ethylene glycol 4.3ml).
(b) take the NiFe that 1g makes 2O 4Slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse 30min.
(c) reaction finishes, standing one day filtering-depositing, the magnetic ink that must prepare.
Specific embodiment 3: nano metal iron powder magnetic ink preparation
The preparation of nanometer iron powder:
(a) with FeSO 4(3.04g, 0.02mol), in 15mL N 2H 42H 2O is dissolved in 60mL deionized water and 20ml ethanol through magnetic agitation, and dripping NaOH solution to pH value is 10.
The solution that (b) will prepare and tensio-active agent (oleic acid) change in hydrothermal reaction kettle, fill 70%, 150 ℃ of hydrothermal treatment consists 6h of reactor.
(c) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 3h, obtains black powder under 60 ℃ of vacuum drying ovens.
The preparation of ink:
(a) in the mixed solvent of 120ml deionized water, 10ml ethanol and 20ml Virahol, add the sodium oleate of 0.25g as dispersion agent; Adding defoamer (hexadecanol 0.048g) and tensio-active agent adjustment sheet surface tension is 35mN/m (polyoxyethylene glycol 4.8g), and adding the linking agent adjusting viscosity is 5mpas (water-borne acrylic resin 3g, ethylene glycol 4.3ml).
(b) take the Fe that 1g makes and slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse 30min.
(c) reaction finishes, standing one day filtering-depositing, the magnetic ink that must prepare.
Print experiment: the ink that will prepare, inject the print cartridge that cleans up, put into Epson ME1+ printer, print the film that obtains printing on the PET film.
Through the magnetic ink based on flexible big area spray ink Printing of above technique preparation, the particle diameter of its dispersion is all less than 500nm, and the particle diameter that simultaneously different dispersion agents disperse is through ZetaPALS, and ZetaPotential Analyzer analyzes.The initial permeability μ of material iAnalyze the saturation induction density B of printing thin film with HP4275LCR s, residual magnetic flux density B rWith coercive force H cTest with vibrating sample magnetometer (VSM).Its performance index are as follows:
Sodium hexametaphosphate 99 disperses particle diameter and with the spray orifice ratio, is respectively: 160nm; 1: 77.1
Sodium dodecylbenzene sulfonate disperses particle diameter and spray orifice ratio to be respectively: 180nm; 1: 65.8
Sodium oleate disperses particle diameter and spray orifice ratio to be respectively: 260nm; 1: 54.
Fig. 1 demonstration does not add dispersion agent Fe 3O 4The sreen analysis of ferrite nanometer particle.Can find out the Fe that does not add dispersion agent on scheming 3O 4Two sections distributions about 300nm and 1350nm respectively, appear in the sreen analysis curve of solution.Naturally the Fe that disperses in solution 3O 4Size distribution is inhomogeneous, and mean particle size is at 394nm.And due to the injection diameter of ink-jet printer at 27 μ m, realize good printing, needing discrete particles and spray orifice ratio is below 1: 50.And be the Fe that disperses 3O 4Particle has a large amount of particles greater than 1 micron, can cause shower nozzle to stop up, irrealizable printing.
Fig. 2 be add Sodium hexametaphosphate 99 (SMHP), Sodium dodecylbenzene sulfonate (SDBS) and sodium oleate as dispersion agent to Fe 3O 4, NiFe 2O 4The sreen analysis that disperses with the nano particle of Fe Nano-Powders.As can be seen from the figure the particle diameter of SMHP, SDBS and sodium oleate concentrates on respectively 160nm, 180nm and 260nm left and right.The median size degree of test is respectively 166nm, 192.8nm and 274.4nm.Show that from figure its maximum particle diameter is no more than 500nm, discrete particles maximum particle diameter and injection diameter ratio were respectively 1: 77.1,1: 65.8 and 1: 54, all met and printed requirement.
Fig. 3 represents to add the impact of the additional proportion (dispersion agent is in the mass ratio of raw material) of dispersion agent on the zeta current potential of solution.As can be seen from the figure at the ratio that adds dispersion agent from minimum to greatly.Its current potential is the V trend, adding than being that 0 to 0.25 o'clock potential value is the negative growth value, causing it mainly due to anion surfactant is negative value, and simultaneously seldom, seldom potential value is less so cause conductive particle for the particle in not adding dispersion agent or being dispersed in liquid due to coating seldom the time, and along with the increase of dispersion agent, the particle that disperses is more, conducts electricity, and current potential reduces, electrostatic repulsion forces is large, and is scattered.And along with the dispersion agent that adds is too much, coatedparticles is reunited and is caused disperseing charged amounts of particles to descend, so the current potential increase, disperses variation.
Adopt Fe of the present invention 3O 4Ink is printed as film on the flexible polyester film substrate, the high-frequency electromagnetic parameter of testing film then, as the variation with frequency of magnetic permeability and specific inductivity.Fe as Fig. 4 3O 4The dynamic permeadility performance curve of film.As can be seen from Figure 4, comparatively significantly magnetic permeability dispersion peak is arranged in 1-3GHZ.In measured range of frequency, the magnetic permeability real part changes between 0.8～1.65.The imaginary part of magnetic permeability changes between 0～0.6.As can be seen from Figure 5 Fe 3O 4The real part of its specific inductivity of film that ink is printed changes between 7.5～4, the imaginary part of specific inductivity changes between 0～2.4.Find to exist an obvious dispersion peak near 12GHz.
Provided the Fe for the configuration ink of the present invention in Fig. 6 3O 4The static magnetic performance curve of powder (being magnetic hysteresis loop).Can find out that therefrom this material is soft magnetic materials, its coercive force (H) is 420Oe, and saturation magnetization (M) is 75emu/g, it can be used for ink-jet printing process and prepare the flexible magnetic absorbing material.
What Fig. 7 provided is the magnetic Fe of ink-jet printing process preparation 3O 4The absorbing property of film.Can have certain absorption of electromagnetic wave performance by this fexible film (thickness is 3mm) between 9.3～15GHz from figure, the reflection of electromagnetic wave loss in this bandwidth is less than-10dB.
Provided the NiFe of configuring print ink of the present invention in Fig. 8 2O 4The static magnetic performance curve of material.This material is soft magnetic materials as can be known from this magnetic hysteresis loop, and coercive force (H) size is 130Oe, and saturation magnetization (M) is 27emu/g.
Adopt NiFe of the present invention 2O 4Ink, and with ink-jet printing process, prepared flexible NiFe 2O 4Magneticthin film, measured the absorption of electromagnetic wave performance (reflection of electromagnetic wave loss RL) of this film, as shown in Figure 9.As can be seen from the figure work as NiFe 2O 4The thickness of magneticthin film when 8.5mm, is to have certain absorption of electromagnetic wave performance when frequency between 9.0-9.2GHz and 12-13GHz.
The static magnetic performance curve of Fe Nano-Powders in the magnetic ink that provides in Figure 10 (average nanometer diameter is 55nm).Its coercive force (H) is 500Oe as known in the figure, and saturation magnetization (M) size is 82emu/g.Adopt the preparation of this magnetic ink the flexible magnetic film the absorption of electromagnetic wave performance as shown in figure 11.Be 2.5mm and frequency between 5.5-8GHz the time in thin and thick, this film has absorption of electromagnetic wave performance preferably, and its reflection of electromagnetic wave loss is less than-10dB.

Claims (5)

1. the preparation method of magnetic ink, is characterized in that, comprises the steps:
1) preparing the soft magnetism nano magnetic particle is raw material;
2) take a certain amount of dispersion agent, fully being dissolved in deionized water, ethanol and Virahol ratio is in the solvent of x:y:z, and the mass ratio of raw material and dispersion agent is 25:1-4:3, the mass volume ratio of raw material and solvent is 1:50-1:500,6≤x≤12,1≤y≤4,1≤z≤3; Mass unit is gram, and volume unit is milliliter; Dispersion agent is sodium laurylsulfonate, dodecyl sodium naphthalene sulfonate, sodium oleate or Sodium hexametaphosphate 99;
3) add linking agent, tensio-active agent in solvent, adjust viscosity in 2-10mpas, surface tension, at 32-45mN/m, adds the defoamer of solvent quality 0.001-0.05%, cmpletely be dissolved in solvent; Defoamer is hexadecanol, and tensio-active agent is the polyoxyethylene glycol of 0.5%-5% solution quality; Linking agent is the water-base resin of 1-5% solution quality;
4) the soft magnetism nano magnetic particle is slowly added the solution of step 3) gained and with ultrasonic wave, disperse 30-60min, standing separation goes out precipitation, namely obtains the nano-magnetic ink;
Described soft magnetism nano magnetic particle composition is Fe, Co, Ni, Fe 3O 4, CoFe 2O 4Or NiFe 2O 4, particle diameter is less than 50nm.
2. the preparation method of magnetic ink as claimed in claim 1, is characterized in that, described step 1) comprises:
(1.1) in mole, dissolve the FeCl of 0.01mol in every 100mL water 24H 2The FeCl of O and 0.04mol 36H 2O, after magnetic agitation, slowly drip excessive ammonia solution, cleans, and obtains pre-reaction material;
(1.2) after the precursor ultra-sonic dispersion, and the tensio-active agent mixing, 180 ℃ of hydrothermal treatment consists 12h;
(1.3) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 4h, obtains Fe under 60 ℃ 3O 4Powder is as the soft magnetism nano magnetic particle.
3. the preparation method of magnetic ink as claimed in claim 1, is characterized in that, described step 1) comprises:
(2.1) in mole, dissolve the Ni (NO of 0.01mol in every 120mL water 3) 26H 2Fe (the NO of O, 0.02mol 3) 39H 2O, after magnetic agitation, slowly dripping excessive ammonia solution to pH value is 10, after fully reacting one hour, with suction filtration, cleans 3～5 times, obtains pre-reaction material;
(2.2) precursor of ultra-sonic dispersion and tensio-active agent are changed in hydrothermal reaction kettle over to 200 ℃ of hydrothermal treatment consists 15h;
(2.3) reaction finishes, and product cleans repeatedly through deionized water and ethanol, after dry 3h, obtains NiFe under 60 ℃ of vacuum drying ovens 2O 4Black powder as the soft magnetism nano magnetic particle.
4. the preparation method of magnetic ink as claimed in claim 3, is characterized in that,
Described step 2) in～step 4), in the mixed solvent of every 120ml deionized water, 20ml ethanol and 10ml Virahol, add the Sodium dodecylbenzene sulfonate of 0.25g as dispersion agent; Add defoamer hexadecanol 0.048g and surfactant polyethylene 4.8g, add the linking agent adjusting viscosity to 5mpas, linking agent is the mixing solutions of water-borne acrylic resin 3g and ethylene glycol 4.3ml; Take the NiFe that 1g makes 2O 4Slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse 30min.
5. the preparation method of magnetic ink as claimed in claim 3, is characterized in that,
Described step 2) in～step 4), in the mixed solvent of every 95ml deionized water, 31.5ml ethanol and 23.5ml Virahol, add the Sodium dodecylbenzene sulfonate of 0.25g as dispersion agent; Add defoamer hexadecanol 0.048g and surfactant polyethylene 4.8g, add the linking agent adjusting viscosity to 5mpas, linking agent is the mixing solutions of water-borne acrylic resin 3g and ethylene glycol 4.3ml; Take the NiFe that 1g makes 2O 4Slowly add in the solution that mixes, carry out simultaneously ultrasonic wave and disperse 30min.
CN2011101449813A 2011-05-31 2011-05-31 Method for preparing magnetic ink Expired - Fee Related CN102277034B (en)

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CN102229763B (en) * 2011-06-10 2013-11-13 电子科技大学 Magnetic ink and preparation method for ink-jet printing flexible electromagnetic wave absorption film
CN104059426B (en) * 2014-07-03 2016-12-07 北京科技大学 A kind of method utilizing nano-magnetic powder to prepare magnetic fluid ink
TWI634171B (en) * 2017-08-29 2018-09-01 國立成功大學 Method for fabricating anti-corrosion paint

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US4094804A (en) * 1974-08-19 1978-06-13 Junzo Shimoiizaka Method for preparing a water base magnetic fluid and product
CN1797624A (en) * 2004-12-29 2006-07-05 巨东英 Ferrimagnetism fluid

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US6767396B2 (en) * 2002-07-01 2004-07-27 Nu-Kote International, Inc. Process for the preparation of aqueous magnetic ink character recognition ink-jet ink compositions

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Publication number Priority date Publication date Assignee Title
US4094804A (en) * 1974-08-19 1978-06-13 Junzo Shimoiizaka Method for preparing a water base magnetic fluid and product
CN1797624A (en) * 2004-12-29 2006-07-05 巨东英 Ferrimagnetism fluid

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