CN105152643A - Water-based tape-casting slurry for magnetic substrate, preparation method of water-based tape-casting slurry, and magnetic substrate - Google Patents
Water-based tape-casting slurry for magnetic substrate, preparation method of water-based tape-casting slurry, and magnetic substrate Download PDFInfo
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- CN105152643A CN105152643A CN201510479212.7A CN201510479212A CN105152643A CN 105152643 A CN105152643 A CN 105152643A CN 201510479212 A CN201510479212 A CN 201510479212A CN 105152643 A CN105152643 A CN 105152643A
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Abstract
The invention discloses water-based tape-casting slurry for a magnetic substrate, a preparation method of the water-based tape-casting slurry, and the magnetic substrate. The water-based tape-casting slurry for the magnetic substrate comprises: 70-81 parts of ferrite powder, 3-8 parts of an acrylamide monomer, 0.4-1 part of a cross-linking agent, 3-5 parts of a plasticizer, 3-5 parts of a dispersant, and 20-30 parts of water. The preparation method of the water-based tape-casting slurry for the magnetic substrate comprises steps, such as weighing, preparing a mixed solution, and adding ferrite powder into the mixed solution. The water-based tape-casting slurry for the magnetic substrate is prepared through treatment of tape-casting, a gel reaction, cutting, mechanical processing, and sintering. The water-based tape-casting slurry for the magnetic substrate is high in volume fraction of a solid phase, fast in drying, easy in defoaming, uniform in density of a tape-casting substrate, good in flexibility, low in porosity, and high in mechanical strength. The water-based tape-casting slurry is capable of being subjected to mechanical processing.
Description
Technical field
The Magnetic Substrate that the present invention relates to a kind of Magnetic Substrate aqueous tape casting slurry and its preparation method and utilize described Magnetic Substrate aqueous tape casting slurry to prepare.
Background technology
Near-field communication technology (NearFieldCommunication, NFC) be that to combine of release with mobile phone by well-known manufacturers such as PHILIPS Co.'s initiation, Nokia, Sonys be carrier, non-contact IC card application is incorporated in mobile phone, with card, reader, point-to-point three kinds of application models, realize the technical service of the multiple application such as mobile-phone payment, data transmission, accumulated point exchanging, electronic bill, identification, false proof, advertisement.NFC is the simple merging of RF identification (RFID) technology and network technology at first, is be the REID of 13.56MHz based on frequency, has now developed into a kind of short-distance wireless communication technology, and developing state is quite rapid.But, RF identification is very sensitive to some medium, as water, metal etc. all can affect the identification of NFC, hertzian wave often makes the reading/writing distance of label shorten in the effect such as reflection, refraction, decay of media surface or inside simultaneously, thus affects the performance of whole system.In order to ensure that the mobile hand-held device being integrated with NFC function is to the normal reading of transmitter signal, the method of current employing increases one deck soft magnetism shielding material between metal (environment) and antenna, play the induced electricity eddy current that partition metal (environment) produces, holding signal intensity simultaneously, realize high magnetic convergence effect, improve the receiving sensitivity accepting sensitivity and NFC read write line of antenna, increase the reading/writing distance of label.
Wireless charging technology (WirelessChargingTechnology, WCT) refers to the Radio Transmission Technology of electric energy, and popular says, is exactly the wireless reception and registration not realizing electric energy by line in kind.Compared with traditional wired charging, wireless charging have convenient, fast, economize on resources, reduce and use the advantages such as the danger brought of cable under severe conditions.Wireless charging has three kinds of implementations: induction, wireless waves and magnetic field resonance type.Induction is by changing electric field or the magnetic field that two are aimed in coil one, thus induces electric current in another coil, realizes charging to battery, through-put power is large, can reach hundreds of kilowatt but charging distance is limited, and the limit is 10cm, when distance becomes large, efficiency can sharply decline.Wireless waves is that electric energy is launched with the form of microwave by Microwave emission end, and microwave receiving terminal converts the microwave of acceptance to electric current, and its charging distance can reach 10m, but power is little, loss is large, efficiency is low.Magnetic field resonance type wireless charging is that medium intercouples transferring energy with magnetic field, be characterized in that not there is responsive directivity, transmission range carries out Energy Transfer for passing through non-magnetic substance, only have the resonance coupling body consumed energy of same frequency, therefore the wireless power transmission of this mode has higher transmission efficiency.
In above-mentioned NFC and WCT technology, magnetic ferrites is all crucial assemblies.Particularly, in NFC technique, NFC Magnetic Substrate is then the significant components that NFC antenna normally can work in metal environment.In the embody rule of the wireless charging technology of WCT technology, at transmitting terminal and receiving end, soft magnetic ferrite sheet is set in order to increase inducedmagnetic field and shielding coil interference, improves wireless charging efficiency.
Due to modern electronic equipment miniaturization, lighting and integrated requirement, therefore the thickness of Magnetic Substrate must be very thin, can not take too large space and require that Magnetic Substrate has certain snappiness, can fit with device into intimate.Because the Magnetic Substrate green sheet of micron order thickness may or be difficult to by compacting or extrusion forming hardly, and by flow casting molding can easily and effectively, large-arealy prepare slim blank.Flow casting molding is as a kind of important forming method, be widely used in ceramic substrate (comprising NFC Magnetic Substrate) and sandwich preparation, and shaping quality affects the heterogeneous microstructure of material to a great extent, determine the performance of product, application and price.Flow casting molding can be divided into water base shaping with non-aqueous tape-casting according to the type of solvent of slurry.
The current comparative maturity of non-aqueous tape-casting moulding process, can prepare the chip multilayer device of various oxide compound, non-oxidized substance.Solvent conventional in casting technique has ethanol, butanone, trieline, toluene etc.The molecular weight of organic solvent, easily volatilizees, and in film process, volatilization completely.In actual production, use mixed solvent commonplace, especially binary or ternary azeotropic body.Dispersion agent in industry mainly comprises phosphoric acid ester, ethoxy compound, triglyceride and fish oil.Binding agent conventional in slurry is polyvinyl alcohol butyraldehyde (PVB), polymethyl acrylate and ethyl cellulose etc.Conventional softening agent has polyoxyethylene glycol, phthalic ester and ethylene glycol etc.The diaphragm rate of drying adopting non-aqueous tape-casting moulding process to prepare is fast, smooth surface, and microtexture is even, and diaphragm quality can be well controlled.But organic content is higher, after causing diaphragm to sinter, density is low, and working condition is severe, causes very large harm to human body and environment.Simultaneously its solvent is all inflammable substance, there is very large potential safety hazard, and production cost is higher in production process, and therefore, to study with safety, clean, low cost be feature, and aqueous tape casting forming technique has become irreversible trend.
Aqueous tape casting forming technique uses water to substitute organic solvent as solvent, and great majority research at present is all in the experimental phase.And be polar molecule and surface tension is large due to water molecules, and dispersion agent, binding agent, fluidizer, auxiliary agent etc. are organic additives, and there is compatibility problem between water molecules.Therefore, cause that the wettability of the shaping middle water of aqueous tape casting to powder is poor, volatilization is slow and time of drying is long, slurry deaeration is difficult, the defects such as casting films snappiness is poor, and shaping rear warpage easy to crack, easy, intensity are low.
As in an existing specific embodiment, in CN104177077A, disclose a kind of NFC Magnetic Substrate aqueous casting slurry and NFC Magnetic Substrate.Its aqueous casting slurry take water as solvent, containing components such as ferrite powder, dispersion agent, binding agent, softening agent.Wherein, dispersion agent is polyacrylic acid (PAA), binding agent be polyvinyl alcohol (PVA) and polyacrylic acid, softening agent is polyoxyethylene glycol.First measure distilled water with graduated cylinder, weigh dispersion agent, binding agent and softening agent by proportioning, after add in beaker and prepare solution.Under the stirring of stirrer, slowly add ferrite powder, after stirring, slurry is proceeded to ball milling 20 ~ 30h in ball mill, rotational speed of ball-mill is 300 ~ 500r/min, obtains casting slurry, and crosses 100 ~ 200 mesh sieves.The slurry that ball milling is good adds defoamer, put into band vacuum pump container vacuumize, under the negative pressure of 0.1 ~ 0.3MPa, vacuumize 8 ~ 15h, and carry out old process by 1 ~ 1.8h/L, viscosity controller at 10000 ~ 15000mPa.s, obtained flow casting molding slurry.By obtained slurry carrying out flow casting molding containing on the steel bands casting machine of six warm areas, obtain the green sheet band of 80 ~ 150um.Green tape is cut into the small pieces of certain specification size, stores.Finally the green tape of cutting is sintered, and carry out the test of magnetic permeability.
But the chip density after this NFC Magnetic Substrate aqueous casting slurry is shaping is lower, there is density gradient, drying is slow and dried substrate intensity is low, cannot carry out mechanical workout, the efficiency having a strong impact on subsequent handling and the yield rate cut.This is because PVA contains great amount of hydroxy group, can dissolve or swelling in water, is wrapped up by powder granule, give the intensity that substrate is certain by physical actions such as the Van der Waals force of intermolecular generation, hydrogen bond and London forces.Due to the physical action that these effects are only the intermolecular generations of PVA, its reactive force is much smaller than the reactive force of chemical bond.
From the above mentioned, flow casting molding is a kind of forming method that can obtain good quality ceramic substrate of current comparative maturity.But making the base substrate obtained there is following defect due to the inherent defect in shaping mechanism: density is lower, there is density gradient, shaping slow and intensity is low, the defect such as bubble, crackle is easily produced in biscuit, and cracking easy to foaming during drying and sintering, fragility is large, and flexible distortion, dimensional change is also larger.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of Magnetic Substrate aqueous tape casting slurry and its preparation method are provided, to solve, the existence of existing aqueous tape casting slurry is poor to the wettability of powder, volatilization is slow and time of drying is long, slurry deaeration difficulty, casting films snappiness is poor, shaping rear warpage easy to crack, easy, the technical problem that intensity is low.
Another object of the present invention is the above-mentioned deficiency overcoming prior art, a kind of Magnetic Substrate utilizing Magnetic Substrate aqueous tape casting slurry of the present invention to prepare is provided, poor to solve existing Magnetic Substrate snappiness, shaping rear warpage easy to crack, easy, the technical problem that intensity is low.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of Magnetic Substrate aqueous tape casting slurry, comprises the component of following weight part
And a kind of preparation method of Magnetic Substrate aqueous tape casting slurry, comprises the steps:
Each component is taken according to Magnetic Substrate aqueous tape casting pulp components ratio of the present invention;
The described acrylamide monomer taken, linking agent, softening agent, dispersion agent are added in described water component and carries out mixing treatment, obtain mixing solutions;
In described mixing solutions, add described ferrite powder, after carry out ball-milling processing and degassed process.
And a kind of Magnetic Substrate, it is by Magnetic Substrate aqueous tape casting slurry of the present invention through comprising flow casting molding process, and gel reaction process, cuts process, and machining processes and sintering processes form.
Compared with prior art, the invention described above Magnetic Substrate aqueous tape casting slurry adopts acrylamide monomer component to build gel injection system, makes Magnetic Substrate aqueous tape casting slurry of the present invention can gel casting forming with the component effect such as linking agent.This component effect such as acrylamide monomer component and dispersion agent, effectively can improve ferrite powder body burden, thus improves the solid volume fraction of Magnetic Substrate aqueous tape casting slurry of the present invention.Therefore, Magnetic Substrate aqueous tape casting slurry of the present invention is by the component synergism contained by it, make Magnetic Substrate aqueous tape casting slurry solid volume fraction of the present invention high, good to the wettability of steel band, volatilization is fast, time of drying is short, slurry deaeration easily, curtain coating chip density is even, snappiness is good, physical strength is high, can carry out mechanical workout.
The invention described above Magnetic Substrate preparation method of aqueous tape casting slurry passes through its blending process, makes each component disperses even, to form stable dispersion system, and easy deaeration, thus ensure that curtain coating chip density is even, snappiness is good, high mechanical strength.In addition, its preparation method technique is simple, and condition is easily controlled, low for equipment requirements, effectively reduces its production cost, is suitable for suitability for industrialized production.
Therefore, above-mentioned Magnetic Substrate carries out attached gel molding process with Magnetic Substrate aqueous tape casting slurry basis of the present invention and casting technique is prepared from, and therefore, Magnetic Substrate even density of the present invention, intensity is high, snappiness good, can carry out mechanical workout.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is preparation method's process flow sheet of Magnetic Substrate aqueous tape casting slurry;
Fig. 2 is Magnetic Substrate preparation method process flow sheet.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment and accompanying drawing, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of solid volume fraction high, the Magnetic Substrate aqueous tape casting slurry that dispersion system is stable.This Magnetic Substrate aqueous tape casting slurry comprises the component of following weight part:
Wherein, the ferrite powder in above-mentioned Magnetic Substrate aqueous tape casting slurry embodiment, as function matrix component, gives Magnetic Substrate as strengthened the function such as inducedmagnetic field and shielding interference.In order to improve this effect of ferrite powder, in one embodiment, described ferrite powder selects particle diameter to be micron-sized ferrite powder.In a particular embodiment, described ferrite powder selects particle diameter to be the ferrite powder of 3-5 μm.In another specific embodiment, described ferrite powder selects nickel-copper-zinc ferrite powder.
In certain embodiments, this ferrite powder can be the weight parts such as 70 parts, 71 parts, 72 parts, 73 parts, 74 parts, 75 parts, 76 parts, 77 parts, 78 parts, 79 parts, 80 parts, 81 parts at the content of Magnetic Substrate aqueous tape casting slurry, by adjusting its content, to realize the performance regulating curtain coating substrate, as correlated performances such as intensity, density, physical strengths.
Acrylamide monomer component in above-mentioned Magnetic Substrate aqueous tape casting slurry embodiment builds gel injection system, can significantly improve the slurry solid volume fraction of Magnetic Substrate aqueous tape casting slurry.This component effect such as acrylamide monomer component and linking agent simultaneously makes Magnetic Substrate aqueous tape casting slurry of the present invention can gel casting forming, thus make Magnetic Substrate aqueous tape casting slurry of the present invention after casting molding processes, under the effect of the components such as initiator, this acrylamide monomer and linking agent carry out crosslinking reaction, to realize the in-situ solidifying of ferrite powder particle, thus ensure that curtain coating chip density is even, avoid the curtain coating substrate formed as existing aqueous tape casting slurry to there is the deficiency of density gradient.
Therefore, the crosslinker component in above-mentioned Magnetic Substrate aqueous tape casting slurry selects at least one in N,N methylene bis acrylamide, polyethylene glycol dimethacrylate.This preferred linking agent can carry out crosslinking reaction with acrylamide monomer after casting molding processes, better to realize the in-situ solidifying of ferrite powder particle, improves the even performance of curtain coating chip density.
In certain embodiments, this acrylamide monomer can be the weight parts such as 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts at the content of Magnetic Substrate aqueous tape casting slurry.
In other specific embodiments, this linking agent can be the weight parts such as 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts at the content of Magnetic Substrate aqueous tape casting slurry.
By adjusting the content of acrylamide monomer and linking agent, to realize the performance regulating curtain coating substrate, as correlated performances such as intensity, even density, mechanical workouts.
In one embodiment, the plasticizer components in above-mentioned Magnetic Substrate aqueous tape casting slurry selects at least one in polyoxyethylene glycol, polyvinyl alcohol, glycerol.This softening agent selected effectively can improve the plasticity of curtain coating substrate, improves the efficiency cut of curtain coating substrate.
In certain embodiments, this softening agent can be the weight parts such as 3 parts, 3.5 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts at the content of Magnetic Substrate aqueous tape casting slurry.
Dispersant component in above-mentioned Magnetic Substrate aqueous tape casting slurry can with the effect of the component such as acrylamide monomer, linking agent, improve the Magnetic Substrate solid volume fraction of aqueous tape casting slurry.For in one embodiment, this dispersant component selects mixture, ammonium polyacrylate, ammonium polymethacrylate, the magnesium citrate of polyacrylic acid and ammonium citrate) at least one.Select this dispersion agent can significantly improve the solid volume fraction of Magnetic Substrate aqueous tape casting slurry.
In a further embodiment, in the mixture of above-mentioned polyacrylic acid and ammonium citrate, the mass ratio of polyacrylic acid and ammonium citrate is (6 ~ 1): 1.
In certain embodiments, this dispersion agent can be the weight parts such as 3 parts, 3.5 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts at the content of Magnetic Substrate aqueous tape casting slurry.By adjusting the content of dispersion agent, with the component synergism such as acrylamide monomer, to realize regulating and to improve the solid volume fraction of Magnetic Substrate aqueous tape casting slurry.
Water in above-mentioned Magnetic Substrate aqueous tape casting slurry is as dissolving and disperse other each components, to form stable dispersion system.In one embodiment, this wet concentration deionized water, to reduce the foreign matter content of Magnetic Substrate aqueous tape casting slurry.
Further, the Magnetic Substrate in the various embodiments described above with aqueous tape casting slurry also containing pH adjusting agent, in order to by pH regulator to 11 ~ 12 of Magnetic Substrate with aqueous tape casting slurry.The pH of this scope effectively can reduce the viscosity of Magnetic Substrate aqueous tape casting slurry, to improve the homogeneity of curtain coating chip density.In one embodiment, realize pH11 ~ 12 pH adjusting agent can but be not limited only to ammoniacal liquor.
In addition, the Magnetic Substrate aqueous tape casting slurry in the various embodiments described above can also contain the components such as defoamer, in order to reduce the air bubble content in Magnetic Substrate aqueous tape casting slurry, to reduce the void content of curtain coating substrate.
Therefore, the various embodiments described above Magnetic Substrate by the component synergism contained by it, makes Magnetic Substrate aqueous tape casting slurry solid volume fraction high with aqueous tape casting slurry, good to the wettability of steel band, volatilization is fast, time of drying is short, and slurry deaeration is easy, and viscosity is little, as being less than 650mPa.s, solid volume fraction, up to 62vol%, effectively reduces the shrinking percentage of Magnetic Substrate, reduces Magnetic Substrate cracking phenomena; And shaping curtain coating chip density is even, snappiness is good, and physical strength is high, can carry out mechanical workout.Wherein, adopt acrylamide monomer component to build gel injection system, make Magnetic Substrate aqueous tape casting slurry of the present invention can gel casting forming with the component effect such as linking agent.This component effect such as acrylamide monomer component and dispersion agent, effectively can improve ferrite powder body burden, thus improves the solid volume fraction of Magnetic Substrate aqueous tape casting slurry of the present invention.
Correspondingly, the embodiment of the present invention additionally provides a kind of preparation method of above-mentioned Magnetic Substrate aqueous tape casting slurry.In one embodiment, this Magnetic Substrate with preparation method's process flow sheet of aqueous tape casting slurry as shown in Figure 1, it comprises the steps:
Step S01: take each component according to Magnetic Substrate aqueous tape casting pulp components ratio mentioned above;
Step S02: the described acrylamide monomer taken in step S01, linking agent, softening agent, dispersion agent are added in described water component and carries out mixing treatment, obtain mixing solutions;
Step S03: to step S02 preparation mixing solutions in add described ferrite powder, after carry out ball-milling processing and degassed process.
Particularly, in above-mentioned steps S01, each component preferred content of Magnetic Substrate aqueous tape casting slurry and kind as described above, in order to save length, do not repeat them here.
Mixing treatment in above-mentioned rapid S02 can select conventional mode to process, and as stirred, the modes such as supersound process, make each component disperses evenly.
Amount and kind and the particle diameter etc. of the ferrite powder added to mixing solutions in above-mentioned rapid S03 preferably require all as described above, in order to save length, do not repeat them here.Ball-milling processing can adopt conventional condition to process, as long as can form stable dispersion system by dispersed for ferrite powder to mixing solutions.
If Magnetic Substrate aqueous tape casting slurry mentioned above containing component of antifoam agent time, in one embodiment, before ball milling, first can adding appropriate defoamer and carry out ball-milling processing again, as carried out ball milling 24 hours, forming stable dispersion system.
In one embodiment, the degassed process in this step S04 can be carried out as follows:
By slurry vacuum outgas under the negative pressure of 0.2 ~ 0.5MPa good for ball milling, according to 0.5 ~ 2h/L process.
In one preferred embodiment, after above-mentioned steps S02, before step S03, also comprise the step of the pH regulator to 11 of mixing solutions ~ 12, as the step S02 ' in Fig. 1.By the pH regulator to mixing solutions, to regulate and the final viscosity reducing Magnetic Substrate aqueous tape casting slurry.
In one embodiment, for regulating the pH adjusting agent of mixing solutions pH can select but not only be only ammoniacal liquor.
Therefore, the preparation method of above-mentioned Magnetic Substrate aqueous tape casting slurry is by its blending process, make each component disperses even, to form stable dispersion system, easy deaeration, viscosity is little, as being less than 650mPa.s, solid volume fraction up to 62vol%, effectively reduce the shrinking percentage of Magnetic Substrate, reduce Magnetic Substrate cracking phenomena; And effectively can ensure that curtain coating chip density is even, snappiness is good, high mechanical strength.In addition, its preparation method technique is simple, and condition is easily controlled, low for equipment requirements, effectively reduces its production cost, is suitable for suitability for industrialized production.Secondly, it also has the security feature as other aqueous tape casting slurries, safety and environmental protection.
Correspondingly, on the basis of embodiment of the present invention Magnetic Substrate with aqueous tape casting slurry and preparation method thereof above, the embodiment of the present invention additionally provides a kind of Magnetic Substrate.Embodiment of the present invention Magnetic Substrate Magnetic Substrate aqueous tape casting slurry is by mentioned earlier through comprising flow casting molding process, and gel reaction process, cuts process, and machining processes and sintering processes form, concrete technique as shown in Figure 2.
In one embodiment, the process of flow casting molding shown in Fig. 2 as step S04 method comprise to as described in add initiator and catalyzer in Magnetic Substrate aqueous tape casting slurry after carry out the step of casting molding processes process.
Wherein, initiator and catalyzer select the initiator and catalyzer that can make acrylamide monomer in embodiment of the present invention Magnetic Substrate aqueous tape casting slurry above and linking agent generation crosslinking reaction, in a particular embodiment, ammonium persulphate (APS) selected by initiator, as the ammonium persulfate solution of 10wt%; In another specific embodiment, Tetramethyl Ethylene Diamine (TEMED) selected by this catalyzer.
Accordingly, in a preferred embodiment, add after 10wt% ammonium persulfate solution (according to 2-4ml/10ml slurry) stirs 2-4h in first magnetotropism substrate aqueous tape casting slurry, then add Tetramethyl Ethylene Diamine (TEMED) and stir 3 ~ 5h.
In one embodiment, casting molding processes process be the Magnetic Substrate aqueous tape casting slurry after being added with initiator and catalyzer is added fixed temperature and humidity tape casting machine on carry out flow casting molding, curtain coating substrate thickness is calculated by following formula:
In formula (1), H is casting films thickness, and α is shrinkage coefficient, and h is scraper height, and Δ P is hopper base pressure, and N is slurry viscosity, and V is curtain coating speed, and L is scraper length.
In a preferred embodiment, the temperature of the flow casting molding of fixed temperature and humidity is 10-20 DEG C, relative humidity is 50-70%.
Gel reaction process shown in above-mentioned Fig. 2 step S05 makes the acrylamide monomer in the curtain coating substrate after casting molding processes process and linking agent, under the effect of initiator and catalyzer, crosslinking reaction occur, and forms gel biscuit.In one embodiment, the temperature of this gel reaction process is 5-10 DEG C, humidity is 50-80%.
It is axiomatic that the gel biscuit obtained also needs to carry out drying treatment cutting, before machining processes, concrete can carry out drying at the temperature of 130 DEG C-170 DEG C, concrete can in the baking oven of 130 DEG C, 150 DEG C, 170 DEG C bake drying.
Cutting process shown in above-mentioned Fig. 2 step S06 directly can adopt conventional cutting to process according to the needs of actual production.
Machining processes shown in above-mentioned Fig. 2 step S07 is the thickness in order to regulate the biscuit through cutting process, as cut the wet-milling on carborundum paper of rear biscuit, obtains the thin slice of specific thickness.
Sintering processes shown in above-mentioned Fig. 2 step S08 is by through cutting the biscuit after process and machining processes in 900-1200 DEG C of thermal treatment, obtains Magnetic Substrate finished product.
Therefore, the invention described above Magnetic Substrate carries out being prepared from conjunction with glue molding process and casting technique with aqueous tape casting slurry basis of the present invention, and therefore, Magnetic Substrate even density of the present invention, intensity is high, snappiness good, can carry out mechanical workout.Biscuit intensity particularly after flow casting molding, gel reaction is high, conveniently cuts, and is very beneficial for improving labor productivity, and carries out mechanical workout to dried biscuit, can reach the thickness of below 60um.In addition, the biscuit void content after flow casting molding, gel reaction is low, reduces the loss of Magnetic Substrate.
Now for Magnetic Substrate aqueous tape casting slurry and preparation method and Magnetic Substrate, the present invention is further elaborated.
Embodiment 1
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is the ferrite powder 70 parts of 3 ~ 5um, the mass ratio of acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.4 part, 3 parts, polyoxyethylene glycol softening agent, polyacrylic acid and ammonium citrate is dispersion agent 3 parts, the deionized water 20.6 parts of 3:1.
The present embodiment Magnetic Substrate aqueous tape casting slurry preparation method, comprises the steps:
S11. weigh: by weighing monomeric acrylamide, linking agent N,N methylene bis acrylamide, dispersion agent polyacrylic acid and ammonium citrate, softening agent (polyoxyethylene glycol), micron order ferrite powder in the present embodiment 1, for subsequent use;
S12. prepare premixed liquid: add in measured deionized water by load weighted acrylamide, N,N methylene bis acrylamide, polyacrylic acid, ammonium citrate, polyoxyethylene glycol, stir, until solution clear;
S13. adjust ph: add ammoniacal liquor and regulate the pH value of premixed liquid to be 11 ~ 12;
S14. prepare slurry: in the premixed liquid regulating pH value, add the ferrite powder weighed up, after stirring 2h, add defrother, then ball milling 24h;
S15. vacuum stripping: by slurry vacuum outgas under the negative pressure of 0.2 ~ 0.5MPa good for ball milling, according to 0.5 ~ 2h/L process, acquired substrate aqueous tape casting slurry.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 650mPa.s, and solid volume fraction is the slurry of 55vol%.
Embodiment 2
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is the ferrite powder 81 parts of 3 ~ 5um, the mass ratio of acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.5 part, 3 parts, polyvinyl alcohol softening agent, polyacrylic acid and ammonium citrate is dispersion agent 4 parts, the deionized water 8.5 parts of 3:1.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 650mPa.s, and solid volume fraction is the slurry of 62vol%.
Embodiment 3
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is ferrite powder 81 parts, acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.5 part, 3 parts, polyvinyl alcohol softening agent, ammonium polyacrylate dispersion agent 4 parts, the deionized water 8.5 parts of 3 ~ 5um.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 600mPa.s, and solid volume fraction is the slurry of 62vol%.
Embodiment 4
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is ferrite powder 81 parts, acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.5 part, 3 parts, polyvinyl alcohol softening agent, ammonium polymethacrylate dispersion agent 4 parts, the deionized water 8.5 parts of 3 ~ 5um.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 550mPa.s, and solid volume fraction is the slurry of 62vol%.
Embodiment 5
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is ferrite powder 81 parts, acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.5 part, 3 parts, polyvinyl alcohol softening agent, ammonium polymethacrylate dispersion agent 2 parts, magnesium citrate 2 parts, the deionized water 8.5 parts of 3 ~ 5um.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 500mPa.s, and solid volume fraction is the slurry of 62vol%.
Embodiment 6
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is ferrite powder 81 parts, acrylamide monomer 3 parts, polyethylene glycol dimethacrylate linking agent 0.5 part, 3 parts, polyvinyl alcohol softening agent, ammonium polymethacrylate dispersion agent 2 parts, magnesium citrate 2 parts, the deionized water 8.5 parts of 3 ~ 5um.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 600mPa.s, and solid volume fraction is the slurry of 62vol%.
Embodiment 7
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is ferrite powder 81 parts, acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.5 part, glycerol plasticizer 1.5 parts, 1.5 parts, polyoxyethylene glycol softening agent, ammonium polymethacrylate dispersion agent 2 parts, magnesium citrate 2 parts, the deionized water 8.5 parts of 3 ~ 5um.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 500mPa.s, and solid volume fraction is the slurry of 62vol%.
Embodiment 8
A kind of Magnetic Substrate aqueous tape casting slurry and preparation method thereof, it comprises the component of following weight part:
Particle diameter is ferrite powder 75 parts, acrylamide monomer 3 parts, N,N methylene bis acrylamide linking agent 0.5 part, glycerol plasticizer 1.5 parts, 1.5 parts, polyoxyethylene glycol softening agent, ammonium polymethacrylate dispersion agent 2 parts, magnesium citrate 2 parts, the deionized water 14.5 parts of 3 ~ 5um.
The present embodiment Magnetic Substrate preparation method of aqueous tape casting slurry preparation method with reference to Magnetic Substrate aqueous tape casting slurry in embodiment 1.
After measured, the viscosity of the present embodiment 1 Magnetic Substrate aqueous tape casting slurry is less than 400mPa.s, and solid volume fraction is the slurry of 58vol%.
Magnetic Substrate embodiment
Magnetic Substrate aqueous tape casting slurry embodiment 1 ~ 8 provided is respectively through comprising flow casting molding process, and gel reaction process, cuts process, and machining processes and sintering processes prepare Magnetic Substrate.Particularly,
Flow casting molding: the ammonium persulfate solution (APS of preparation 10wt%, initiator), first add after 10wt% ammonium persulfate solution (according to 2 ~ 4ml/10ml slurry) stirs 2 ~ 4h in slurry, add Tetramethyl Ethylene Diamine (TEMED again, catalyzer), stir 3 ~ 5h; Put into by above-mentioned slurry on the tape casting machine that temperature is 10 ~ 20 DEG C, relative humidity is the fixed temperature and humidity of 50 ~ 70% again and carry out flow casting molding, curtain coating substrate thickness above formula (1) calculates;
Gel reaction: the slurry of above-mentioned flow casting molding is placed in the environment that temperature is 5 ~ 10 DEG C, humidity is 50 ~ 80% and carries out gel reaction, obtain gel base substrate;
Dry: the gel base substrate that gel reaction obtains is dry in the baking oven of 130 DEG C, 150 DEG C, 170 DEG C respectively in temperature;
Cut;
Mechanical workout: by the substrate wet-milling on carborundum paper cut, obtain the thin slice of specific thickness;
Sintering: sample is placed in electric furnace, in 900 ~ 1200 DEG C of sintering, obtains ferrite substrate.
Magnetic Substrate correlated performance is tested:
The Magnetic Substrate prepared according to the method described above is carried out following performance test, records result as shown in table 1 below:
Table 1
As shown in Table 1, Magnetic Substrate intensity prepared by embodiment of the present invention Magnetic Substrate aqueous tape casting slurry is high, void content is low, Magnetic Substrate even density after gel reaction process, can carry out machining processes, and the magnetic ferrite structure base board magnetic permeability after sintering is high.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a Magnetic Substrate aqueous tape casting slurry, comprises the component of following weight part:
2. Magnetic Substrate aqueous tape casting slurry according to claim 1, is characterized in that: the pH of described Magnetic Substrate aqueous tape casting slurry is 11 ~ 12; And/or
The size controlling of described ferrite powder is micron order.
3. Magnetic Substrate aqueous tape casting slurry according to claim 1 and 2, is characterized in that: the particle diameter of described ferrite powder is 3-5 μm.
4. Magnetic Substrate aqueous tape casting slurry according to claim 1, is characterized in that: at least one in N,N methylene bis acrylamide, polyethylene glycol dimethacrylate selected by described linking agent; And/or
At least one in polyoxyethylene glycol, polyvinyl alcohol, glycerol selected by described softening agent; And/or
Described dispersion agent selects at least one in the mixture of polyacrylic acid and ammonium citrate, ammonium polyacrylate, ammonium polymethacrylate, magnesium citrate; And/or
Described ferrite powder selects nickel-copper-zinc ferrite powder.
5. Magnetic Substrate aqueous tape casting slurry according to claim 4, is characterized in that: the polyacrylic acid in the mixture of described polyacrylic acid and ammonium citrate and the mass ratio of ammonium citrate are 1:1 ~ 6:1.
6. a Magnetic Substrate preparation method for aqueous tape casting slurry, comprises the steps:
Each component is taken according to the arbitrary described Magnetic Substrate aqueous tape casting pulp components ratio of claim 1-5;
The described acrylamide monomer taken, linking agent, softening agent, dispersion agent are added in described water component and carries out mixing treatment, obtain mixing solutions;
In described mixing solutions, add described ferrite powder, after carry out ball-milling processing and degassed process.
7. the preparation method of Magnetic Substrate aqueous tape casting slurry according to claim 6, is characterized in that: before add described ferrite powder in described mixing solutions, also comprises the step described mixing solutions pH being adjusted to 11 ~ 12.
8. a Magnetic Substrate, Magnetic Substrate aqueous tape casting slurry described in described Magnetic Substrate is arbitrary by claim 1-5 or the Magnetic Substrate aqueous tape casting slurry prepared by the arbitrary described Magnetic Substrate aqueous tape casting slurry preparation method of claim 6-7 pass through and comprise flow casting molding process, gel reaction process, cut process, machining processes and sintering processes form.
9. Magnetic Substrate according to claim 8, is characterized in that: described flow casting molding treatment process comprise in described Magnetic Substrate aqueous tape casting slurry, add initiator and catalyzer after carry out the step of casting molding processes process; And/or
Gel reaction process be by the curtain coating substrate of gained after casting molding processes process temperature be 5-10 DEG C, humidity is carry out crosslinking reaction in the environment of 50-80%, obtains biscuit; And/or
Sintering processes be by through cut process and machining processes after biscuit in 900-1200 DEG C of thermal treatment.
10. Magnetic Substrate according to claim 9, is characterized in that: the temperature of described casting molding processes process is 10 ~ 20 DEG C, relative humidity is 50 ~ 70%.
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| CN109467424A (en) * | 2018-11-21 | 2019-03-15 | 重庆市鸿富诚电子新材料有限公司 | A kind of nickel-zinc ferrite green tape, preparation method and its Preparation equipment |
| CN116003117A (en) * | 2022-12-12 | 2023-04-25 | 北京航空航天大学 | High solid content soft magnetic Mn-Zn ferrite slurry for gel casting and preparation method thereof |
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| CN101224600A (en) * | 2008-01-25 | 2008-07-23 | 北京科技大学 | Hard magnet ferrite ceramics parts magnetic field gel inject film forming method |
| CN104250096A (en) * | 2013-06-27 | 2014-12-31 | 深圳振华富电子有限公司 | Ferrite material, laminated sheet type inductor and preparation method of laminated sheet type inductor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105682438A (en) * | 2016-02-19 | 2016-06-15 | 深圳鹏汇功能材料有限公司 | High-magnetic-conductivity wave-absorbing sheet and tape-casting slurry and preparation method therefor |
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| CN109467424A (en) * | 2018-11-21 | 2019-03-15 | 重庆市鸿富诚电子新材料有限公司 | A kind of nickel-zinc ferrite green tape, preparation method and its Preparation equipment |
| CN116003117A (en) * | 2022-12-12 | 2023-04-25 | 北京航空航天大学 | High solid content soft magnetic Mn-Zn ferrite slurry for gel casting and preparation method thereof |
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